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

NASA Astrophysics Data System (ADS)

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

2006-11-01

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

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

Carreras, Alejo C., E-mail: acarreras@famaf.unc.edu.ar; Cangiano, María de los A.; Ojeda, Manuel W.

The influence of the amount of complexing agent added to the starting solution on the physicochemical properties of Cu–Ni nanostructured alloys obtained through a chemical route, was studied. For this purpose, three Cu–Ni nanoalloy samples were synthesized by a previously developed procedure, starting from solutions with citric acid to metal molar ratios (C/Me) of 0.73, 1.00 and 1.50. The synthesis technique consisted in preparing a precursor via the citrate-gel method, and carrying out subsequent thermal treatments in controlled atmospheres. Sample characterization was performed by scanning electron microscopy, X-ray microanalysis, X-ray diffraction, transmission electron microscopy, X-ray nanoanalysis and electron diffraction. Inmore » the three cases, copper and nickel formed a solid solution with a Cu/Ni atomic ratio close to 50/50, and free of impurities inside the crystal structure. The citric acid content of the starting solution proved to have an important influence on the morphology, size distribution, porosity, and crystallinity of the Cu–Ni alloy microparticles obtained, but a lesser influence on their chemical composition. The molar ratio C/Me = 1.00 resulted in the alloy with the Cu/Ni atomic ratio closest to 50/50. - Highlights: • We synthesize Cu–Ni nanoalloys by a chemical route based on the citrate-gel method. • We study the influence of the complexing agent content of the starting solution. • We characterize the samples by electron microscopy and X-ray techniques. • Citric acid influences the shape, size, porosity and crystallinity of the alloys.« less

Effect of ophthalmic solution components on acrylic intraocular lenses.

PubMed

Ayaki, Masahiko; Nishihara, Hitoshi; Yaguchi, Shigeo; Koide, Ryohei

2007-01-01

To investigate the effect of ophthalmic solution components on the surface of acrylic intraocular lenses (IOLs). Department of Opthalmology, Showa University School of Medicine. Measurement of the contact angles of ophthalmic solutions on 3 acrylic IOLs was performed. The solutions were diclofenac sodium (Diclod), bromfenac sodium (Bronuck), betamethasone phosphate (Rinderon), dibekacin sulfate (Panimycin), polysorbate 80 (Tween 20), benzalkonium chloride, chlorobutanol, methylparahydroxybenzoate, and propylparahydroxybenzoate. The IOLs were incubated at 35 degrees C for 2 weeks in undiluted ophthalmic solutions and in 1:10 dilutions of ophthalmic solution components. The IOLs were sectioned and observed by scanning electron microscopy. The contact angle of Diclod and Bronuck solutions was the smallest. The contact angle of Rinderon and Panimycin was similar to that of distilled water. Scanning electron microscopy examination of IOLs incubated in ophthalmic solution components showed intralenticular changes. The IOLs immersed in ophthalmic solutions did not show any change, even after extended incubation. The chemical components of ophthalmic solutions, such as surfactants and solvents, permeate acrylic IOLs, suggesting the potential for long-term adverse effects of eyedrops in pseudophakic eyes.

The feasibility of using solution-processed aqueous La2O3 as effective hole injection layer in organic light-emitting diode

NASA Astrophysics Data System (ADS)

Zhang, Yan; Li, Wanshu; Zhang, Ting; Yang, Bo; Zheng, Qinghong; Xu, Jiwen; Wang, Hua; Wang, Lihui; Zhang, Xiaowen; Wei, Bin

2018-01-01

Low-cost and scalable manufacturing boosts organic electronic devices with all solution process. La2O3 powders and corresponding aqueous solutions are facilely synthesized. Atomic force microscopy and scanning electron microscopy measurements show that solution-processed La2O3 behaves superior film morphology. X-ray diffraction and X-ray photoelectron spectroscopy measurements verify crystal phase and typical La signals. In comparison with the most widely-used hole injection layers (HILs) of MoOx and poly(ethylene dioxythiophene):poly(styrene sulfonate) (PEDOT:PSS), enhanced luminous efficiency is observed in organic light-emitting diode (OLED) using solution-processed La2O3 HIL. Current-voltage, impedance-voltage and phase angle-voltage transition curves clarify that solution-processed La2O3 behaves nearly comparable hole injection capacity to MoOx and PEDOT:PSS, and favorably tailors carrier balance. Moreover, the hole injection mechanism of solution-processed La2O3 is proven to be predominantly controlled by Fowler-Nordheim tunneling process and the hole injection barrier height between ITO and NPB via La2O3 interlayer is estimated to be 0.098 eV. Our experiments provide a feasible application of La2O3 in organic electronic devices with solution process.

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.

Microstructure and Properties of a High-Strength Cu-Ni-Si-Co-Zr Alloy

NASA Astrophysics Data System (ADS)

Chenna Krishna, S.; Srinath, J.; Jha, Abhay K.; Pant, Bhanu; Sharma, S. C.; George, Koshy M.

2013-07-01

A high-strength Cu-Ni-Si alloy was developed with the additions of Co and Zr. The aging curve for the alloy was generated using hardness. Electron microscopy studies were conducted to analyze the phases in the alloy. Two types of phases, one of copper matrix and the other of Ni-Si-Co-Zr intermetallic phase, could be identified using scanning electron microscopy. Transmission electron microscopy studies confirmed the presence of two types of precipitates in solution-treated and aged (STA) condition, i.e., Ni2Si and Co2Si. Mechanical properties and electrical conductivity were evaluated in solution-treated (ST) and STA conditions. Aging of the ST samples at 500 °C for 3 h has shown an increase of 72 and 15% in yield strength (YS) and electrical conductivity, respectively. This increase in YS and conductivity on aging is primarily attributed to the formation of fine Ni2Si and Co2Si precipitates.

Microstructure and hardness of bovine enamel in roselle extract solution

NASA Astrophysics Data System (ADS)

Dame, M. T.; Noerdin, A.; Indrani, D. J.

2017-08-01

The aim of this study was to analyze the effect of roselle extract solution on the microstructure and hardness of bovine enamel. Ten bovine teeth and a 5% concentration of roselle extract solution were prepared. Immersions of each bovine tooth in roselle extract solution were conducted up to 60 minutes. The bovine enamel surface was characterized in hardness and microscopy. It was apparent that the initial hardness was 328 KHN, and after immersion in 15 and 60 min, the values decrease to 57.4 KHN and 11 KHN, respectively. Scanning electron microscopy (SEM) revealed changes in enamel rods after immersion in the roselle extract solution.

Synergic Investigation Of The Self-Assembly Structure And Mechanism Of Retroviral Capsid Proteins By Solid State NMR, Transmission Electron Microscopy And Multiscale simulation

DTIC Science & Technology

2017-03-29

310 helix. Green: this work. Cyans: solution NMR RSV CA structure in PDB entry 1D1D.[18] Magentas: X-ray crystallography structure of flat hexameric...to combine cryo-electron microscopy and X-ray crystallography , Methods, 49 (2009) 174-180. [8] K.Y. Chan, J. Gumbart, R. McGreevy, J.M. Watermeyer

Studying localized corrosion using liquid cell transmission electron microscopy

DOE PAGES

Chee, See Wee; Pratt, Sarah H.; Hattar, Khalid; ...

2014-11-07

Using liquid cell transmission electron microscopy (LCTEM), localized corrosion of Cu and Al thin films immersed in aqueous NaCl solutions was studied. We demonstrate that potentiostatic control can be used to initiate pitting and that local compositional changes, due to focused ion beam implantation of Au + ions, can modify the corrosion susceptibility of Al films. Likewise, a discussion on strategies to control the onset of pitting is also presented.

Salt-assistant combustion synthesis of nanocrystalline Nd{sub 2}(Zr{sub 1-x}Sn{sub x}){sub 2}O{sub 7} (0 {<=} x {<=} 1) solid solutions

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

Tong Yuping, E-mail: huabeitong@yahoo.cn; Wang Yanping

2009-11-15

Nanocrystalline Nd{sub 2}(Zr{sub 1-x}Sn{sub x}){sub 2}O{sub 7} series solid solutions were prepared by a convenient salt-assisted combustion process using glycine as fuel. The samples were characterized by X-ray diffraction, Fourier transform infrared spectroscopy, Raman spectroscopy, transmission electron microscopy and high-resolution transmission electron microscopy. The results showed the Zr ion can be partially replaced by Sn ion. The partial substituted products were still single-phase solid solutions and the crystal form remained unchanged. TEM images reveal that the products are composed of well-dispersed square-shaped nanocrystals. The method provides a convenient and low-cost route for the synthesis of nanostructures of oxide materials.

Water-assisted growth of graphene on carbon nanotubes by the chemical vapor deposition method.

PubMed

Feng, Jian-Min; Dai, Ye-Jing

2013-05-21

Combining carbon nanotubes (CNTs) with graphene has been proved to be a feasible method for improving the performance of graphene for some practical applications. This paper reports a water-assisted route to grow graphene on CNTs from ferrocene and thiophene dissolved in ethanol by the chemical vapor deposition method in an argon flow. A double injection technique was used to separately inject ethanol solution and water for the preparation of graphene/CNTs. First, CNTs were prepared from ethanol solution and water. The injection of ethanol solution was suspended and water alone was injected into the reactor to etch the CNTs. Thereafter, ethanol solution was injected along with water, which is the key factor in obtaining graphene/CNTs. Transmission electron microscopy, scanning electron microscopy, X-ray diffraction, and Raman scattering analyses confirmed that the products were the hybrid materials of graphene/CNTs. X-ray photo-electron spectroscopy analysis showed the presence of oxygen rich functional groups on the surface of the graphene/CNTs. Given the activity of the graphene/CNT surface, CdS quantum dots adhered onto it uniformly through simple mechanical mixing.

Novel mesoporous FeAl bimetal oxides for As(III) removal: Performance and mechanism.

PubMed

Ding, Zecong; Fu, Fenglian; Cheng, Zihang; Lu, Jianwei; Tang, Bing

2017-02-01

In this study, novel mesoporous FeAl bimetal oxides were successfully synthesized, characterized, and employed for As(III) removal. Batch experiments were conducted to investigate the effects of Fe/Al molar ratio, dosage, and initial solution pH values on As(III) removal. The results showed that the FeAl bimetal oxide with Fe/Al molar ratio 4:1 (shorten as FeAl-4) can quickly remove As(III) from aqueous solution in a wide pH range. The FeAl-4 before and after reaction with As(III) was characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HR-TEM) and selected area electron diffraction (SAED), Brunauer-Emmett-Teller (BET) surface area measurement, and X-ray photoelectron spectroscopy (XPS). The BET results showed that the original FeAl-4 with a high surface area of 223.9 m 2 /g was a mesoporous material. XPS analysis indicated that the surface of FeAl-4 possessed a high concentration of M-OH (where M represents Fe and Al), which was beneficial to the immobility of As(III). The excellent performance of FeAl-4 makes it a potentially attractive material for As(III) removal from aqueous solution. Copyright © 2016 Elsevier Ltd. All rights reserved.

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

PubMed

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

2004-05-17

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

MORPHOLOGICAL CHANGES IN POLYURETHANE COATINGS ON EXPOSURE TO WATER. (R828081E01)

EPA Science Inventory

When a polyurethane self-priming coating on a sol-gel treated aluminum panel was immersed in dilute Harrison's solution, subsequent change of the polyurethane coating surface was inspected with atomic force microscopy (AFM) and scanning electron microscopy (SEM). After immersi...

Investigation on structural and electrical properties of Fe doped ZnO nanoparticles synthesized by solution combustion method

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

Ram, Mast, E-mail: mastram1999@yahoo.com; Bala, Kanchan; Sharma, Hakikat

In the present study, nanoparticles of Fe doped zinc oxide (ZnO) [Zn{sub 1-x}Fe{sub x}O where x=0.0, 0.01, 0.02, 0.03 and 0.05] were prepared by cost effective solution combustion method. The powder X-ray diffractometry confirms the formation of single phase wurtzite structure. Scanning electron microscopy (SEM) and transmission electron microscopy (TEM) were used to investigate the micrsostructure of Fe-doped ZnO nanoparticles. The DC electrical conductivity was found to increase with temperature and measurement was carried out in the temperature range of 300-473K. DC electrical conductivity increases with temperature and decreases with Fe doping concentration.

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

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

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

2015-06-15

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

Ag(I)-bovine serum albumin hydrosol-mediated formation of Ag3PO4/reduced graphene oxide composites for visible-light degradation of Rhodamine B solution.

PubMed

Ma, Peiyan; Chen, Anliang; Wu, Yan; Fu, Zhengyi; Kong, Wei; Che, Liyuan; Ma, Ruifang

2014-03-01

A cost-effective Ag(I)-bovine serum albumin (BSA) supramolecular hydrosol strategy was utilized to assemble Ag3PO4 nanospheres onto reduced graphene oxide (rGO) sheets. The obtained composites were characterized by X-ray diffraction, scanning electron microscopy, transmission electron microscopy, atomic force microscopy, X-ray photoelectron spectroscopy, UV-vis absorption spectroscopy and Fourier transform infrared spectroscopy. Compared with the pure Ag3PO4 crystals and Ag3PO4 particles prepared with Ag(I)-BSA hydrosol as precursor, the Ag3PO4/rGO composites obtained with different content of graphene oxide indicated improved visible-light-driven photocatalysis activity for the decomposition of Rhodamine B aqueous solution. The results pointed to the possibility of synthesizing graphene-based photocatalysts by metal ion-BSA hydrosol. Copyright © 2013 Elsevier Inc. All rights reserved.

Characterization of Discontinuous Coarsening Reaction Products in INCONEL® Alloy 740H® Fusion Welds

NASA Astrophysics Data System (ADS)

Bechetti, Daniel H.; Dupont, John N.; Watanabe, Masashi; de Barbadillo, John J.

2017-04-01

Characterization of γ' coarsened zones (CZs) in alloy 740H fusion welds via a variety of electron microscopy techniques was conducted. The effects of solute partitioning during nonequilibrium solidification on the amount of strengthening precipitates along the grain boundaries were evaluated via electron-probe microanalysis and scanning electron microscopy. Electron backscatter diffraction was used to present evidence for the preferential growth of CZs toward regions of lower γ' content, even if growth in that direction increases grain boundary area. Scanning electron microscopy and image analysis were used to quantify the propensity for CZs to develop along certain segments of the grain boundaries, as governed by the local variations in γ' content. Scanning transmission electron microscopy with X-ray energy-dispersive spectrometry (XEDS) was used to assess the compositions of the matrix and precipitate phases within the CZs and to quantify the segregation of alloying components to the reaction front. Thermodynamic and kinetic modeling were used to compare calculated and experimental compositions. The work presented here provides new insight into the progression of the discontinuous coarsening (DC) reaction in a complex engineering alloy.

Nanocrystals of [Cu3(btc)2] (HKUST-1): a combined time-resolved light scattering and scanning electron microscopy study.

PubMed

Zacher, Denise; Liu, Jianing; Huber, Klaus; Fischer, Roland A

2009-03-07

The formation of [Cu(3)(btc)(2)] (HKUST-1; btc = 1,3,5-benzenetricarboxylate) nanocrystals from a super-saturated mother solution at room temperature was monitored by time-resolved light scattering (TLS); the system is characterized by a rapid growth up to a size limit of 200 nm within a few minutes, and the size and shape of the crystallites were also determined by scanning electron microscopy (SEM).

Sample Preparation of Nano-sized Inorganic Materials for Scanning Electron Microscopy or Transmission Electron Microscopy: Scientific Operating Procedure SOP-P-2

DTIC Science & Technology

2015-07-01

samples must be thoroughly degreased and dried to eliminate any outgassing from organic contamination and water. Samples can be cleaned ultrasonically ...in an ultrasonic bath for at least 10 minutes to ensure separation of particles (University of California, Riverside, n.d.). These solutions can...be further agitated in the ultrasonic bath to separate particles. It should be noted that excessive ultrasonic agitation can damage samples

Arc-discharge in solution: A novel synthesis method for carbon nanotubes and in situ decoration of carbon nanotubes with nanoparticles

NASA Astrophysics Data System (ADS)

Bera, Debasis

2005-11-01

During the last decade, carbon nanotubes (CNTs) have been envisioned for a host of different new applications. One of the objectives of the present research is to develop a simplified synthesis method for the production of large-scale, low-cost carbon nanotubes with functionality. Herein, a unique, simple, inexpensive and one-step synthesis route of CNTs and CNTs decorated with nanoparticles is reported. The method is simple arc-discharge in solution (ADS). For this new method, a full-fledged optoelectronically controlled instrument is reported here to achieve high efficiency and continuous bulk production of CNTs. In this system, a constant gap between the two electrodes is maintained using a photosensor which allows a continuous synthesis of the carbon nanostructures. The system operates in a feedback loop consisting of an electrode-gap detector and an analogue electronic unit, as controller. This computerized feed system was also used in single process step to produce in situ-decorated CNTs with a variety of industrially important nanoparticles. To name a few, we have successfully synthesized CNTs decorated with 3--4 nm ceria, silica and palladium nanoparticles for many industrially relevant applications. This process can be extended to synthesize decorated CNTs with other oxide and metallic nanoparticles. Sixty experimental runs were carried out for parametric analysis varying process parameters including voltage, current and precursors. The amount of yield with time, rate of erosion of the anode, and rate of deposition of carbonaceous materials on the cathode electrode were investigated. Normalized kinetic parameters were evaluated for different amperes from the sets of runs. The production rate of pristine CNT at 75 A is as high as 5.89 +/- 0.28 g.min-1. In this study, major emphasis was given on the characterizations of CNTs with and without nanoparticles using various techniques for surface and bulk analysis of the nanostructures. The nanostructures were characterized using transmission electron microscopy, high resolution transmission electron microscopy, scanning transmission electron microscopy, energy dispersive spectroscopy and scanning electron microscopy, x-ray photo electron spectroscopy, x-ray diffraction studies, and surface area analysis. Electron microscopy investigations show that the CNTs, collected from the water and solutions, are highly pure except for the presence of some amorphous carbon. (Abstract shortened by UMI.)

Synthesis of samarium doped gadolinium oxide nanorods, its spectroscopic and physical properties

NASA Astrophysics Data System (ADS)

Boopathi, G.; Gokul Raj, S.; Ramesh Kumar, G.; Mohan, R.; Mohan, S.

2018-06-01

One-dimensional samarium doped gadolinium oxide [Sm:Gd2O3] nanorods have been synthesized successfully through co-precipitation technique in aqueous solution. The as-synthesized and calcined products were characterized by using powder X-ray diffraction pattern, Fourier transform Raman spectroscopy, thermogravimetric/differential thermal analysis, scanning electron microscopy with energy-dispersive X-ray analysis, transmission electron microscopy, Fourier transform infrared spectroscopy, Ultraviolet-Visible spectrometry, photoluminescence spectrophotometer and X-ray photoelectron spectroscopy techniques. The obtained results are discussed in detailed manner.

SILVER IMPREGNATION OF ULTRATHIN SECTIONS FOR ELECTRON MICROSCOPY

PubMed Central

Marinozzi, Vittorio

1961-01-01

A new procedure is described for silver impregnation of thin sections for electron microscopy. Sections of various tissues, fixed in OsO4 and embedded in methacrylate, were treated with an ammoniacal silver solution, directly or after oxidation with periodic acid or hydrogen peroxide. After OsO4 fixation all cellular membranous systems exhibit a primary argentaffinity probably due to the reduction of ammoniacal silver solution by the reduced osmium bound to unsaturated lipids. Bleaching the sections with hydrogen peroxide removes the argentaffinity of protoplasmic structures. Treatment of the sections with periodic acid results in decreased argentaffinity of protoplasmic components while the argentaffinity of metaplasmic structures is greatly enhanced. The latter procedure appears particularly useful for enhancing the contrast of basement membranes. PMID:13766855

Fabrication of homogeneously dispersed graphene/Al composites by solution mixing and powder metallurgy

NASA Astrophysics Data System (ADS)

Zeng, Xiang; Teng, Jie; Yu, Jin-gang; Tan, Ao-shuang; Fu, Ding-fa; Zhang, Hui

2018-01-01

Graphene-reinforced aluminum (Al) matrix composites were successfully prepared via solution mixing and powder metallurgy in this study. The mechanical properties of the composites were studied using microhardness and tensile tests. Compared to the pure Al alloy, the graphene/Al composites showed increased strength and hardness. A tensile strength of 255 MPa was achieved for the graphene/Al composite with only 0.3wt% graphene, which has a 25% increase over the tensile strength of the pure Al matrix. Raman spectroscopy, Fourier transform infrared spectroscopy, scanning electron microscopy, and transmission electron microscopy were used to investigate the morphologies, chemical compositions, and microstructures of the graphene and the graphene/Al composites. On the basis of fractographic evidence, a relevant fracture mechanism is proposed.

Physicochemical properties of micelles of poly(styrene-b-[3-(methacryloylamino)propyl]trimethylammonium chloride-b-ethylene oxide) in aqueous solutions.

PubMed

Liu, Jingjing; Liu, Dian; Yokoyama, Yuuichi; Yusa, Shin-Ichi; Nakashima, Kenichi

2009-01-20

Polymeric micelles from a new triblock copolymer, polystyrene-block-poly[(3-(methacryloylamino)propyl)trimethylammonium chloride]-block-poly(ethylene oxide) (PS-b-PMAPTAC-b-PEO), were prepared in aqueous solutions and characterized by various techniques including dynamic light scattering (DLS), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and fluorescence spectroscopy. The micelle consists of a PS core, PMAPTAC shell, and PEO corona. It was revealed by SEM and DLS measurements that the micelles have a spherical structure with a hydrodynamic diameter about 75 nm. The addition of tungstate to the micellar solution caused a morphological change in the micelles from extended to shrunken spheres, which can be attributed to the fact that electrostatic repulsion among the cationic PMAPTAC blocks is canceled by the negative charge of the bound tungstate ions. Effective incorporation of tungstate ions into the micelles were confirmed by TEM and zeta-potential measurements.

Effect of solution treatment on microstructure and properties of duplex stainless steel

NASA Astrophysics Data System (ADS)

Wang, X. Y.; Luo, J. M.; Huang, L. Q.; Wang, H. B.; Ma, C. W.

2017-09-01

The influence of solution treatment on microstructure and properties of 2205 duplex stainless steel (DSS) was studied. The microstructure, precipitates and corrosion resisting property were observed and analyzed by means of optical microscopy (OM), scanning electron microscopy (SEM) and electrochemical methods. The results showed that a large number of brittle σ-phase precipitates, which deteriorate the plasticity and corrosion resistance of the material, were easy to produce in the duplex stainless steel under the low temperature. The precipitation of σ-phase can be decreased and the plasticity and corrosion resistance can be improved by increasing solution temperature. In addition, the ferrite content increases with the increase of solution temperature, while less affected by cooling rate.

Synthesis, Characterization and Antibacterial Activity of BiVO4 Microstructure

NASA Astrophysics Data System (ADS)

Ekthammathat, Nuengruethai; Phuruangrat, Anukorn; Thongtem, Somchai; Thongtem, Titipun

2018-05-01

Hyperbranched BiVO4 microstructure were successfully synthesized by a hydrothermal method. Upon characterization the products by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), Fourier transform infrared (FTIR) spectroscopy, Raman spectroscopy, selected area electron diffraction (SAED) and photoluminescence (PL) spectroscopy, pure monoclinic hyperbranched BiVO4 with dominant vibration peak at 810 cm-1 and strong photoemission peak at 360 nm was synthesized in the solution with pH 1. In the solution with pH 2, tetragonal BiVO4 phase was also detected. In this research, antibacterial activity against S. aureus and E. coli was investigated by counting the colony forming unit (CFU). At 37°C within 24 h, the monoclinic BiVO4 phase can play the role in inhibiting S. aureus growth (350 CFU/mL remaining bacteria) better than that against E. coli (a large number of remaining bacteria).

Graphene Microcapsule Arrays for Combinatorial Electron Microscopy and Spectroscopy in Liquids

DOE PAGES

Yulaev, Alexander; Guo, Hongxuan; Strelcov, Evgheni; ...

2017-04-27

Atomic-scale thickness, molecular impermeability, low atomic number, and mechanical strength make graphene an ideal electron-transparent membrane for material characterization in liquids and gases with scanning electron microscopy and spectroscopy. Here in this paper, we present a novel sample platform made of an array of thousands of identical isolated graphene-capped microchannels with high aspect ratio. A combination of a global wide field of view with high resolution local imaging of the array allows for high throughput in situ studies as well as for combinatorial screening of solutions, liquid interfaces, and immersed samples. We demonstrate the capabilities of this platform by studyingmore » a pure water sample in comparison with alkali halide solutions, a model electrochemical plating process, and beam-induced crystal growth in liquid electrolyte. Spectroscopic characterization of liquid interfaces and immersed objects with Auger and X-ray fluorescence analysis through the graphene membrane are also demonstrated.« less

Enhanced photocatalytic hydrogen production from water-ethanol solution by Ruthenium doped La-NaTaO3

NASA Astrophysics Data System (ADS)

Husin, H.; Alam, P. N.; Zaki, M.; Sofyana; Jakfar; Husaini; Hasfita, F.

2018-04-01

The photocatalytic hydrogen production from ethanol aqueous solution, with the use ruthenium doped La-NaTaO3 has been investigated. Ruthenium doped La-NaTaO3 catalysts are prepared by impregnation method. The catalysts are by X-ray diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The Ru co-catalyst demonstrated from the TEM image shows a good dispersion on the surface of La-C-NaTaO3 with an average particle size between 4-5 nm. The photocatalytic reaction is carried out in a closed reactor with a gas circulation system. The catalytic activity of La-NaTaO3 improved markedly (6.6 times from pure water) when Ru is loaded onto its surface. The hydrogen production is notably enhanced in the presence of ethanol as electron donors. This result is much higher when compared with the rate of hydrogen production in the sample without co- catalysts about 9.4 times higher after Ru deposition from ethanol aqueous solution. Increasing the production of hydrogen on the Ru/La-NaTaO3 closely related to the decrease in recombination between electron-hole pairs.

Synthesis of GaN:ZnO solid solution by solution combustion method and characterization for photocatalytic application

NASA Astrophysics Data System (ADS)

Menon, Sumithra Sivadas; Anitha, R.; Gupta, Bhavana; Baskar, K.; Singh, Shubra

2016-05-01

GaN-ZnO solid solution has emerged as a successful and reproducible photocatalyst for overall water splitting by one-step photoexcitation, with a bandgap in visible region. When the solid solution is formed, some of the Zn and O ions are replaced by Ga and N ions respectively and there is a narrowing of bandgap which is hypothesized as due to Zn3d-N2p repulsion. The traditional method of synthesis of GaN-ZnO solid solution is by nitridation of the starting oxides under constant ammonia flow. Here we report a solution combustion technique for the synthesis of the solid solution at a temperature about 500 ° C in a muffle furnace with metal nitrates as precursors and urea as the fuel. The as prepared samples showed change in color with the increased concentration of ZnO in the solution. The structural, microstructural, morphological and optical properties of the samples were realized by Powder X ray diffraction, Scanning electron microscopy, Energy dispersive X ray analysis, Transmission electron microscopy and Photoluminescence. Finally the hydrogen production efficiency of the GaN-ZnO nanopowders by water splitting was found, using methanol as a scavenger. The apparent quantum yield (AQY) of 0.048% is obtained for GaN-ZnO solid solution.

High oxygen nanocomposite barrier films based on xylan and nanocrystalline cellulose

Treesearch

Amit Saxena; Thomas J. Elder; Jeffrey Kenvin; Arthur J. Ragauskas

2010-01-01

The goal of this work is to produce nanocomposite film with low oxygen permeability by casting an aqueous solution containing xylan, sorbitol and nanocrystalline cellulose. The morphology of the resulting nanocomposite films was examined by scanning electron microscopy and atomic force microscopy which showed that control films containing xylan and sorbitol had a more...

Effect of mint solution concentration on the absorption spectra of silver nanoparticles in thulium ions presence

NASA Astrophysics Data System (ADS)

Rasmagin, S. I.; Krasovskii, V. I.; Apresyan, L. A.; Novikov, I. K.; Krystob, V. I.; Kazaryan, M. A.

2018-04-01

By the method of green synthesis, silver nanoparticles were obtained in colloidal solutions. The solutions were modified with thulium ions. Using the method of electron microscopy and optical method, the properties of silver nanoparticles obtained are studied. The influence of change in concentration of the solution of mint and thulium ions on the properties of colloidal silver nanoparticles was studied.

Green synthesis and characterization of alginate nanoparticles and its role as a biosorbent for Cr(VI) ions

NASA Astrophysics Data System (ADS)

Geetha, P.; Latha, M. S.; Pillai, Saumya S.; Deepa, B.; Santhosh Kumar, K.; Koshy, Mathew

2016-02-01

Green synthesis of nanoparticles has attained considerable attention in recent years because of its myriad of applications including drug delivery, tissue engineering and water purification. In the present study, alginate nanoparticles stabilized by honey were prepared by cross-linking aqueous solution of alginate with calcium ions. Honey mediated synthesis has been reported earlier for the production of metal nanoparticles. However no literature is available on the use of this technique for polymeric nanoparticles. Highly stable nanoparticles of 10-100 nm size were generated by this technique. The synthesised nanoparticles were characterized by transmission electron microscopy, scanning electron microscopy, atomic force microscopy, dynamic light scattering and Fourier transform infrared spectroscopic techniques. Potential of using these nanoparticles for heavy metal removal was studied by using Cr(VI) from aqueous solution, where a maximum removal efficiency of 93.5% was obtained. This method was also successfully employed for the production of other polymeric nanoparticles like casein, chitosan and albumin.

Worming Their Way into Shape: Toroidal Formations in Micellar Solutions

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

Cardiel Rivera, Joshua J.; Tonggu, Lige; Dohnalkova, Alice

2013-11-01

We report the formation of nanostructured toroidal micellar bundles (nTMB) from a semidilute wormlike micellar solution, evidenced by both cryogenicelectron microscopy and transmission electron microscopy images. Our strategy for creating nTMB involves a two-step protocol consisting of a simple prestraining process followed by flow through a microfluidic device containing an array of microposts, producing strain rates in the wormlike micelles on the order of 105 s^1. In combination with microfluidic confinement, these unusually large strain rates allow for the formation of stable nTMB. Electron microscopy images reveal a variety of nTMB morphologies and provide the size distribution of the nTMB.more » Small-angle neutron scattering indicates the underlying microstructural transition from wormlike micelles to nTMB. We also show that other flow-induced approaches such as sonication can induce and control the emergence of onion-like and nTMB structures, which may provide a useful tool for nanotemplating.« less

Morphology selection for cupric oxide thin films by electrodeposition.

PubMed

Dhanasekaran, V; Mahalingam, T; Chandramohan, R

2011-10-01

Polycrystalline cupric oxide thin films were deposited using alkaline solution bath employing cathodic electrodeposition method. The thin films were electrodeposited at various solution pH. The surface morphology and elemental analyzes of the films were studied using scanning electron microscopy (SEM) and energy dispersive X-ray analysis, respectively. SEM studies revealed that the surface morphology could be tailored suitably by adjusting the pH value during deposition. Mesh average on multiple lattice mode atomic force microscopy image was obtained and reported. Copyright © 2011 Wiley-Liss, Inc.

Retracing in correlative light electron microscopy: where is my object of interest?

PubMed

Hodgson, Lorna; Nam, David; Mantell, Judith; Achim, Alin; Verkade, Paul

2014-01-01

Correlative light electron microscopy (CLEM) combines the strengths of light and electron microscopy in a single experiment. There are many ways to perform a CLEM experiment and a variety of microscopy modalities can be combined either on separate instruments or as completely integrated solutions. In general, however, a CLEM experiment can be divided into three parts: probes, processing, and analysis. Most of the existing technologies are focussed around the development and use of probes or describe processing methodologies that explain or circumvent some of the compromises that need to be made when performing both light and electron microscopy on the same sample. So far, relatively little attention has been paid to the analysis part of CLEM experiments. Although it is an essential part of each CLEM experiment, it is usually a cumbersome manual process. Here, we briefly discuss each of the three above-mentioned steps, with a focus on the analysis part. We will also introduce an automated registration algorithm that can be applied to the analysis stage to enable the accurate registration of LM and EM images. This facilitates tracing back the right cell/object seen in the light microscope in the EM. © 2014 Elsevier Inc. All rights reserved.

Synthesis and characterization of dextran-coated iron oxide nanoparticles

NASA Astrophysics Data System (ADS)

Predescu, Andra Mihaela; Matei, Ecaterina; Berbecaru, Andrei Constantin; Pantilimon, Cristian; Drăgan, Claudia; Vidu, Ruxandra; Predescu, Cristian; Kuncser, Victor

2018-03-01

Synthesis and characterization of iron oxide nanoparticles coated with a large molar weight dextran for environmental applications are reported. The first experiments involved the synthesis of iron oxide nanoparticles which were coated with dextran at different concentrations. The synthesis was performed by a co-precipitation technique, while the coating of iron oxide nanoparticles was carried out in solution. The obtained nanoparticles were characterized by using scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction spectrometry, Fourier transform infrared spectroscopy and superconducting quantum interference device magnetometry. The results demonstrated a successful coating of iron oxide nanoparticles with large molar weight dextran, of which agglomeration tendency depended on the amount of dextran in the coating solution. SEM and TEM observations have shown that the iron oxide nanoparticles are of about 7 nm in size.

Steady-state solution growth of microcrystalline silicon on nanocrystalline seed layers on glass

NASA Astrophysics Data System (ADS)

Bansen, R.; Ehlers, C.; Teubner, Th.; Boeck, T.

2016-09-01

The growth of polycrystalline silicon layers on glass from tin solutions at low temperatures is presented. This approach is based on the steady-state solution growth of Si crystallites on nanocrystalline seed layers, which are prepared in a preceding process step. Scanning electron microscopy and atomic force microscopy investigations reveal details about the seed layer surfaces, which consist of small hillocks, as well as about Sn inclusions and gaps along the glass substrate after solution growth. The successful growth of continuous microcrystalline Si layers with grain sizes up to several ten micrometers shows the feasibility of the process and makes it interesting for photovoltaics. Project supported by the German Research Foundation (DFG) (No. BO 1129/5-1).

Solution-Processible Crystalline NiO Nanoparticles for High-Performance Planar Perovskite Photovoltaic Cells.

PubMed

Kwon, Uisik; Kim, Bong-Gi; Nguyen, Duc Cuong; Park, Jong-Hyeon; Ha, Na Young; Kim, Seung-Joo; Ko, Seung Hwan; Lee, Soonil; Lee, Daeho; Park, Hui Joon

2016-07-28

In this work, we report on solution-based p-i-n-type planar-structured CH3NH3PbI3 perovskite photovoltaic (PV) cells, in which precrystallized NiO nanoparticles (NPs) without post-treatment are used to form a hole transport layer (HTL). X-ray diffraction and high-resolution transmission electron microscopy showed the crystallinity of the NPs, and atomic force microscopy and scanning electron microscopy confirmed the uniform surfaces of the resultant NiO thin film and the subsequent perovskite photoactive layer. Compared to the conventional poly(3,4-ethylenedioxythiophene):poly(styrenesulfonate) ( PSS) HTL, the NiO HTL had excellent energy-level alignment with that of CH3NH3PbI3 and improved electron-blocking capability, as analyzed by photoelectron spectroscopy and diode modeling, resulting in Voc ~0.13 V higher than conventional PSS-based devices. Consequently, a power conversion efficiency (PCE) of 15.4% with a high fill factor (FF, 0.74), short-circuit current density (Jsc, 20.2 mA·cm(-2)), and open circuit voltage (Voc, 1.04 V) having negligible hysteresis and superior air stability has been achieved.

Solution-Processible Crystalline NiO Nanoparticles for High-Performance Planar Perovskite Photovoltaic Cells

PubMed Central

Kwon, Uisik; Kim, Bong-Gi; Nguyen, Duc Cuong; Park, Jong-Hyeon; Ha, Na Young; Kim, Seung-Joo; Ko, Seung Hwan; Lee, Soonil; Lee, Daeho; Park, Hui Joon

2016-01-01

In this work, we report on solution-based p-i-n-type planar-structured CH3NH3PbI3 perovskite photovoltaic (PV) cells, in which precrystallized NiO nanoparticles (NPs) without post-treatment are used to form a hole transport layer (HTL). X-ray diffraction and high-resolution transmission electron microscopy showed the crystallinity of the NPs, and atomic force microscopy and scanning electron microscopy confirmed the uniform surfaces of the resultant NiO thin film and the subsequent perovskite photoactive layer. Compared to the conventional poly(3,4-ethylenedioxythiophene):poly(styrenesulfonate) (PEDOT:PSS) HTL, the NiO HTL had excellent energy-level alignment with that of CH3NH3PbI3 and improved electron-blocking capability, as analyzed by photoelectron spectroscopy and diode modeling, resulting in Voc ~0.13 V higher than conventional PEDOT:PSS-based devices. Consequently, a power conversion efficiency (PCE) of 15.4% with a high fill factor (FF, 0.74), short-circuit current density (Jsc, 20.2 mA·cm−2), and open circuit voltage (Voc, 1.04 V) having negligible hysteresis and superior air stability has been achieved. PMID:27465263

Field-Flow Fractionation of Carbon Nanotubes and Related Materials

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

John P. Selegue

During the grant period, we carried out FFF studies of carbonaceous soot, single-walled and multi-walled carbon nanotubes, carbon nano-onions and polyoxometallates. FFF alone does not provide enough information to fully characterize samples, so our suite of characterization techniques grew to include light scattering (especially Photon Correlation Spectroscopy), scanning and transmission electron microscopy, thermogravimetric analysis and spectroscopic methods. We developed convenient techniques to deposit and examine minute FFF fractions by electron microscopy. In collaboration with Arthur Cammers (University of Kentucky), we used Flow Field-Flow Fractionation (Fl-FFF) to monitor the solution-phase growth of keplerates, a class of polyoxometallate (POM) nanoparticles. We monitoredmore » the evolution of Mo-POM nanostructures over the course of weeks by by using flow field-flow fractionation and corroborated the nanoparticle structures by using transmission electron microscopy (TEM). Total molybdenum in the solution and precipitate phases was monitored by using inductively coupled plasma analyses, and total Mo-POM concentration by following the UV-visible spectra of the solution phase. We observe crystallization-driven formation of (Mo132) keplerate and solution phase-driven evolution of structurally related nanoscopic species (3-60 nm). FFF analyses of other classes of materials were less successful. Attempts to analyze platelets of layered materials, including exfoliated graphite (graphene) and TaS2 and MoS2, were disappointing. We were not able to optimize flow conditions for the layered materials. The metal sulfides react with the aqueous carrier liquid and settle out of suspension quickly because of their high density.« less

Structural defects in GaN revealed by Transmission Electron Microscopy

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

Liliental-Weber, Zuzanna

This paper reviews the various types of structural defects observed by Transmission Electron Microscopy in GaN heteroepitaxial layers grown on foreign substrates and homoepitaxial layers grown on bulk GaN substrates. The structural perfection of these layers is compared to the platelet self-standing crystals grown by High Nitrogen Pressure Solution. Defects in undoped and Mg doped GaN are discussed. Lastly, some models explaining the formation of inversion domains in heavily Mg doped layers that are possible defects responsible for the difficulties of p-doping in GaN are also reviewed.

Structural defects in GaN revealed by Transmission Electron Microscopy

DOE PAGES

Liliental-Weber, Zuzanna

2014-09-08

This paper reviews the various types of structural defects observed by Transmission Electron Microscopy in GaN heteroepitaxial layers grown on foreign substrates and homoepitaxial layers grown on bulk GaN substrates. The structural perfection of these layers is compared to the platelet self-standing crystals grown by High Nitrogen Pressure Solution. Defects in undoped and Mg doped GaN are discussed. Lastly, some models explaining the formation of inversion domains in heavily Mg doped layers that are possible defects responsible for the difficulties of p-doping in GaN are also reviewed.

Three phase crystallography and solute distribution analysis during residual austenite decomposition in tempered nanocrystalline bainitic steels

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

Caballero, F.G.; Yen, Hung-Wei; Australian Centre for Microscopy and Microanalysis, The University of Sydney, NSW 2006

2014-02-15

Interphase carbide precipitation due to austenite decomposition was investigated by high resolution transmission electron microscopy and atom probe tomography in tempered nanostructured bainitic steels. Results showed that cementite (θ) forms by a paraequilibrium transformation mechanism at the bainitic ferrite–austenite interface with a simultaneous three phase crystallographic orientation relationship. - Highlights: • Interphase carbide precipitation due to austenite decomposition • Tempered nanostructured bainitic steels • High resolution transmission electron microscopy and atom probe tomography • Paraequilibrium θ with three phase crystallographic orientation relationship.

Simple synthesis of MoS{sub 2} inorganic fullerene-like nanomaterials from MoS{sub 2} amorphous nanoparticles

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

Chang Lianxia; China Faw Group Corporation R and D Center, Changchun, 130011; Yang Haibin

The amorphous MoS{sub 2} nanoparticles have been synthesized by a simple oxidation-reduction reaction in an aqueous solution. A series of products with different morphologies, such as MoS{sub 2} nanospheres, inorganic fullerene-like nanospheres, nanorods and Mo bended rods, can be obtained by annealing the amorphous MoS{sub 2} nanoparticles under N{sub 2} atmosphere under 400-1200 deg. C. These products have been characterized by X-ray diffraction, field emission scanning electronic microscopy, transmission electron microscopy and high-resolution transmission electron microscopy in detail. The possible transformation mechanism for the structure has been discussed based on the experimental results. In addition, the optical properties of IF-MoS{submore » 2} have also been performed by UV-vis absorption spectroscopy.« less

In vitro corrosion resistance of plasma source ion nitrided austenitic stainless steels.

PubMed

Le, M K; Zhu, X M

2001-04-01

Plasma source ion nitriding has emerged as a low-temperature, low-pressure nitriding approach for low-energy implanting nitrogen ions and then diffusing them into steel and alloy. In this work, a single high nitrogen face-centered-cubic (f.c.c.) phase (gammaN) formed on the 1Cr18Ni9Ti and AISI 316L austenitic stainless steels with a high nitrogen concentration of about 32 at % was characterized using Auger electron spectroscopy, electron probe microanalysis, glancing angle X-ray diffraction, and transmission electron microscopy. The corrosion resistance of the gammaN-phase layer was studied by the electrochemical cyclic polarization measurement in Ringer's solutions buffered to pH from 3.5 to 7.2 at a temperature of 37 degrees C. No pitting corrosion in the Ringer's solutions with pH = 7.2 and 5.5 was detected for the gammaN-phase layers on the two stainless steels. The high pitting potential for the gammaN-phase layers is higher, about 500 and 600 mV, above that of the two original stainless steels, respectively, in the Ringer's solution with pH = 3.5. The corroded surface morphologies of the gammaN-phase layers observed by scanning electron microscopy are consistent with the results of the electrochemical polarization measurement.

Microstructural evolution and magnetic properties of ultrafine solute-atom particles formed in a Cu75-Ni20-Fe5 alloy on isothermal annealing

NASA Astrophysics Data System (ADS)

Kim, Jun-Seop; Takeda, Mahoto; Bae, Dong-Sik

2016-12-01

Microstructural features strongly affect magnetism in nano-granular magnetic materials. In the present work we have investigated the relationship between the magnetic properties and the self-organized microstructure formed in a Cu75-Ni20-Fe5 alloy comprising ferromagnetic elements and copper atoms. High resolution transmission electron microscopy (HRTEM) observations showed that on isothermal annealing at 873 K, nano-scale solute (Fe,Ni)-rich clusters initially formed with a random distribution in the Cu-rich matrix. Superconducting quantum interference device (SQUID) measurements revealed that these ultrafine solute clusters exhibited super-spinglass and superparamagnetic states. On further isothermal annealing the precipitates evolved to cubic or rectangular ferromagnetic particles and aligned along the <100> directions of the copper-rich matrix. Electron energy-band calculations based on the first-principle Korringa-Kohn-Rostocker (KKR) method were also implemented to investigate both the electronic structure and the magnetic properties of the alloy. Inputting compositions obtained experimentally by scanning transmission electron microscopy-electron dispersive X-ray spectroscopy (STEM-EDS) analysis, the KKR calculation confirmed that ferromagnetic precipitates (of moment 1.07μB per atom) formed after annealing for 2 × 104 min. Magneto-thermogravimetric (MTG) analysis determined with high sensitivity the Curie temperatures and magnetic susceptibility above room temperature of samples containing nano-scale ferromagnetic particles.

Immunoactive two-dimensional self-assembly of monoclonal antibodies in aqueous solution revealed by atomic force microscopy

NASA Astrophysics Data System (ADS)

Ido, Shinichiro; Kimiya, Hirokazu; Kobayashi, Kei; Kominami, Hiroaki; Matsushige, Kazumi; Yamada, Hirofumi

2014-03-01

The conformational flexibility of antibodies in solution directly affects their immune function. Namely, the flexible hinge regions of immunoglobulin G (IgG) antibodies are essential in epitope-specific antigen recognition and biological effector function. The antibody structure, which is strongly related to its functions, has been partially revealed by electron microscopy and X-ray crystallography, but only under non-physiological conditions. Here we observed monoclonal IgG antibodies in aqueous solution by high-resolution frequency modulation atomic force microscopy (FM-AFM). We found that monoclonal antibodies self-assemble into hexamers, which form two-dimensional crystals in aqueous solution. Furthermore, by directly observing antibody-antigen interactions using FM-AFM, we revealed that IgG molecules in the crystal retain immunoactivity. As the self-assembled monolayer crystal of antibodies retains immunoactivity at a neutral pH and is functionally stable at a wide range of pH and temperature, the antibody crystal is applicable to new biotechnological platforms for biosensors or bioassays.

Synthesis of GaN:ZnO solid solution by solution combustion method and characterization for photocatalytic application

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

Menon, Sumithra Sivadas; Anitha, R.; Baskar, K.

2016-05-23

GaN-ZnO solid solution has emerged as a successful and reproducible photocatalyst for overall water splitting by one-step photoexcitation, with a bandgap in visible region. When the solid solution is formed, some of the Zn and O ions are replaced by Ga and N ions respectively and there is a narrowing of bandgap which is hypothesized as due to Zn3d-N2p repulsion. The traditional method of synthesis of GaN-ZnO solid solution is by nitridation of the starting oxides under constant ammonia flow. Here we report a solution combustion technique for the synthesis of the solid solution at a temperature about 500 °more » C in a muffle furnace with metal nitrates as precursors and urea as the fuel. The as prepared samples showed change in color with the increased concentration of ZnO in the solution. The structural, microstructural, morphological and optical properties of the samples were realized by Powder X ray diffraction, Scanning electron microscopy, Energy dispersive X ray analysis, Transmission electron microscopy and Photoluminescence. Finally the hydrogen production efficiency of the GaN-ZnO nanopowders by water splitting was found, using methanol as a scavenger. The apparent quantum yield (AQY) of 0.048% is obtained for GaN-ZnO solid solution.« less

Luminescent properties under X-ray excitation of Ba(1-x)PbxWO4 disordered solid solution

NASA Astrophysics Data System (ADS)

Bakiz, B.; Hallaoui, A.; Taoufyq, A.; Benlhachemi, A.; Guinneton, F.; Villain, S.; Ezahri, M.; Valmalette, J.-C.; Arab, M.; Gavarri, J.-R.

2018-02-01

A series of polycrystalline barium-lead tungstate Ba1-xPbxWO4 with 0 ≤ x ≤ 1 was synthesized using a classical solid-state method with thermal treatment at 1000 °C. These materials were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), Fourier Transform Raman (FT-Raman) spectroscopy. X-ray diffraction profile analyses were performed using Rietveld method. These materials crystallized in the scheelite tetragonal structure and behaved as quasi ideal solid solution. Raman spectroscopy confirmed the formation of the solid solution. Structural distortions were evidenced in X-ray diffraction profiles and in vibration Raman spectra. The scanning electron microscopy experiments showed large and rounded irregular grains. Luminescence experiments were performed under X-ray excitation. The luminescence emission profiles have been interpreted in terms of four Gaussian components, with a major contribution of blue emission. The integrated intensity of luminescence reached a maximum value in the composition range x = 0.3-0.6, in relation with distortions of crystal lattice.

Ultrasound-assisted synthesis of CuO nanostructures templated by cotton fibers

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

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

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

Isomorphism and solid solutions among Ag- and Au-selenides

NASA Astrophysics Data System (ADS)

Palyanova, Galina A.; Seryotkin, Yurii V.; Kokh, Konstantin A.; Bakakin, Vladimir V.

2016-09-01

Au-Ag selenides were synthesized by heating stoichiometric mixtures of elementary substances of initial compositions Ag2-xAuxSe with a step of х=0.25 (0≤х≤2) to 1050 °С and annealing at 500 °C. Scanning electron microscopy, optical microscopy, electron microprobe analysis and X-ray powder diffraction methods have been applied to study synthesized samples. Results of studies of synthesized products revealed the existence of three solid solutions with limited isomorphism Ag↔Au: naumannite Ag2Se - Ag1.94Au0.06Se, fischesserite Ag3AuSe2 - Ag3.2Au0.8Se2 and gold selenide AuSe - Au0.94Ag0.06Se. Solid solutions and AgAuSe phases were added to the phase diagram of Ag-Au-Se system. Crystal-chemical interpretation of Ag-Au isomorphism in selenides was made on the basis of structural features of fischesserite, naumannite, and AuSe.

All-printed capacitors with continuous solution dispensing technology

NASA Astrophysics Data System (ADS)

Ge, Yang; Plötner, Matthias; Berndt, Andreas; Kumar, Amit; Voit, Brigitte; Pospiech, Doris; Fischer, Wolf-Joachim

2017-09-01

Printed electronics have been introduced into the commercial markets in recent years. Various printing technologies have emerged aiming to process printed electronic devices with low cost, environmental friendliness, and compatibility with large areas and flexible substrates. The aim of this study is to propose a continuous solution dispensing technology for processing all-printed thin-film capacitors on glass substrates using a leading-edge printing instrument. Among all printing technologies, this study provides concrete proof of the following outstanding advantages of this technology: high tolerance to inks, high throughput, low cost, and precise pattern transfers. Ag nanoparticle ink based on glycol ethers was used to print the electrodes. To obtain dielectric ink, a copolymer powder of poly(methyl methacrylate-co-benzoylphenyl methacrylate) containing crosslinkable side groups was dissolved in anisole. Various layouts were designed to support multiple electronic applications. Scanning electron microscopy and atomic force microscopy were used to investigate the all-printed capacitor layers formed using the proposed process. Additionally, the printed capacitors were electrically characterized under direct current and alternating current. The measured electrical properties of the printed capacitors were consistent with the theoretical results.

In situ transmission electron microscopy of lead dendrites and lead ions in aqueous solution.

PubMed

White, Edward R; Singer, Scott B; Augustyn, Veronica; Hubbard, William A; Mecklenburg, Matthew; Dunn, Bruce; Regan, Brian C

2012-07-24

An ideal technique for observing nanoscale assembly would provide atomic-resolution images of both the products and the reactants in real time. Using a transmission electron microscope we image in situ the electrochemical deposition of lead from an aqueous solution of lead(II) nitrate. Both the lead deposits and the local Pb(2+) concentration can be visualized. Depending on the rate of potential change and the potential history, lead deposits on the cathode in a structurally compact layer or in dendrites. In both cases the deposits can be removed and the process repeated. Asperities that persist through many plating and stripping cycles consistently nucleate larger dendrites. Quantitative digital image analysis reveals excellent correlation between changes in the Pb(2+) concentration, the rate of lead deposition, and the current passed by the electrochemical cell. Real-time electron microscopy of dendritic growth dynamics and the associated local ionic concentrations can provide new insight into the functional electrochemistry of batteries and related energy storage technologies.

Preparation of graphene-ZrO2 nanocomposites by heat treatment and photocatalytic degradation of organic dyes.

PubMed

Cho, Bum Hwi; Ko, Weon Bae

2013-11-01

ZrO2 nanoparticles were synthesized by combining a solution containing zinconyl chloride in distilled water with a NH4OH solution under microwave irradiation. Graphene and ZrO2 nanocomposites were synthesized in an electric furnace at 700 degrees C for 2 hours. The heated graphene-ZrO2 nanocomposites were characterized by X-ray diffraction, scanning electron microscopy and transmission electron microscopy. In addition, UV-vis spectrophotometry was used to evaluate the heated graphene-ZrO2 nanocomposites as a catalyst in the photocatalytic degradation of organic dyes. The photocatalytic effect of the heated graphene-ZrO2 nanocomposites was compared with that of unheated graphene nanoparticles, heated graphene nanoparticles, and unheated graphene-ZrO2 nanocomposites in organic dyes (methylene blue, methyl orange, and rhodamine B) under ultraviolet light at 254 nm.

The adsorption of L-phenylalanine on oxidized single-walled carbon nanotubes.

PubMed

Piao, Lingyu; Liu, Quanrun; Li, Yongdan; Wang, Chen

2009-02-01

A simple and green approach was proceeded to obtain a stable single-walled carbon nanotubes (SWNTs)/L-phenylalanine (Phe) solution. The oxidized SWNTs (OSWNT) were used in this work. The scanning electron microscopy (SEM), High-resolution transmission electron microscopy (HRTEM), Raman spectrometer, Fourier transform-infrared resonance (FT-IR), Ultraviolet-visible (UV-vis) spectroscopy, Thermogravimetric analysis (TGA) and High performance liquid chromatography (HPLC) were joined together to investigate the interaction between OSWNT and Phe. The OSWNT became soluble in the water and formed a stable solution since the Phe was adsorbed. The absorbed amount of Phe on the OSWNT is around 33 wt%. Adsorption of the Phe was mainly carried out on the OSWNT with smaller diameters. The Phe molecules were absorbed on the OSWNT by conjunct interaction of the pi-pi stacking, hydrogen bond and part of covalent bond.

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

Zhao, Donghui; Key Lab of Inorganic Coating Materials, Shanghai Institute of Ceramics, Chinese Academy of Sciences, 1295 Dingxi, Changning, Shanghai 200050; Zhu, Yingchun, E-mail: yzhu@mail.sic.ac.cn

In this article, the polymorph selection of calcium carbonate has been successfully achieved in water-soluble carboxymethyl chitosan aqueous solution at different temperatures (25-95 {sup o}C). Vaterite is formed in carboxymethyl chitosan solution 25 {sup o}C accompanied with trace of calcite, whereas pure aragonite is obtained at 95 {sup o}C. Scanning electron microscopy and transmission electron microscopy analyses show that the products are formed from the recrystallization of nanometer crystallites. Thermodynamic and kinetic analyses reveal that the polymorph of calcium carbonate is controlled and selected by kinetics in various temperatures. As a heterogeneous nucleator and stabilizing agent, carboxymethyl chitosan changes themore » nucleation and growth of calcium carbonate from thermodynamic into kinetic control. Under kinetic limitation, the reaction rate of aragonite increases along with the elevating of temperature and surpasses the rate of vaterite above 327 K.« less

Transmission electron microscopy as a tool for nanocrystal characterization pre- and post-injector

PubMed Central

Stevenson, H. P.; DePonte, D. P.; Makhov, A. M.; Conway, James F.; Zeldin, O. B.; Boutet, S.; Calero, G.; Cohen, A. E.

2014-01-01

Recent advancements at the Linac Coherent Light Source X-ray free-electron laser (XFEL) enabling successful serial femtosecond diffraction experiments using nanometre-sized crystals (NCs) have opened up the possibility of X-ray structure determination of proteins that produce only submicrometre crystals such as many membrane proteins. Careful crystal pre-characterization including compatibility testing of the sample delivery method is essential to ensure efficient use of the limited beamtime available at XFEL sources. This work demonstrates the utility of transmission electron microscopy for detecting and evaluating NCs within the carrier solutions of liquid injectors. The diffraction quality of these crystals may be assessed by examining the crystal lattice and by calculating the fast Fourier transform of the image. Injector reservoir solutions, as well as solutions collected post-injection, were evaluated for three types of protein NCs (i) the membrane protein PTHR1, (ii) the multi-protein complex Pol II-GFP and (iii) the soluble protein lysozyme. Our results indicate that the concentration and diffraction quality of NCs, particularly those with high solvent content and sensitivity to mechanical manipulation may be affected by the delivery process. PMID:24914151

Effect of pre-strain on precipitation and exfoliation corrosion resistance in an Al-Zn-Mg alloy

NASA Astrophysics Data System (ADS)

Lu, Xianghan; Du, Zhiwei; Han, Xiaolei; Li, Ting; Wang, Guojun; Lu, Liying; Bai, Xiaoxia; Zhou, Tietao

2017-12-01

To investigate the effect of pre-strain on behaviors in a specially developed Al-4.5Zn-1.2Mg alloy, transmission electron microscopy (TEM) bright field (BF) imaging combined with select area electron diffraction (SAED), Vickers-hardness tests and electrical conductivity tests was conducted for insight into precipitation in aluminum (Al) matrix during two step ageing, and standard exfoliation corrosion (EXCO) test combined with high-angle angular dark field scanning transmission electron microscopy (HAADF-STEM) and scanning electron microscopy (SEM) was carried out for corrosion behavior. Results showed that pre-strain accelerated precipitation during two step ageing as the sequence of: (i) supersaturated solid solution (SSS), GPI zones precipitations, GPI dissolution; (ii) SSS, fcc precipitates, η’ phases or η phases. And the precipitation hardening of the fcc precipitates was not effective as GPI zones. Pre-strain also accelerated EXCO developing, which was mainly attributed to the coverage ratio of η phases on high-angle grain boundaries (HAGBs) increasing as pre-strain increase.

CMC-coated Fe3O4 nanoparticles as new MRI probes for hepatocellular carcinoma

NASA Astrophysics Data System (ADS)

Sitthichai, Sudarat; Pilapong, Chalermchai; Thongtem, Titipun; Thongtem, Somchai

2015-11-01

Pure Fe3O4 nanoparticles and Fe3O4 magnetic nanoparticles (MNPs) coated with carboxymethyl cellulose (CMC) were successfully prepared by co-precipitating of FeCl2·4H2O and FeCl3·6H2O in the solutions containing ammonia at 80 °C for 3 h. Phase, morphology, particle-sized distribution, surface chemistry, and weight loss were characterized by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM), transmission electron microscopy (TEM) including high-resolution transmission electron microscopy (HRTEM) and selected area electron diffraction (SAED), thermogravimetric analysis (TGA), and Fourier transform infrared (FTIR) spectroscopy. In this research, CMC-coated Fe3O4 MNPs consisting of Fe2+ and Fe3+ ions with 543.3-mM-1 s-1 high relaxivity were detected and were able to be used for magnetic resonance imaging (MRI) application with very good contrast for targeting hepatocellular carcinoma (HCC) without any further vectorization.

A Thin Film Nanocomposite Membrane with MCM-41 Silica Nanoparticles for Brackish Water Purification.

PubMed

Kadhom, Mohammed; Yin, Jun; Deng, Baolin

2016-12-06

Thin film nanocomposite (TFN) membranes containing MCM-41 silica nanoparticles (NPs) were synthesized by the interfacial polymerization (IP) process. An m -phenylenediamine (MPD) aqueous solution and an organic phase with trimesoyl chloride (TMC) dissolved in isooctane were used in the IP reaction, occurring on a nanoporous polysulfone (PSU) support layer. Isooctane was introduced as the organic solvent for TMC in this work due to its intermediate boiling point. MCM-41 silica NPs were loaded in MPD and TMC solutions in separate experiments, in a concentration range from 0 to 0.04 wt %, and the membrane performance was assessed and compared based on salt rejection and water flux. The prepared membranes were characterized via scanning electron microscopy (SEM), transmission electron microscopy (TEM), contact angle measurement, and attenuated total reflection Fourier transform infrared (ATR FT-IR) analysis. The results show that adding MCM-41 silica NPs into an MPD solution yields slightly improved and more stable results than adding them to a TMC solution. With 0.02% MCM-41 silica NPs in the MPD solution, the water flux was increased from 44.0 to 64.1 L/m²·h, while the rejection virtually remained the same at 95% (2000 ppm NaCl saline solution, 25 °C, 2068 kPa (300 psi)).

Catalyst free growth of CNTs by CVD on nanoscale rough surfaces of silicon substrates

NASA Astrophysics Data System (ADS)

Damodar, D.; Sahoo, R. K.; Jacob, C.

2013-06-01

Catalyst free growth of carbon nanotubes (CNT) has been achieved using atmospheric pressure chemical vapor deposition (APCVD) on surface modified Si(111) substrates. The effect of the substrate surface has been observed by partially etching with KOH (potassium hydroxide) solution which is an anisotropic etchant. Scanning electron microscopy (SEM) confirmed the formation of CNTs over most of the area of the substrate where substrates were anisotropically etched. Transmission electron microscopy (TEM) was used to observe the internal structure of the CNTs. Raman spectroscopy further confirmed the formation of the carbon nanostructures and also their graphitic crystallinity.

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

Zou, Lianfeng; Li, Jonathan; Zakharov, Dmitri

Using in situ transmission electron microscopy that spatially and temporally resolves the evolution of the atomic structure in the surface and subsurface regions, we Find that the surface segregation of Au atoms in a Cu(Au) solid solution results in the nucleation and growth of a (2 × 1) missing-row reconstructed, half-unit-cell thick L1 2 Cu 3Au(110) surface alloy. Our in situ electron microscopy observations and atomistic simulations demonstrate that the (2 × 1) reconstruction of the Cu 3Au(110) surface alloy remains as a stable surface structure as a result of the favored Cu-Au diatom configuration.

Ag-doped TiO2 hollow microspheres with visible light response by template-free route for removal of tetracycline hydrochloride from aqueous solution

NASA Astrophysics Data System (ADS)

Zhang, Jian; Li, Xuanhua; Peng, Meiling; Tang, Yuanyuan; Ke, Anqi; Gan, Wei; Fu, Xucheng; Hao, Hequn

2018-06-01

In this study, Ag-doped TiO2 hollow microspheres were synthesized by a template-free route, and their photocatalytic performance and catalytic mechanism were investigated. The hollow microspheres were characterized by x-ray diffraction, scanning electron microscopy, transmission electron microscopy, x-ray photoelectron spectroscopy and UV–vis spectroscopy. Ag-doped hollow TiO2 microspheres exhibited excellent photocatalytic performance for tetracycline hydrochloride (TC) in water. TC degradation follows pseudo first-order kinetics, and hydroxyl radical (OH·) and holes (h+) were active substances in the photocatalytic reaction.

Freeze drying vs microwave drying-methods for synthesis of sinteractive thoria powders

NASA Astrophysics Data System (ADS)

Annie, D.; Chandramouli, V.; Anthonysamy, S.; Ghosh, Chanchal; Divakar, R.

2017-02-01

Thoria powders were synthesized by oxalate precipitation from an aqueous solution of the nitrate. The filtered precipitates were freeze dried or microwave dried before being calcined at 1073 K. The thoria powders obtained were characterized for crystallite size, specific surface area, bulk density, particle size distribution and residual carbon. Microstructure of the product was studied using scanning electron microscopy (SEM) and transmission electron microscopy (TEM). Sinterability of the synthesized powders was studied by measuring the density of the sintered compacts. Powders that can be consolidated and sintered to densities ∼96% theoretical density (TD) at 1773 K were obtained.

Preparation of porous palladium nanowire arrays and their catalytic performance for hydrogen peroxide electroreduction in acid medium

NASA Astrophysics Data System (ADS)

Wang, Xin; Ye, Ke; Gao, Yinyi; Zhang, Hongyu; Cheng, Kui; Xiao, Xue; Wang, Guiling; Cao, Dianxue

2016-01-01

Nanoporous palladium supported on the carbon coated titanium carbide (C@TiC) nanowire arrays (Pd NP/C@TiC) are successfully prepared by a facile chemical vapor deposition of three-dimensional (3D) C@TiC substrate, followed by electrochemical codeposition of Pd-Ni and removal of Ni via dealloying. The structure and morphology of the obtained Pd NP/C@TiC electrodes are characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDX), field-emission scanning electron microscopy (FESEM) and transmission electron microscopy (TEM). Cyclic voltammetry (CV), linear sweep voltammetry (LSV), chronoamperometry (CA) and electrochemical impedance spectroscopy (EIS) are used to examine the catalytic performances of the electrodes for H2O2 electroreduction in H2SO4 solution. The Pd NP/C@TiC electrode exhibits a largely effective specific surface area owing to its open nanoporous structure allowing the full utilization of Pd surface active sites. At the potential of 0.2 V in 2.0 mol L-1 H2O2 and 2 mol L-1 H2SO4 solutions, the reduction current density reaches 3.47 A mg-1, which is significantly higher than the catalytic activity of H2O2 electroreduction achieved previously with precious metals as catalysts.

Solution-Based Synthesis of Crystalline Silicon from Liquid Silane through Laser and Chemical Annealing

DOE PAGES

Iyer, Ganjigunte R. S.; Hobbie, Erik K.; Guruvenket, Srinivasan; ...

2012-05-23

We report a solution process for the synthesis of crystalline silicon from the liquid silane precursor cyclohexasilane (Si 6H 12). Polysilane films were crystallized through thermal and laser annealing, with plasma hydrogenation at atmospheric pressure generating further structural changes in the films. The evolution from amorphous to microcrystalline is characterized using scanning electron microscopy (SEM), atomic force microscopy (AFM), Raman spectroscopy and impedance spectroscopy. A four-decade enhancement in the electrical conductivity is attributed to a disorder-order transition in a bonded Si network. Lastly, our results demonstrate a potentially attractive approach that employs a solution process coupled with ambient post-processing tomore » produce crystalline silicon thin films.« less

Synthesis of camptothecin-loaded gold nanomaterials

NASA Astrophysics Data System (ADS)

Xing, Zhimin; Liu, Zhiguo; Zu, Yuangang; Fu, Yujie; Zhao, Chunjian; Zhao, Xiuhua; Meng, Ronghua; Tan, Shengnan

2010-04-01

Camptothecin-loaded gold nanomaterials have been synthesized by the sodium borohydride reduction method under a strong basic condition. The obtained gold nanomaterials have been characterized by transmission electron microscopy (TEM), atomic force microscopy (AFM) and UV-vis absorption spectroscopy. The camptothecin-loaded gold colloidal solution was very stable and can be stored for more than two months at room temperature without obvious changes. The color of the colloidal solution can change from wine red to purple and blue during the acidifying process. It was revealed that the release of camptothecin and the aggregation of gold nanoparticles can be controlled by tuning the solution pH. The present study implied that the gold nanomaterials can be used as the potential carrier for CPT delivery.

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

NASA Astrophysics Data System (ADS)

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

2015-10-01

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

Effects of Piper cubeba L. essential oil on methicillin-resistant Staphylococcus aureus: an AFM and TEM study.

PubMed

Alharbi, Naiyf S; Khaled, Jamal M; Alzaharni, Khalid E; Mothana, Ramzi A; Alsaid, Mansour S; Alhoshan, Mansour; Dass, Lawrence Arockiasamy; Kadaikunnan, Shine; Alobaidi, Ahmed S

2017-01-01

The increasing prevalence of antibiotic-resistant bacteria is creating a real challenge for health care systems worldwide, making the development of novel antibiotics a necessity. In addition to the development of new antibiotics, there is an urgent need for in-depth characterization of the mechanisms of bacterial resistance toward new drugs. Here, we used essential oils extracted in our laboratory from Piper cubeba against methicillin-resistant Staphylococcus aureus ATCC 43300, one of the most prominent antibiotic-resistant bacteria. Effects of the essential oils extracted from P cubeba on bacteria were mainly evaluated using 2 powerful microscopy techniques: atomic force microscopy and transmission electron microscopy. High-resolution atomic force microscopy images of the cells were obtained close to their native environment by immobilizing the cells on porous Polyether sulfone membranes, which were prepared in our laboratory with a wide range and distribution of pore sizes and depth. Inhibition zones (mm) and minimum inhibitory concentrations were determined. Two different concentrations of the oil were used to treat the cells: 50 μg/mL minimum inhibitory concentration and 25 μg/mL. The 50 μg/mL oil solution caused severe damage to the bacterial cells at microscopic levels while the 25 μg/mL solution showed no effects compared to the control. However, at nanoscopic levels, the 25 μg/mL oil solution caused significant changes in the cell wall, which could potentially impair bacterial activities. These results were also confirmed by transmission electron microscopy micrographs. Our results indicate that the extract has a good biological activity against methicillin- and oxacillin-resistant S aureus and that it acts on the cell wall and plasma (cytoplasmic) membrane. Copyright © 2016 John Wiley & Sons, Ltd.

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

NASA Astrophysics Data System (ADS)

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

2017-08-01

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

A novel cetyltrimethyl ammonium silver bromide complex and silver bromide nanoparticles obtained by the surfactant counterion.

PubMed

Liu, Xian-Hao; Luo, Xiao-Hong; Lu, Shu-Xia; Zhang, Jing-Chang; Cao, Wei-Liang

2007-03-01

A novel cetyltrimethyl ammonium silver bromide (CTASB) complex has been prepared simply through the reaction of silver nitrate with cetyltrimethyl ammonium bromide (CTAB) in aqueous solution at room temperature by controlling the concentration of CTAB and the molar ratio of CTAB to silver nitrate in the reaction solution, in which halogen in CTAB is used as surfactant counterion. The structure and thermal behavior of cetyltrimethyl ammonium silver bromide have been investigated by using X-ray diffraction (XRD), infrared spectroscopy (IR), X-ray photoelectron spectroscopy (XPS), UV/vis spectroscopy, thermal analysis (TG-DTA), transmission electron microscopy (TEM), and scanning electron microscopy (SEM). The results show that the complex possesses a metastable layered structure. Upon heating the CTASB aqueous dispersion to above 80 degrees C, the structure change of the complex took place and CTAB-capped nanosized silver bromide particles further formed.

Potential of using multiscale kenaf fibers as reinforcing filler in cassava starch-kenaf biocomposites.

PubMed

Zainuddin, Siti Yasmine Zanariah; Ahmad, Ishak; Kargarzadeh, Hanieh; Abdullah, Ibrahim; Dufresne, Alain

2013-02-15

Biodegradable materials made from cassava starch and kenaf fibers were prepared using a solution casting method. Kenaf fibers were treated with NaOH, bleached with sodium chlorite and acetic buffer solution, and subsequently acid hydrolyzed to obtain cellulose nanocrystals (CNCs). Biocomposites in the form of films were prepared by mixing starch and glycerol/sorbitol with various filler compositions (0-10 wt%). X-ray diffraction revealed that fiber crystallinity increased after each stage of treatment. Morphological observations and size reductions of the extracted cellulose and CNCs were studied using field emission scanning electron microscopy and transmission electron microscopy. The effects of different treatments and filler contents of the biocomposites were evaluated through mechanical tests. Results showed that the tensile strengths and moduli of the biocomposites increased after each treatment and the optimum filler content was 6%. Copyright © 2012 Elsevier Ltd. All rights reserved.

Electrical relaxation, optical and magnetic studies of nanocrystalline lithium ferrite synthesized by different chemical routes

NASA Astrophysics Data System (ADS)

Cheruku, Rajesh; Govindaraj, G.; Vijayan, Lakshmi

2017-12-01

The nanocrystalline lithium ferrite was synthesized by wet chemical methods such as solution combustion technique, sol-gel, and hydrothermal for a comparative study. Different characterization techniques like x-ray powder diffraction and thermal analysis were employed to confirm the structure and phase. Temperature-dependent Raman analysis was employed to classify the phonon modes associated with precise atomic motions existing in the synthesized materials. Morphology of sample surface was explored by scanning electron microscopy, and elemental analysis was done by energy dispersive spectroscopy analysis. The nanocrystalline nature of the materials was confirmed through transmission electron microscopy. Magnetic properties of these samples were explored through a vibrating sample magnetometer. Ac electrical impedance spectroscopy data were investigated using two Cole-Cole functions, and activation energies were calculated for all materials. Among them, solution combustion prepared lithium ferrite shows the highest conductivity and lowest activation energy.

Nano-crystalline hydroxyapatite bio-mineral for the treatment of strontium from aqueous solutions.

PubMed

Handley-Sidhu, Stephanie; Renshaw, Joanna C; Yong, Ping; Kerley, Robert; Macaskie, Lynne E

2011-01-01

Hydroxyapatites were analysed using electron microscopy, X-ray diffraction (XRD) and X-ray fluorescence (XRF) analysis. Examination of a bacterially produced hydroxyapatite (Bio-HA) by scanning electron microscopy showed agglomerated nano-sized particles; XRD analysis confirmed that the Bio-HA was hydroxyapatite, with an organic matter content of 7.6%; XRF analysis gave a Ca/P ratio of 1.55, also indicative of HA. The size of the Bio-HA crystals was calculated as ~25 nm from XRD data using the Scherrer equation, whereas Comm-HA powder size was measured as ≤ 50 μm. The nano-crystalline Bio-HA was ~7 times more efficient in removing Sr(2+) from synthetic groundwater than Comm-HA. Dissolution of HA as indicated by the release of phosphate into the solution phase was higher in the Comm-HA than the Bio-HA, indicating a more stable biomaterial which has a potential for the remediation of contaminated sites.

Preparation, characterization and photocatalytic behavior of WO3-fullerene/TiO2 catalysts under visible light

PubMed Central

2011-01-01

WO3-treated fullerene/TiO2 composites (WO3-fullerene/TiO2) were prepared using a sol-gel method. The composite obtained was characterized by BET surface area measurements, X-ray diffraction, scanning electron microscopy, energy dispersive X-ray analysis, transmission electron microscopy, and UV-vis analysis. A methyl orange (MO) solution under visible light irradiation was used to determine the photocatalytic activity. Excellent photocatalytic degradation of a MO solution was observed using the WO3-fullerene, fullerene-TiO2, and WO3-fullerene/TiO2 composites under visible light. An increase in photocatalytic activity was observed, and WO3-fullerene/TiO2 has the best photocatalytic activity; it may attribute to the increase of the photo-absorption effect by the fullerene and the cooperative effect of the WO3. PMID:21774800

Facile approach to prepare Pt decorated SWNT/graphene hybrid catalytic ink

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

Mayavan, Sundar, E-mail: sundarmayavan@cecri.res.in; Department of Nuclear and Quantum Engineering, Korea Advanced Institute of Science and Technology, Daejeon, 305-701; Mandalam, Aditya

Highlights: • Pt NPs were in situ synthesized onto CNT–graphene support in aqueous solution. • The as-prepared material was used directly as a catalyst ink without further treatment. • Catalyst ink is active toward methanol oxidation. • This approach realizes both scalable and greener production of hybrid catalysts. - Abstract: Platinum nanoparticles were in situ synthesized onto hybrid support involving graphene and single walled carbon nanotube in aqueous solution. We investigate the reduction of graphene oxide, and platinum nanoparticle functionalization on hybrid support by X-ray photoelectron spectroscopy, Raman spectroscopy, X-ray diffraction, scanning electron microscopy and transmission electron microscopy. The as-preparedmore » platinum on hybrid support was used directly as a catalyst ink without further treatment and is active toward methanol oxidation. This work realizes both scalable and greener production of highly efficient hybrid catalysts, and would be valuable for practical applications of graphene based fuel cell catalysts.« less

Reactive Brazing of Carbon-Carbon Composites to Titanium

NASA Technical Reports Server (NTRS)

Shpargel, Tarah; Singh, M.; Morscher, Gregory; Asthana, Rajiv

2004-01-01

The Ti-metal/C-C composite joints were formed by reactive brazing with three commercial brazes, namely, Cu-ABA, TiCuNi, and TiCuSil. The joint microstructures were examined using optical microscopy, and scanning electron microscopy (SEM) coupled with energy dispersive spectrometry (EDS). The results of the microstructure analysis indicate solute redistribution across the joint and possible metallurgical bond formation via interdiffusion, which led to good wetting and spreading.

Active Metal Brazing of Carbon-Carbon Composites to Titanium

NASA Technical Reports Server (NTRS)

Singh, M.; Shpargel, T. P.; Morscher, G.; Asthana, R.

2004-01-01

The Ti-metal/C-C composite joints were formed by reactive brazing with three commercial brazes, namely, Cu-ABA, TiCuNi, and TiCuSil. The joint microstructures were examined using optical microscopy, and scanning electron microscopy (SEM) coupled with energy dispersive spectrometry (EDS). The results of the microstructure analysis indicate solute redistribution across the joint which led to good wetting, spreading, and metallurgical bond formation via interdiffusion.

Magnetic whiskers of p-aminobenzoic acid and their use for preparation of filled and microchannel silicone rubbers

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

Semenov, V. V., E-mail: vvsemenov@iomc.ras.ru; Loginova, V. V.; Zolotareva, N. V.

A thin cobalt layer has been formed on the surface of p-aminobenzoic acid whiskers by chemical vapor deposition (CVD). The metallized crystals have been oriented in liquid polydimethylsiloxane rubber by applying a dc magnetic field. After vulcanization, the filler has been removed by processing in an alcohol solution of trifluoroacetic acid. The cobalt deposition on the surface of the organic compound and the properties of metallized whiskers are investigated by optical microscopy, scanning electron microscopy (SEM), and atomic force microscopy (AFM).

Cephradine as corrosion inhibitor for copper in 0.9% NaCl solution

NASA Astrophysics Data System (ADS)

Tasić, Žaklina Z.; Petrović Mihajlović, Marija B.; Radovanović, Milan B.; Simonović, Ana T.; Antonijević, Milan M.

2018-05-01

The effect of (6R,7R)-7-[[(2R)-2-amino-2-cyclohexa-1,4-dien-1-ylacetyl]amino]-3-methyl-8-oxo-5-thia-1-azobicyclo[4.2.0]oct-2-ene-2-carboxylic acid (cephradine) on corrosion behavior of copper in 0.9% NaCl solution was investigated. The electrochemical methods including the open circuit potential measurements, potentiodynamic polarization and electrochemical impedance spectroscopy measurements, scanning electron microscopy with energy dispersive X-ray spectroscopy and quantum chemical calculations were used for this investigation. According to the results obtained by potentiodynamic polarization, cephradine acts as mixed type inhibitor. Also, the results obtained by electrochemical impedance spectroscopy indicate that cephradine provides good copper protection in 0.9% NaCl solution. The inhibition efficiency of cephradine increases with increasing its concentration. The scanning electron microscopy with energy dispersive X-ray spectroscopy confirms that a protective layer is formed on the copper surface due to the adsorption of cephradine on the active sites on the copper surface. Adsorption of cephradine in 0.9% NaCl solution follows the Langmuir adsorption isotherm. Quantum chemical calculations are in agreement with results obtained by electrochemical measurements.

Conversion of borate-based glass scaffold to hydroxyapatite in a dilute phosphate solution.

PubMed

Liu, Xin; Pan, Haobo; Fu, Hailuo; Fu, Qiang; Rahaman, Mohamed N; Huang, Wenhai

2010-02-01

Porous scaffolds of a borate-based glass (composition in mol%: 6Na2O, 8K2O, 8MgO, 22CaO, 36B2O3, 18SiO2, 2P2O5), with interconnected porosity of approximately 70% and pores of size 200-500 microm, were prepared by a polymer foam replication technique. The degradation of the scaffolds and conversion to a hydroxyapatite-type material in a 0.02 M K2HPO4 solution (starting pH = 7.0) at 37 degrees C were studied by measuring the weight loss of the scaffolds, as well as the pH and the boron concentration of the solution. X-ray diffraction, scanning electronic microscopy and energy dispersive x-ray analysis showed that a hydroxyapatite-type material was formed on the glass surface within 7 days of immersion in the phosphate solution. Cellular response to the scaffolds was assessed using murine MLO-A5 cells, an osteogenic cell line. Scanning electron microscopy showed that the scaffolds supported cell attachment and proliferation during the 6 day incubation. The results indicate that this borate-based glass could provide a promising degradable scaffold material for bone tissue engineering applications.

Oral astringent stimuli alter the enamel pellicle's ultrastructure as revealed by electron microscopy.

PubMed

Rehage, Melanie; Delius, Judith; Hofmann, Thomas; Hannig, Matthias

2017-08-01

This electron microscopic study aimed at investigating effects of oral astringent stimuli on the enamel pellicle's morphology. Pellicles were formed in situ within 30min on bovine enamel slabs, fixed to individuals' upper jaw splints. The pellicle-coated specimens were immersed in vitro in seven diverse astringent solutions and subsequently analyzed by scanning electron microscopy (SEM), energy dispersive X-ray (EDX) spectroscopy, as well as transmission electron microscopy (TEM). Four biocompatible astringents, namely the polyphenol epigallocatechin gallate, the metal salt iron(III) sulfate, the basic protein lysozyme, and the aminopolysaccharide chitosan, were additionally applied in situ. After rinsing the oral cavity with these compounds, the pellicle's ultrastructure was imaged by SEM and TEM, respectively. Untreated pellicle samples served as controls. Exposure to polyphenols and lysozyme induced particularly thicker and electron-denser pellicles in comparison to the control pellicle with similar characteristics in vitro and in situ. In contrast, acidic chitosan and metal salt solutions, respectively, revealed minor pellicle alterations. The incorporation of Fe and Al into the pellicles treated with the corresponding inorganic salts was verified by EDX analysis. Astringent-induced pellicle modifications were for the first time visualized by TEM. The ultrastructural alterations of the dental pellicle may partly explain the tooth-roughening effect caused by oral astringent stimuli. Astringents might modify the pellicle's protective properties against dental erosion, attrition, as well as bacterial adhesion, and by this means may influence tooth health. The findings may thus be particularly relevant for preventive dentistry. Copyright © 2017 Elsevier Ltd. All rights reserved.

A facile synthesis of Zn(x)Cd(1-x)S/CNTs nanocomposite photocatalyst for H2 production.

PubMed

Wang, Lei; Yao, Zhongping; Jia, Fangzhou; Chen, Bin; Jiang, Zhaohua

2013-07-21

The sulfide solid solution has become a promising and important visible-light-responsive photocatalyst for hydrogen production nowadays. Zn(x)Cd(1-x)S/CNT nanocomposites were synthesized to improve the dispersion, adjust the energy band gap, and enhance the separation of the photogenerated electrons and holes. The as-prepared photocatalysts were characterized by scanning electron-microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS) and UV-visible diffuse reflectance spectra (UV-visible), respectively. And the effects of CNTs on structure, composition and optical absorption property of the sulfide solid solutions were investigated along with their inherent relationships. For Zn0.83Cd0.17S/CNTs, sulfide solid solution is assembled along the CNTs orderly, with a diameter of 100 nm or so. XPS analysis shows that there is bonding effect between the solid solutions and the CNTs due to the strong adsorption of Zn(2+) and Cd(2+) on the surface of CNTs. There are two obvious absorption edges for Zn0.83Cd0.17S/CNTs, corresponding to two kinds of sulfide solid solutions with different molar ratios of Zn/Cd. The hybridization of solid solutions with CNTs makes the absorption spectrum red shift. The photocatalytic property was evaluated by splitting Na2S + Na2SO3 solution into H2, and the highest rate of H2 evolution of 6.03 mmol h(-1) g(-1) was achieved over Zn0.83Cd0.17S/CNTs. The high activity of photocatalytic H2 production is attributed to the following factors: (1) the optimum band gap and a moderate position of the conduction band (which needs to match the irradiation spectrum of the Xe lamp best), (2) the efficient separation of photogenerated electrons and holes by hybridization, and (3) the improvement of the dispersion of nanocomposites by assembling along the CNTs as well.

Directly Observing Micelle Fusion and Growth in Solution by Liquid-Cell Transmission Electron Microscopy

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

Parent, Lucas R.; Bakalis, Evangelos; Ramírez-Hernández, Abelardo

Amphiphilic small molecules and polymers form commonplace nanoscale macromolecular compartments and bilayers, and as such are truly essential components in all cells and in many cellular processes. The nature of these architectures, including their formation, phase changes, and stimuli-response behaviors, is necessary for the most basic functions of life, and over the past half-century, these natural micellar structures have inspired a vast diversity of industrial products, from biomedicines to detergents, lubricants, and coatings. The importance of these materials and their ubiquity have made them the subject of intense investigation regarding their nanoscale dynamics with increasing interest in obtaining sufficient temporalmore » and spatial resolution to directly observe nanoscale processes. However, the vast majority of experimental methods involve either bulk-averaging techniques including light, neutron, and X-ray scattering, or are static in nature including even the most advanced cryogenic transmission electron microscopy techniques. Here, we employ in situ liquid-cell transmission electron microscopy (LCTEM) to directly observe the evolution of individual amphiphilic block copolymer micellar nanoparticles in solution, in real time with nanometer spatial resolution. These observations, made on a proof-of-concept bioconjugate polymer amphiphile, revealed growth and evolution occurring by unimer addition processes and by particle-particle collision-and-fusion events. The experimental approach, combining direct LCTEM observation, quantitative analysis of LCTEM data, and correlated in silico simulations, provides a unique view of solvated soft matter nanoassemblies as they morph and evolve in time and space, enabling us to capture these phenomena in solution.« less

Chemical synthesis of oriented ferromagnetic LaSr-2 × 4 manganese oxide molecular sieve nanowires

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

Carretero-Genevrier, Adrián; Gazquez, Jaume; Magen, Cesar

2012-04-25

Here we report a chemical solution based method using nanoporous track-etched polymer templates for producing long and oriented LaSr-2 × 4 manganese oxide molecular sieve nanowires. Scanning transmission electron microscopy and electron energy loss spectroscopy analyses show that the nanowires are ferromagnetic at room temperature, single crystalline, epitaxially grown and self-aligned.

A post Gurney quantum mechanical perspective on the electrolysis of water: ion neutralization in solution

NASA Astrophysics Data System (ADS)

Guo, Enyi; McKenzie, David R.

2017-11-01

Electron fluxes crossing the interface between a metallic conductor and an aqueous environment are important in many fields; hydrogen production, environmental scanning tunnelling microscopy, scanning electrochemical microscopy being some of them. Gurney (Gurney 1931 Proc. R. Soc. Lond. 134, 137 (doi:10.1098/rspa.1931.0187)) provided in 1931 a scheme for tunnelling during electrolysis and outlined conditions for it to occur. We measure the low-voltage current flows between gold electrodes in pure water and use the time-dependent behaviour at voltage switch-on and switch-off to evaluate the relative contribution to the steady current arising from tunnelling of electrons between the electrodes and ions in solution and from the neutralization of ions adsorbed onto the electrode surface. We ascribe the larger current contribution to quantum tunnelling of electrons to and from ions in solution near the electrodes. We refine Gurney's barrier scheme to include solvated electron states and quantify energy differences using updated information. We show that Gurney's conditions would prevent the current flow at low voltages we observe but outline how the ideas of Marcus (Marcus 1956 J. Chem. Phys. 24, 966-978 (doi:10.1063/1.1742723)) concerning solvation fluctuations enable the condition to be relaxed. We derive an average barrier tunnelling model and a multiple pathways tunnelling model and compare predictions with measurements of the steady-state current-voltage relation. The tunnelling barrier was found to be wide and low in agreement with other experimental studies. Applications as a biosensing mechanism are discussed that exploit the fast tunnelling pathways along molecules in solution.

Monetite formed in mixed solvents of water and ethylene glycol and its transformation to hydroxyapatite.

PubMed

Ma, Ming-Guo; Zhu, Ying-Jie; Chang, Jiang

2006-07-27

Agglomerated nanorods of hydroxyapatite have been synthesized using monetite as a precursor in a NaOH solution. Monetite consisting of nanosheets has been successfully synthesized by a one-step microwave-assisted method using CaCl(2).2.5H(2)O, NaH(2)PO(4), and sodium dodecyl sulfate (SDS) in water/ethylene glycol (EG) mixed solvents. The effects of the molar ratio of water to EG and the reaction time on the products were investigated. The products were characterized by X-ray powder diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and Fourier transform infrared spectrometry (FTIR).

Atomically Visualizing Elemental Segregation-Induced Surface Alloying and Restructuring

DOE PAGES

Zou, Lianfeng; Li, Jonathan; Zakharov, Dmitri; ...

2017-12-01

Using in situ transmission electron microscopy that spatially and temporally resolves the evolution of the atomic structure in the surface and subsurface regions, we Find that the surface segregation of Au atoms in a Cu(Au) solid solution results in the nucleation and growth of a (2 × 1) missing-row reconstructed, half-unit-cell thick L1 2 Cu 3Au(110) surface alloy. Our in situ electron microscopy observations and atomistic simulations demonstrate that the (2 × 1) reconstruction of the Cu 3Au(110) surface alloy remains as a stable surface structure as a result of the favored Cu-Au diatom configuration.

Corrosion behavior of surface films on boron-implanted high purity iron and stainless steels

NASA Technical Reports Server (NTRS)

Kim, H. J.; Carter, W. B.; Hochman, R. F.; Meletis, E. I.

1985-01-01

Boron (dose, 2 x 10 to the 17th ions/sq cm) was implanted into high purity iron, AISI 316 austenitic stainless steel, and AISI 440C martensitic stainless steel, at 40 keV. The film structure of implanted samples was examined and characterized by contrast and diffraction analyses utilizing transmission electron microscopy. The effect of B(+) ion implantation on the corrosion behavior was studied using the potentiodynamic polarization technique. Tests were performed in deaerated 1 N H2SO4 and 0.1 M NaCl solutions. Scanning electron microscopy was used to examine the morphology of the corroded surfaces after testing.

Electrochemical Deposition of Niobium onto the Surface of Copper Using a Novel Choline Chloride-Based Ionic Liquid

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

Wixtroma, Alex I.; Buhlera, Jessica E.; Reece, Charles E.

2013-06-01

Recent research has shown that choline chloride-based solutions can be used to replace acid-based electrochemical polishing solutions. In this study niobium metal was successfully deposited on the surface of copper substrate via electrochemical deposition using a novel choline chloride-based ionic liquid. The niobium metal used for deposition on the Cu had been dissolved in the solution from electrochemical polishing of a solid niobium piece prior to the deposition. The visible coating on the surface of the Cu was analyzed using scanning electron microscopy (SEM) and electron dispersive x-ray spectroscopy (EDX). This deposition method effectively recycles previously dissolved niobium from electrochemicalmore » polishing.« less

Chemical mechanism of the Gram stain and synthesis of a new electron-opaque marker for electron microscopy which replaces the iodine mordant of the stain.

PubMed Central

Davies, J A; Anderson, G K; Beveridge, T J; Clark, H C

1983-01-01

Crystal violet (hexamethyl-para-rosaniline chloride) interacts with aqueous KI-I2 during the Gram stain via a simple metathetical anion exchange to produce a chemical precipitate. There is an apparent 1:1 stoichiometry between anion (I-) and cation (hexamethyl-para-rosaniline+) during the reaction and, since the small chloride anion is replaced by the bulkier iodide, the complex formed becomes insoluble in water. It is this same precipitate which forms in the cellular substance of bacteria (both gram-positive and gram-negative types) and which initiates the Gram reaction. Potassium trichloro(eta 2-ethylene)-platinum(II), as an electronopaque marker for electron microscopy, was chemically synthesized, and it produced an anion in aqueous solution which was compatible with crystal violet for the Gram stain. It interacted with crystal violet in a similar manner as iodide to produce an insoluble complex which was chemically and physically analogous to the dye-iodide precipitate. This platinum anion therefore allows the Gram staining mechanism to be followed by electron microscopy. Images PMID:6195147

Enhanced photocatalytic performance of RGO/Ag nanocomposites produced via a facile microwave irradiation for the degradation of Rhodamine B in aqueous solution

NASA Astrophysics Data System (ADS)

Divya, K. S.; Chandran, Akash; Reethu, V. N.; Mathew, Suresh

2018-06-01

A series of RGO/Ag nanocomposites with different weight addition ratios of graphene oxide (GO) have been successfully prepared in situ through the simultaneous reduction of GO and AgNO3 via a facile microwave irradiation. X-ray diffraction analysis, Fourier Transform Infrared Spectroscopy, UV-vis diffuse reflectance spectra, Scanning electron microscopy, Photoluminescence spectra, Raman spectra, Atomic Force Microscopy, X-ray photoelectron spectroscopy (XPS) and Transmission electron microscopy are employed to determine the properties of the samples. It is found that RGO/Ag nanocomposites with a proper weight addition ratios of GO exhibit higher photocatalytic activity toward liquid phase photodegradation of Rhodamine B under visible light irradiation. The improved photoactivity of RGO/Ag nanocomposites can be ascribed to the integrative synergestic effect of enhanced adsorption capacity, the prolonged lifetime of photogenerated electron-hole pairs and effective interfacial hybridization between RGO and Ag nanoparticles. This study also shows that graphene sheets act as electronic conductive channels to efficiently separate charge carriers from Ag nanoparticles.

Electrochemical electron beam lithography: Write, read, and erase metallic nanocrystals on demand

PubMed Central

Park, Jeung Hun; Steingart, Daniel A.; Kodambaka, Suneel; Ross, Frances M.

2017-01-01

We develop a solution-based nanoscale patterning technique for site-specific deposition and dissolution of metallic nanocrystals. Nanocrystals are grown at desired locations by electron beam–induced reduction of metal ions in solution, with the ions supplied by dissolution of a nearby electrode via an applied potential. The nanocrystals can be “erased” by choice of beam conditions and regrown repeatably. We demonstrate these processes via in situ transmission electron microscopy using Au as the model material and extend to other metals. We anticipate that this approach can be used to deposit multicomponent alloys and core-shell nanostructures with nanoscale spatial and compositional resolutions for a variety of possible applications. PMID:28706992

Synthesis and characterization of micro/nanoscopic Pb(Zr0.52Ti0.48)O3 fibers by electrospinning

NASA Astrophysics Data System (ADS)

Wang, Y.; Furlan, R.; Ramos, I.; Santiago-Aviles, J. J.

Micro/nanoscopic Pb(Zr0.52Ti0.48)O3 fibers were synthesized from commercially available zirconium n-pro-poxide, titanium isopropoxide, and lead 2-ethylhexanoate. Using xylene as a solvent, they were mixed to form a precursor solution with a suitable viscosity for electrospinning. The solution was analyzed using thermo-gravimetric and differential thermal methods. Ultra-fine fibers and mats were electrostatically drawn from the precursor solution. The as-deposited materials were sintered for 2 h at 400, 500, 600, 700 and 800 °C, respectively. Sintered mats or fibers were characterized using X-ray diffraction (XRD), scanning electron microscopy (SEM), Auger electron spectroscopy (AES), Raman micro-spectrometry and scanning-probe microscopy (SPM). The SEM results revealed that the fibers had diameters varying from hundreds of nanometers to 10 μm. Using AES, the elements Pb, Zr, Ti and O, as well as residual C, were detected on the surface of the fibers. Raman and XRD spectra indicated that the precursors began to transform into the intermediate pyrochlore phase at 400 °C, followed by the perovskite Pb(Zr0.52Ti0.48)O3 phase above 600 °C. Scanning-probe microscopy (SPM), operated in the piezo-response imaging mode, revealed spontaneous polarization domains in the fibers, with diameters ranging from 100 to 500 nm.

Growth of tungsten oxide nanostructures by chemical solution deposition

NASA Astrophysics Data System (ADS)

Jin, L. H.; Bai, Y.; Li, C. S.; Wang, Y.; Feng, J. Q.; Lei, L.; Zhao, G. Y.; Zhang, P. X.

2018-05-01

Tungsten oxide nanostructures were fabricated on LaAlO3 (00l) substrates by a simple chemical solution deposition. The decomposition behavior and phase formation of ammonium tungstate precursor were characterized by thermal analysis and X-ray diffraction. Moreover, the morphology and chemical state of nanostructures were analyzed by scanning electron microscopy, atomic force microscopy and X-ray photoelectron spectra. The effects of crystallization temperature on the formation of nanodots and nanowires were investigated. The results indicated that the change of nanostructures had close relationship with the crystallization temperature during the chemical solution deposition process. Under higher crystallization temperature, the square-like dots transformed into the dome-like nanodots and nanowires. Moreover high density well-ordered nanodots could be obtained on the substrate with the further increase of crystallization temperature. It also suggested that this simple chemical solution process could be used to adjust the nanostructures of tungsten oxide compounds on substrate.

Characterization of stress corrosion cracks in Ni-based weld alloys 52, 52M and 152 grown in high-temperature water

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

Xie, Yi; Wu, Yaqiao; Burns, Jatuporn

Ni-based weld alloys 52, 52M and 152 are extensively used in repair and mitigation of primary water stress corrosion cracking (SCC) in nuclear power plants. In the present study, a series of microstructure and microchemistry at the SCC tips of these alloys were examined with scanning electron microscopy (SEM), electron backscatter diffraction (EBSD), transmission electron microscopy (TEM), energy-dispersive X-ray spectroscopy (EDS), scanning transmission electron microscopy (STEM) and energy filtered transmission electron microscopy (EFTEM). The specimens have similar chemical compositions and testing conditions. Intergranular (IG) and transgranular (TG) SCC was observed in all of them. The cracks were filled with nickel-oxidesmore » and partial precipitations of chrome carbides (CrCs), niobium carbides (NbCs), titanium nitrides (TiNs) and silicon carbides (SiCs), while iron (Fe) was largely dissolved into the solution. However, the crack densities, lengths and distributions were different for all three specimens. - Highlights: • Microstructure and microchemistry at the SCC tips of Ni-based weld alloys 52, 52M and 152 were examined. • The crack densities, lengths and distributions were found to be different for different alloys. • IGSCC and TGSCC were observed on alloy 52, only TGSCC was observed on alloy 52M and 152. • The cracks were filled by Ni-oxides and precipitated CrCs, NbCs, TiNs and SiCs.« less

The collection of MicroED data for macromolecular crystallography.

PubMed

Shi, Dan; Nannenga, Brent L; de la Cruz, M Jason; Liu, Jinyang; Sawtelle, Steven; Calero, Guillermo; Reyes, Francis E; Hattne, Johan; Gonen, Tamir

2016-05-01

The formation of large, well-ordered crystals for crystallographic experiments remains a crucial bottleneck to the structural understanding of many important biological systems. To help alleviate this problem in crystallography, we have developed the MicroED method for the collection of electron diffraction data from 3D microcrystals and nanocrystals of radiation-sensitive biological material. In this approach, liquid solutions containing protein microcrystals are deposited on carbon-coated electron microscopy grids and are vitrified by plunging them into liquid ethane. MicroED data are collected for each selected crystal using cryo-electron microscopy, in which the crystal is diffracted using very few electrons as the stage is continuously rotated. This protocol gives advice on how to identify microcrystals by light microscopy or by negative-stain electron microscopy in samples obtained from standard protein crystallization experiments. The protocol also includes information about custom-designed equipment for controlling crystal rotation and software for recording experimental parameters in diffraction image metadata. Identifying microcrystals, preparing samples and setting up the microscope for diffraction data collection take approximately half an hour for each step. Screening microcrystals for quality diffraction takes roughly an hour, and the collection of a single data set is ∼10 min in duration. Complete data sets and resulting high-resolution structures can be obtained from a single crystal or by merging data from multiple crystals.

Genipin-crosslinked O-carboxymethyl chitosan-gum Arabic coacervate as a pH-sensitive delivery system and microstructure characterization.

PubMed

Huang, Guo-Qing; Cheng, Ling-Yun; Xiao, Jun-Xia; Wang, Shi-Qing; Han, Xiao-Na

2016-08-01

The possibility of genipin-crosslinked O-carboxymethyl chitosan-gum Arabic coacervate as a pH-sensitive delivery vehicle was investigated. O-carboxymethyl chitosan-gum Arabic coacervates separated in pH 3.0, 4.5, and 6.0 were crosslinked by genipin for different durations and the crosslinked products were subjected to crosslinking degree, swelling behavior, bovine serum albumin release profile, and microstructure characterization. Genipin-crosslinking greatly improved the stability of the coacervates against the simulated gastric solution and created certain pH-sensitivity. The coacervates displayed higher swelling ratios in the simulated gastric solution than in the simulated intestine and colon solutions; meanwhile, the coacervates prepared in pH 4.5 and 6.0 swelled more severely than the complex separated in pH 3.0. Nevertheless, the bovine serum albumin release in the simulated gastric solution from the microcapsules prepared in pH 6.0 was much lower than those prepared in pH 4.5 and 3.0, whose cumulative release percentages in the three simulated solutions were 17.14%, 55.23%, and 79.79%, respectively, in crosslinking duration 2 h. X-ray diffraction, scanning electron microscopy, and transmission electron microscopy analysis revealed that genipin-crosslinking improved the regularity and compactness of coacervate structure, whereas confocal laser scanning microscopy observation indicated that O-carboxymethyl chitosan content was possibly the major reason for the different swelling and bovine serum albumin release behavior of the coacervates. It was concluded that the genipin-crosslinked O-carboxymethyl chitosan-gum Arabic coacervate was a potential intestine-targeted delivery system and its delivery performance could be tailored by varying the crosslinking degree and coacervation acidity. © The Author(s) 2016.

Espina: A Tool for the Automated Segmentation and Counting of Synapses in Large Stacks of Electron Microscopy Images

PubMed Central

Morales, Juan; Alonso-Nanclares, Lidia; Rodríguez, José-Rodrigo; DeFelipe, Javier; Rodríguez, Ángel; Merchán-Pérez, Ángel

2011-01-01

The synapses in the cerebral cortex can be classified into two main types, Gray's type I and type II, which correspond to asymmetric (mostly glutamatergic excitatory) and symmetric (inhibitory GABAergic) synapses, respectively. Hence, the quantification and identification of their different types and the proportions in which they are found, is extraordinarily important in terms of brain function. The ideal approach to calculate the number of synapses per unit volume is to analyze 3D samples reconstructed from serial sections. However, obtaining serial sections by transmission electron microscopy is an extremely time consuming and technically demanding task. Using focused ion beam/scanning electron microscope microscopy, we recently showed that virtually all synapses can be accurately identified as asymmetric or symmetric synapses when they are visualized, reconstructed, and quantified from large 3D tissue samples obtained in an automated manner. Nevertheless, the analysis, segmentation, and quantification of synapses is still a labor intensive procedure. Thus, novel solutions are currently necessary to deal with the large volume of data that is being generated by automated 3D electron microscopy. Accordingly, we have developed ESPINA, a software tool that performs the automated segmentation and counting of synapses in a reconstructed 3D volume of the cerebral cortex, and that greatly facilitates and accelerates these processes. PMID:21633491

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

NASA Astrophysics Data System (ADS)

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

2015-12-01

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

Investigation of Different Colloidal Porous Silicon Solutions and Their Composite Solid Matrix Rods by Optical Techniques

NASA Astrophysics Data System (ADS)

Khan, M. Naziruddin; Aldalbahi, Ali; Almohammedi, Abdullah

2018-03-01

Colloidal porous silicon (PSi) in different solvents was synthesized by simple chemical etching. Colloidal solutions were then prepared using different quantities of silicon wafer pieces (Pcs) and chloroplatinic (Pt) acid in catalyst solution. The effect on the properties of the colloidal solutions and composite rods were investigated using various optical characterization techniques. Absorption and photoluminescence (PL) intensity of the colloidal PSi solutions are observed to depend on the quantity of wafer Pcs, the Pt-solution, and the porosity formation on the wafer surface. The morphological structure of the PSi in a solvent and the solid-rod environments were studied using field-emission scanning electron microscopy (FE-SEM) and were observed to have different structures. A mono-oriented structure of PSi exists in tetrahydrofuran, which has stereo orientation in dioxane and dimethylsulfoxide (approximately 5-8 nm as confirmed using high resolution transmission electron microscopy). Subsequently, some colloidal PSi solutions were directly embedded in three types of sol-gel-based matrices, silica, ormosils (or organically modified silica) and polymer, which easily generated solid rods. Spontaneous emission (SE) of the PSi solutions and their composite rods were examined using a high power picosecond 355 nm laser source. The emitted PL and SE signals of the colloidal PSi solutions were dependent on the Pt volume, nature of the solvent, quantity of Si wafer piece, and pumping energy. The response of SE signals from the PSi composites rods is an interesting phenomenon, and such nanocomposites may be used for future research on light amplification.

Investigation of Different Colloidal Porous Silicon Solutions and Their Composite Solid Matrix Rods by Optical Techniques

NASA Astrophysics Data System (ADS)

Khan, M. Naziruddin; Aldalbahi, Ali; Almohammedi, Abdullah

2018-07-01

Colloidal porous silicon (PSi) in different solvents was synthesized by simple chemical etching. Colloidal solutions were then prepared using different quantities of silicon wafer pieces (Pcs) and chloroplatinic (Pt) acid in catalyst solution. The effect on the properties of the colloidal solutions and composite rods were investigated using various optical characterization techniques. Absorption and photoluminescence (PL) intensity of the colloidal PSi solutions are observed to depend on the quantity of wafer Pcs, the Pt-solution, and the porosity formation on the wafer surface. The morphological structure of the PSi in a solvent and the solid-rod environments were studied using field-emission scanning electron microscopy (FE-SEM) and were observed to have different structures. A mono-oriented structure of PSi exists in tetrahydrofuran, which has stereo orientation in dioxane and dimethylsulfoxide (approximately 5-8 nm as confirmed using high resolution transmission electron microscopy). Subsequently, some colloidal PSi solutions were directly embedded in three types of sol-gel-based matrices, silica, ormosils (or organically modified silica) and polymer, which easily generated solid rods. Spontaneous emission (SE) of the PSi solutions and their composite rods were examined using a high power picosecond 355 nm laser source. The emitted PL and SE signals of the colloidal PSi solutions were dependent on the Pt volume, nature of the solvent, quantity of Si wafer piece, and pumping energy. The response of SE signals from the PSi composites rods is an interesting phenomenon, and such nanocomposites may be used for future research on light amplification.

Formation of multicomponent matrix metal oxide films in anodic alumina matrixes by chemical deposition

NASA Astrophysics Data System (ADS)

Gorokh, G. G.; Zakhlebayeva, A. I.; Metla, A. I.; Zhilinskiy, V. V.; Murashkevich, A. N.; Bogomazova, N. V.

2017-11-01

The metal oxide films of SnxZnyOz and SnxMoyOz systems deposited onto anodic alumina matrixes by chemical and ion layering from an aqueous solutions were characterized by scanning electron microscopy, Raman spectroscopy, electron probe X-ray microanalysis and IR spectroscopy. The obtained matrix films had reproducible composition and structure and possessed certain morphological characteristics and properties.

Single clay sheets inside electrospun polymer nanofibers

NASA Astrophysics Data System (ADS)

Sun, Zhaohui

2005-03-01

Nanofibers were prepared from polymer solution with clay sheets by electrospinning. Plasma etching, as a well controlled process, was used to supply electrically excited gas molecules from a glow discharge. To reveal the structure and arrangement of clay layers in the polymer matrix, plasma etching was used to remove the polymer by controlled gasification to expose the clay sheets due to the difference in reactivity. The shape, flexibility, and orientation of clay sheets were studied by transmission and scanning electron microscopy. Additional quantitative information on size distribution and degree of exfoliation of clay sheets were obtained by analyzing electron micrograph of sample after plasma etching. Samples in various forms including fiber, film and bulk, were thinned by plasma etching. Morphology and dispersion of inorganic fillers were studied by electron microscopy.

Preparation of high-strength Al-Mg-Si-Cu-Fe alloy via heat treatment and rolling

NASA Astrophysics Data System (ADS)

Liu, Chong-yu; Yu, Peng-fei; Wang, Xiao-ying; Ma, Ming-zhen; Liu, Ri-ping

2014-07-01

An Al-Mg-Si-Cu-Fe alloy was solid-solution treated at 560°C for 3 h and then cooled by water quenching or furnace cooling. The alloy samples which underwent cooling by these two methods were rolled at different temperatures. The microstructure and mechanical properties of the rolled alloys were investigated by optical microscopy, scanning electron microscopy, transmission electron microscopy, X-ray diffraction analysis, and tensile testing. For the water-quenched alloys, the peak tensile strength and elongation occurred at a rolling temperature of 180°C. For the furnace-cooled alloys, the tensile strength decreased initially, until the rolling temperature of 420°C, and then increased; the elongation increased consistently with increasing rolling temperature. The effects of grain boundary hardening and dislocation hardening on the mechanical properties of these rolled alloys decreased with increases in rolling temperature. The mechanical properties of the 180°C rolling water-quenched alloy were also improved by the presence of β″ phase. Above 420°C, the effect of solid-solution hardening on the mechanical properties of the rolled alloys increased with increases in rolling temperature.

You can't measure what you can't see - detectors for microscopies

NASA Astrophysics Data System (ADS)

Denes, Peter

For centuries, the human eye has been the imaging detector of choice thanks to its high sensitivity, wide dynamic range, and direct connection to a built-in data recording and analysis system. The eye, however, is limited to visible light, which excludes microscopies with electrons and X-rays, and the built-in recording system stores archival information at very low rates. The former limitation has been overcome by ``indirect'' detectors, which convert probe particles to visible light, and the latter by a variety of recording techniques, from photographic film to semiconductor-based imagers. Semiconductor imagers have been used for decades as ``direct'' detectors in particle physics, and almost as long for hard X-rays. For soft X-ray microscopy, the challenge has been the small signal levels - plus getting the X-rays into the detector itself, given how quickly they are absorbed in inert layers. For electron microscopy, the challenge has been reconciling detector spatial resolution and pixel count with the large multiple scattering of electrons with energies used for microscopy. Further, a high recording rate (``movies'' rather than ``snapshots'') enables time-resolved studies, time-dependent corrections, shot-by-shot experiments and scanning techniques - at the expense of creating large data volumes. This talk will discuss solutions to these challenges, as well as an outlook towards future developments.

Electrochemical Corrosion of Stainless Steel in Thiosulfate Solutions Relevant to Gold Leaching

NASA Astrophysics Data System (ADS)

Choudhary, Lokesh; Wang, Wei; Alfantazi, Akram

2016-01-01

This study aims to characterize the electrochemical corrosion behavior of stainless steel in the ammoniacal thiosulfate gold leaching solutions. Electrochemical corrosion response was investigated using potentiodynamic polarization and electrochemical impedance spectroscopy, while the semi-conductive properties and the chemical composition of the surface film were characterized using Mott-Schottky analysis and X-ray photoelectron spectroscopy, respectively. The morphology of the corroded specimens was analyzed using scanning electron microscopy. The stainless steel 316L showed no signs of pitting in the ammoniacal thiosulfate solutions.

Reaction mechanisms for enhancing carbon dioxide mineral sequestration

NASA Astrophysics Data System (ADS)

Jarvis, Karalee Ann

Increasing global temperature resulting from the increased release of carbon dioxide into the atmosphere is one of the greatest problems facing society. Nevertheless, coal plants remain the largest source of electrical energy and carbon dioxide gas. For this reason, researchers are searching for methods to reduce carbon dioxide emissions into the atmosphere from the combustion of coal. Mineral sequestration of carbon dioxide reacted in electrolyte solutions at 185°C and 2200 psi with olivine (magnesium silicate) has been shown to produce environmentally benign carbonates. However, to make this method feasible for industrial applications, the reaction rate needs to be increased. Two methods were employed to increase the rate of mineral sequestration: reactant composition and concentration were altered independently in various runs. The products were analyzed with complete combustion for total carbon content. Crystalline phases in the product were analyzed with Debye-Scherrer X-ray powder diffraction. To understand the reaction mechanism, single crystals of San Carlos Olivine were reacted in two solutions: (0.64 M NaHCO3/1 M NaCl) and (5.5 M KHCO3) and analyzed with scanning electron microscopy (SEM), transmission electron microscopy (TEM), electron energy loss spectroscopy (EELS), and fluctuation electron microscopy (FEM) to study the surface morphology, atomic crystalline structure, composition and amorphous structure. From solution chemistry studies, it was found that increasing the activity of the bicarbonate ion increased the conversion rate of carbon dioxide to magnesite. The fastest conversion, 60% conversion in one hour, occurred in a solution of 5.5 M KHCO3. The reaction product particles, magnesium carbonate, significantly increased in both number density and size on the coupon when the bicarbonate ion activity was increased. During some experiments reaction vessel corrosion also altered the mineral sequestration mechanism. Nickel ions from vessel corrosion led to nickel precipitation in the carbonate particles and the lack of an amorphous silica reaction layer on the olivine. It was concluded that nickel ions destabilized the silica passivation layer and led to faster growth of carbonate precipitates. Overall, nickel ions increased the reaction rate of mineral sequestration of carbon dioxide.

Removal of tetracycline from aqueous solution by MCM-41-zeolite A loaded nano zero valent iron: Synthesis, characteristic, adsorption performance and mechanism.

PubMed

Guo, Yige; Huang, Wenli; Chen, Bin; Zhao, Ying; Liu, Dongfang; Sun, Yu; Gong, Bin

2017-10-05

In this study, nano zero valent iron (NZVI) modified MCM-41-zeolite A (Fe-MCM-41-A) composite as a novel adsorbent was prepared by precipitation method and applied for tetracycline (TC) removal from aqueous solution. The adsorbent was characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), Fourier transform infrared (FT-IR) spectroscopy, X-ray photoelectron spectroscopy (XPS) and N 2 -BET analysis. Hysteresis loops indicated that the sample has a desirable magnetic property and can be separated quickly. Adsorption studies were carried out to evaluate its potential for TC removal. Results showed that the optimal Fe-MCM-41-A dosage, initial pH and reaction time at initial TC concentration of 100mgL -1 solution are 1gL -1 , pH=5, and 60 min respectively, at which the removal efficiency of TC was 98.7%. The TC adsorption results fitted the Langmuir isotherm model very well and the adsorption process could be described by a pseudo-second-order kinetic model. A maximum TC adsorption capacity of 526.32mgg -1 was achieved. This study demonstrates that Fe-MCM-41-A is a promising and efficient material for TC adsorption from aqueous solution. Copyright © 2017 Elsevier B.V. All rights reserved.

Scanning Electron Microscopy Findings of Machine Perfused Liver Graft After Warm Ischemia Between Hypothermic and Rewarming Machine Perfusion in Pigs.

PubMed

Meng, L; Matsuno, N; Watanabe, K; Furukori, M; Obara, H; Bochimoto, H; Watanabe, T; Fukukawa, H

2016-09-01

The shortage of organ donors is a universal problem. Use of grafts from donors after cardiac death would greatly contribute to the expansion of the donor organ pool. The two major methods of preservation are cold storage and machine perfusion (MP) preservation, and each has its own advantages. Several studies have reported the relative merits of MP for the preservation for grafts from donors after cardiac death. In this study, we used scanning electron microscopy (SEM) to assess the damage to the liver between hypothermic and rewarming preservation conditions. Porcine livers were perfused with a newly developed MP system. The livers were perfused for 4 hours with a modified University of Wisconsin solution-gluconate solution. In group 1, grafts were preserved with warm ischemic time for 60 minutes and hypothermic machine perfusion (HMP) for 4 hours. In group 2, grafts were preserved with warn ischemic time for 60 minutes and had rewarming up to 22°C by MP (RMP) for 4 hours. A significant enlargement of the mitochondria were observed in both the HMP and RMP groups under higher magnification, Additionally, vacuoles appeared occasionally in hepatocytes in the RMP for 4 hours group, but not in the HMP for 4 hours group. An analysis by scanning electron microscope appears to be useful to evaluate the levels of damage of hepatocytes compared with transmission electron microscopy, and further study is needed to analyze the significance of the appearance of swelling of mitochondria and vacuolization during preservation. Copyright © 2016 The Authors. Published by Elsevier Inc. All rights reserved.

Box-Behnken experimental design for chromium(VI) ions removal by bacterial cellulose-magnetite composites.

PubMed

Stoica-Guzun, Anicuta; Stroescu, Marta; Jinga, Sorin Ion; Mihalache, Nicoleta; Botez, Adriana; Matei, Cristian; Berger, Daniela; Damian, Celina Maria; Ionita, Valentin

2016-10-01

In this study bacterial cellulose-magnetite composites were synthesised for the removal of chromium(VI) from aqueous solutions. Fourier transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD), thermogravimetric analysis and X-ray Photoelectron Spectroscopy (XPS) were used to characterize the bacterial cellulose-magnetite composites and to reveal the uniform dispersion of nanomagnetite in the BC matrix. Magnetic properties were also measured to confirm the magnetite immobilization on bacterial cellulose membrane. The effects of initial Cr(VI) concentration, solution pH and solid/liquid ratio upon chromium removal were examined using the statistical Box-Behnken Design. Because of the possibility of magnetite dissolution during chromium(VI) adsorption, the degree of iron leaching was also analysed in the same conditions as Cr(VI) adsorption. From the factors affecting chromium(VI) adsorption the most important was solution pH. The highest Cr(VI) removal efficiency was observed at pH 4, accompanied by the lowest iron leaching in the solution. The adsorption experiments also indicated that the adsorption process of chromium(VI) is well described by Freundlich adsorption model. Our results proved that the BC-magnetite composites could be used for an efficient removal of chromium(VI) from diluted solutions with a minimum magnetite dissolution during operation. Copyright © 2016 Elsevier B.V. All rights reserved.

Structure and morphology of regenerated silk nano-fibers produced by electrospinning

NASA Astrophysics Data System (ADS)

Zarkoob, Shahrzad

The impressive physical and mechanical properties of natural silk fiberssp1 and the possibility of producing these proteins using biotechnology,sp2 have provided the impetus for recent efforts in both the biosynthesissp{3,4} and the spinning of these protein based biopolymers.sp{5,6,7} The question still remains: whether fibers spun from solutions with similar chemical makeup can produce fibers with similar structures and therefore with the possibility of improved properties. Since genetically engineered silk solutions were not readily available, the first objective of this project was to completely dissolve the Bombyx mori cocoon and the Nephila clavipes dragline silk while maintaining the molecular weight integrity of the polymer. The second objective was to develop a system for re-spinning from very small amount of the resulting silk solutions by the process of electrospinning. The third objective was, to produce regenerated silk fibers with diameters that are several orders of magnitude smaller than the original fibers, suitable for direct observation and analysis by transmission electron microscopy and electron diffraction. And finally, to compare these results to structural information obtained from natural (as spun by the organism) fibers to see if the regenerated solutions are able to form the same structure as the original fibers. Both types of silk fibers were successfully dissolved while maintaining the polymer integrity. Small quantities (25-50 mul) of these solutions were used to electrospin fibers with diameters ranging from 8nm-200nm. The fibers were observed by optical, scanning electron, and transmission electron microscopy. These nano fibers showed optical retardation, appeared to have a circular cross-section, and were dimensionally stable at temperatures above 280sp°C. Electron diffraction patterns of annealed electrospun fibers of B. mori and N. clavipes showed reflections, demonstrating orientational and semicrystalline order in the material comparable to natural silk. In addition, electron diffraction was also obtained form extended microtomed single dragline fibers of N. clavipes, and the d-spacings agreed well with thoes obtained from WAXD of dragline fiber bundles.

Removal of selected pharmaceuticals from aqueous solution using magnetic chitosan: sorption behavior and mechanism.

PubMed

Zhang, Yalei; Shen, Zhe; Dai, Chaomeng; Zhou, Xuefei

2014-11-01

A novel-modified magnetic chitosan adsorbent was used to remove selected pharmaceuticals, i.e., diclofenac (DCF) and clofibric acid (CA) and carbamazepine (CBZ), from aqueous solutions. The characterization of magnetic chitosan was achieved by scanning electron and transmission electron microscopy, X-ray diffraction, X-ray photoelectron spectroscopy, vibrating sample magnetometer, and nitrogen sorption analysis. The magnetic chitosan had effective sorption affinity for DCF and CA but no sorption of CBZ was observed. The sorption capacities of CA and DCF in the individual solutions were 191.2 and 57.5 mg/g, respectively. While in mixed solution, DCF showed higher sorption affinity. Sorption kinetics indicated a quick equilibrium reached within 2 min. Lower solution pH values were found to be advantageous for the adsorption process. The sorption efficacy of CA declined significantly with increasing inorganic salt concentration. However, sorption performance of DCF was stable under different ionic strength conditions.

Corneal collagen cross-linking: a confocal, electron, and light microscopy study of eye bank corneas.

PubMed

Dhaliwal, Jasmeet S; Kaufman, Stephen C

2009-01-01

The purpose of this study was to evaluate morphological changes induced by corneal collagen cross-linking in a human ex vivo cornea, using confocal, electron, and light microscopy. The central epithelium was partially removed from ex vivo human corneal buttons. Riboflavin 0.1% solution was applied before ultraviolet A light treatment and then for every 2 minutes for 30 minutes while the corneas were exposed to ultraviolet A light at a wavelength of 370 nm and intensity of 3 mW/cm(2). Each cornea was evaluated using confocal, electron, and light microscopy. Confocal microscopy demonstrated normal-appearing corneas on their initial pretreatment examination, with reduced stromal detail. After treatment, a superficial layer of highly reflective spherical structures (4-10 microm) was observed. Many of these hyperreflective structures appeared up to a depth of 300 microm. The remainder of the corneal stroma and endothelium appeared normal. Electron microscopy showed keratocyte apoptotic changes to a depth of 300 microm. No observable pathologic changes were seen on histology. Based on clinical studies, corneal cross-linking is a promising treatment that appears to be safe and to halt ectatic corneal disease progression. Initial European studies used animal models to extrapolate human protocols. In conjunction with clinical studies, we believe that human ex vivo corneal studies provide a means to evaluate the structural and morphological changes associated with this procedure, within human corneas, in a manner that cannot be accomplished in vivo.

Fabrication and characterization of poly(L-lactic acid) gels induced by fibrous complex crystallization with solvents

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

Matsuda, Yasuhiro; Fukatsu, Akinobu; Wang, Yangyang

2014-01-01

Complex crystal induced gelation of poly(L-lactic acid) (PLLA) solutions was studied for a series of solvents, including N,N-dimethylformamide (DMF). By cooling the solutions prepared at elevated temperatures, PLLA gels were produced in solvents that induced complex crystals ( -crystals) with PLLA. Fibrous structure of PLLA in the gel with DMF was observed by polarizing optical microscopy, field emission electron microscopy, and atomic force microscopy. Upon heating, the crystal form of PLLA in the DMF gel changed from -crystal to a-crystal, the major crystal form in common untreated PLLA films, but the morphology and high elastic modulus of the gel remainedmore » until the a-crystal dissolved at higher temperature. In addition, a solvent exchanging method was developed, which allowed PLLA gels to be prepared in other useful solvents that do not induce -crystals without losing the morphology and mechanical properties.« less

Cryopreservation of rabbit corneas: assessment by microscopy and transplantation.

PubMed Central

Fong, L P; Hunt, C J; Taylor, M J; Pegg, D E

1986-01-01

Rabbit corneas were frozen and thawed by three methods and compared by full thickness transplantation as well as specular microscopy, histology, and transmission electron microscopy. Two of the methods used a recently described technique, in which the excised cornea was immersed in a potassium-rich buffered solution containing the cryoprotectant dimethyl sulphoxide (Me2SO, 2 mol/l). This solution was designed to restrict the loss of intracellular potassium and to prevent cell swelling at low temperatures. In one group the corneas were frozen and thawed surrounded by 5 ml of medium, while in the second group corneas were drained of excess fluid and frozen in air. The third group consisted of corneas cryopreserved by Capella and colleagues' method. All the cryopreserved corneas were damaged, but those that had been frozen in air after exposure to the new medium showed better structure and function than corneas frozen by either of the other two techniques. Images PMID:3535871

Comparison of the effects of glycerol, dimethyl sulfoxide, and hydroxyethyl starch solutions for cryopreservation of avian red blood cells.

PubMed

Graham, Jennifer E; Meola, Dawn M; Kini, Nisha R; Hoffman, Andrew M

2015-06-01

To compare effectiveness of glycerol, dimethyl sulfoxide (DMSO), and hydroxyethyl starch (HES) solutions for cryopreservation of avian RBCs. RBCs from 12 healthy Ameraucana hens (Gallus gallus domesticus). RBCs were stored in 20% (wt/vol) glycerol, 10% (wt/vol) DMSO freezing medium, or various concentrations of HES solution (7.5%, 11.5%, and 20% [wt/vol]) and frozen for 2 months in liquid nitrogen. Cells were then thawed and evaluated by use of cell recovery and saline stability tests, cell staining (7-aminoactinomycin D and annexin V) and flow cytometry, and scanning electron microscopy. Percentage of RBCs recovered was highest for 20% glycerol solution (mean ± SE, 99.71 ± 0.04%) and did not differ significantly from the value for 7.5% HES solution (99.57 ± 0.04%). Mean saline stability of RBCs was highest for 10% DMSO (96.11 ± 0.25%) and did not differ significantly from the value for 20% HES solution (95.74 ± 0.25%). Percentages of cells with 7-aminoactinomycin D staining but without annexin V staining (indicating necrosis or late apoptosis) were lowest for 10% DMSO freezing medium (3%) and 20% glycerol solution (1%) and highest for all HES concentrations (60% to 80%). Scanning electron microscopy revealed severe membrane changes in RBCs cryopreserved in 20% HES solution, compared with membrane appearance in freshly harvested RBCs and RBCs cryopreserved in 10% DMSO freezing medium. Cryopreservation of avian RBCs with HES solution, regardless of HES concentration, resulted in greater degrees of apoptosis and cell death than did cryopreservation with other media. Transfusion with RBCs cryopreserved in HES solution may result in posttransfusion hemolysis in birds.

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

NASA Astrophysics Data System (ADS)

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

2011-10-01

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

Physiochemical and optical properties of chitosan based graphene oxide bionanocomposite.

PubMed

Kumar, Santosh; Koh, Joonseok

2014-09-01

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

Template-free solution approach to synthesize CdS dendrites with SCN based ionic liquid

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

Li, Kangfeng; Li, Jiajia; Cheng, Xianyi

2011-07-15

Highlights: {yields} Template-free solution approach to synthesize CdS hierarchical dendrites. {yields} The 1-butyl-3-methlyimidazole thiocyanate ([BMIM][SCN]) plays doubly functional roles in the progress. {yields} The CdS hierarchical dendrites exhibit a more intense emission at 710 nm belongs to infrared band. -- Abstract: Cadmium sulfide dendrites were synthesized by a facile hydrothermal treatment from CdCl{sub 2} and ionic liquid 1-butyl-3-methlyimidazole thiocyanate acted both as sulfur source and surfactant. The product was characterized by means of X-ray powder diffraction and scanning electron microscopy. X-ray powder diffraction studies indicated that the product was well-crystallized hexagonal phase of CdS, and the scanning electron microscopy imagesmore » showed that the obtained powders consisted of a wealth of well-defined CdS dendritic microstructures with a pronounced trunk and highly ordered branches. The UV-Vis and photoluminescence spectroscopy measurements were taken as well. The possible formation mechanism of CdS dendrites was simply proposed in the end.« less

Kinetic control of block copolymer self-assembly into multicompartment and novel geometry nanoparticles

NASA Astrophysics Data System (ADS)

Chen, Yingchao; Wang, Xiaojun; Zhang, Ke; Wooley, Karen; Mays, Jimmy; Percec, Virgil; Pochan, Darrin

2012-02-01

Micelles with the segregation of hydrophobic blocks trapped in the same nanoparticle core have been produced through co-self-assembly of two block copolymers in THF/water dilute solution. The dissolution of two block copolymer sharing the same polyacrylic acid PAA blocks in THF undergoes consequent aggregation and phase separation through either slow water titration or quick water addition that triggers the micellar formation. The combination and comparison of the two water addition kinetic pathways are the keys of forming multicompartment structures at high water content. Importantly, the addition of organic diamine provides for acid-base complexation with the PAA side chains which, in turn, plays the key role of trapping unlike hydrophobic blocks from different block copolymers into one nanoparticle core. The kinetic control of solution assembly can be applied to other molecular systems such as dendrimers as well as other block copolymer molecules. Transmission electron microscopy, cryogenic transmission electron microscopy, light scattering have been applied to characterize the micelle structures.

Synthesis of nanometer-sized sodalite without adding organic additives.

PubMed

Fan, Wei; Morozumi, Kazumasa; Kimura, Riichiro; Yokoi, Toshiyuki; Okubo, Tatsuya

2008-06-01

Aggregates (80 nm) of sodalite nanocrystals with crystallite sizes ranging from 20 to 40 nm have been synthesized from a sodium aluminosilicate solution at low temperature, without adding any organic additives, while paying attention to the key factors for the synthesis of nanosized zeolite crystals. The physical properties of nanosized sodalite crystals were characterized by X-ray diffraction, scanning electron microscopy, high-resolution transmission electron microscopy, 29Si solid-state magic-angle spinning (MAS) NMR, and N2 adsorption. As expected, the external surface area of nanosized sodalite crystals is significantly increased compared with that of microsized sodalite crystals. The size of synthesized sodalite crystals can be controlled from 20 nm to 10 microm. It is found that the preparation of a homogeneous aluminosilicate solution followed by the formation of an aluminosilicate hard gel by adjusting the initial composition, for example, SiO2/Al2O3 and Na2O/H2O ratios, is critical for synthesis.

Isotope effect in heavy/light water suspensions of optically active gold nanoparticles

NASA Astrophysics Data System (ADS)

Kutsenko, V. Y.; Artykulnyi, O. P.; Petrenko, V. I.; Avdeev, M. V.; Marchenko, O. A.; Bulavin, L. A.; Snegir, S. V.

2018-04-01

Aqueous suspensions of optically active gold nanoparticles coated with trisodium citrate were synthesized in light (H2O) water and mixture of light and heavy (H2O/D2O) water using the modified Turkevich protocol. The objective of the paper was to verify sensitivity of neutron scattering methods (in particular, neutron reflectometry) to the potential isotope H/D substitution in the stabilizing organic shell around particles in colloidal solutions. First, the isotope effect was studied with respect to the changes in the structural properties of metal particles (size, shape, crystalline morphology) in solutions by electron microscopy including high-resolution transmission electron microscopy from dried systems. The structural factors determining the variation in the adsorption spectra in addition to the change in the optical properties of surrounding medium were discussed. Then, neutron reflectometry was applied to the layered nanoparticles anchored on a silicon wafer via 3-aminopropyltriethoxysilane molecules to reveal the presence of deuterated water molecules in the shell presumably formed by citrate molecules around the metallic core.

Adsorption of Pb(II) from aqueous solution using a magnetic chitosan/graphene oxide composite and its toxicity studies.

PubMed

Samuel, Melvin S; Shah, Sk Sheriff; Bhattacharya, Jayanta; Subramaniam, Kalidass; Pradeep Singh, N D

2018-05-02

This study involves the adsorption of lead using magnetic chitosan/graphene oxide (MCGO) composite material in batch mode. The MCGO composite material was synthesized via modified Hummers method. The MCGO composite material was characterized by powder x-ray diffraction (PXRD), Fourier transform infrared spectroscopy (FT-IR), scanning electron microscopy (SEM), Tunnelling electron microscopy (TEM), thermogravimetric analysis (TGA), Brunauer-Emmett-Teller (BET) and UV-vis diffusive reflectance spectra. The adsorption mechanism of MCGO composite material was well described by Langmuir isotherm and pseudo second order kinetic model, with a high regression coefficient (<0.99). The MCGO composite material was applied for the removal of lead metal from aqueous solution. We have also evaluated toxicity of synthesized MCGO composite material by examining on A549 cells. The results have shown that MCGO material showed viable cell percentage of 53.7% at 50 μg and 44.8% at 100 μg. Copyright © 2018 Elsevier B.V. All rights reserved.

Characterization of Localized Corrosion in an Al-Cu-Li Alloy

NASA Astrophysics Data System (ADS)

Luo, Chen; Zhang, Xinxin; Zhou, Xiaorong; Sun, Zhihua; Zhang, Xiaoyun; Tang, Zhihui; Lu, Feng; Thompson, George E.

2016-05-01

Corrosion behaviors of recently developed 2A97-T6 aluminum-copper-lithium alloy in sodium chloride solution are investigated using scanning electron and transmission electron microscopies in conjunction with electron backscatter diffraction. It has been found that corrosion product rings were established on the alloy surface as early as 5 min during immersion in sodium chloride solution. Meanwhile, hydrogen continuously evolved from within the rings. Pitting corrosion is evident with crystallographic dependant corrosion channel facets mainly parallel to {100} planes. Non-uniform distribution of misorientation in the 2A97 aluminum alloy results in a portion of grains of relatively high stored energy. Such grains were preferentially attacked, serving as local anodes, during the development of crystallographic pitting.

Electron Tomography: A Three-Dimensional Analytic Tool for Hard and Soft Materials Research.

PubMed

Ercius, Peter; Alaidi, Osama; Rames, Matthew J; Ren, Gang

2015-10-14

Three-dimensional (3D) structural analysis is essential to understand the relationship between the structure and function of an object. Many analytical techniques, such as X-ray diffraction, neutron spectroscopy, and electron microscopy imaging, are used to provide structural information. Transmission electron microscopy (TEM), one of the most popular analytic tools, has been widely used for structural analysis in both physical and biological sciences for many decades, in which 3D objects are projected into two-dimensional (2D) images. In many cases, 2D-projection images are insufficient to understand the relationship between the 3D structure and the function of nanoscale objects. Electron tomography (ET) is a technique that retrieves 3D structural information from a tilt series of 2D projections, and is gradually becoming a mature technology with sub-nanometer resolution. Distinct methods to overcome sample-based limitations have been separately developed in both physical and biological science, although they share some basic concepts of ET. This review discusses the common basis for 3D characterization, and specifies difficulties and solutions regarding both hard and soft materials research. It is hoped that novel solutions based on current state-of-the-art techniques for advanced applications in hybrid matter systems can be motivated. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Electron Tomography: A Three-Dimensional Analytic Tool for Hard and Soft Materials Research

PubMed Central

Alaidi, Osama; Rames, Matthew J.

2016-01-01

Three-dimensional (3D) structural analysis is essential to understand the relationship between the structure and function of an object. Many analytical techniques, such as X-ray diffraction, neutron spectroscopy, and electron microscopy imaging, are used to provide structural information. Transmission electron microscopy (TEM), one of the most popular analytic tools, has been widely used for structural analysis in both physical and biological sciences for many decades, in which 3D objects are projected into two-dimensional (2D) images. In many cases, 2D-projection images are insufficient to understand the relationship between the 3D structure and the function of nanoscale objects. Electron tomography (ET) is a technique that retrieves 3D structural information from a tilt series of 2D projections, and is gradually becoming a mature technology with sub-nanometer resolution. Distinct methods to overcome sample-based limitations have been separately developed in both physical and biological science, although they share some basic concepts of ET. This review discusses the common basis for 3D characterization, and specifies difficulties and solutions regarding both hard and soft materials research. It is hoped that novel solutions based on current state-of-the-art techniques for advanced applications in hybrid matter systems can be motivated. PMID:26087941

Nanocrystalline (U0.5Ce0.5)O2±x solid solutions through citrate gel-combustion

NASA Astrophysics Data System (ADS)

Maji, D.; Ananthasivan, K.; Venkata Krishnan, R.; Balakrishnan, S.; Amirthapandian, S.; Joseph, Kitheri; Dasgupta, Arup

2018-04-01

Nanocrystalline powders of (U0.5Ce0.5)O2±x solid solutions were synthesized in bulk (100-200 g) through the citrate gel combustion. The fuel (citric acid) to oxidant (nitrate) mole ratio (R) was varied from 0.1 to 1.0. Two independent lots of the products obtained through the gel-combustion were calcined at 973 K in air and in a mixture of argon containing 8% H2 respectively. All these powders were characterized for their bulk density, X-ray crystallite size, specific surface area, size distribution of the particles, porosity as well as residual carbon. The morphology and microstructures of these powders were studied by using scanning electron microscopy (SEM) and transmission electron microscopy (TEM) respectively. Nanocrystalline single phase fluorite solid solutions having a typical crystallite size of about (7-15 nm) were obtained. These powders were highly porous comprising cuboidal flaky agglomerates. The combustion mixture with an 'R' value of 0.25 was found to undergo volume combustion and was found to yield a product that was distinctly different. The systematic investigation on synthesis and characterization of nanocrystalline UCeO2 is reported for the first time.

Effects of solution concentration and capping agents on the properties of potassium titanyl phosphate noparticles synthesized using a co-precipitation method

NASA Astrophysics Data System (ADS)

Gharibshahian, E.; Jafar Tafershi, M.; Fazli, M.

2018-05-01

In this study, KTiOPO4 (KTP) nanoparticles were synthesized using a co-precipitation method. The effects of the solution concentration (M) and capping agents, such as PVA, oxalic acid, glycine, triethanolamine, and L-alanine, on the structural, microstructural, and optical properties of the products were investigated using X-ray diffraction (XRD), Fourier transform infrared (FTIR) spectroscopy, ultraviolet-visible spectroscopy, field emission scanning electron microscopy, and transmission electron microscopy. Decreasing the solution concentration decreased the crystallite size from 53.07 nm (for M = 2) to 39.42 nm (for M = 0.5). After applying different capping agents to the sample at the optimum concentration (M = 0.5), the crystallite size decreased again and grains as small as 10.61 nm were obtained. XRD and FTIR analyses indicated the formation of KTP nanoparticles with an orthorhombic structure in all of the samples. The optical band gap increased as the crystallite size decreased. Different morphological patterns such as spherical, needle shaped, polyhedron, and tablet forms were observed in the nanoparticles, which were correlated with the effects of the capping agents employed.

Influence of ageing time on hardness, microstructure and wear behaviour of AISI2507 super duplex stainless steel

NASA Astrophysics Data System (ADS)

Davanageri, Mahesh; Narendranath, S.; Kadoli, Ravikiran

2017-08-01

The effect of ageing time on hardness, microstructure and wear behaviour of super duplex stainless AISI 2507 is examined. The material was solution treated at 1050 °C and water quenched, further the ageing has been carried out at 850 °C for 30 min, 60 min and 90 min. The chromium (Cr) and molybdenum (Mo) enriched intermetallic sigma phase (σ) were found to precipitate at the ferrite/austenite interface and within the ferrite region. The concentration of intermetallic sigma phase (σ), which was quantified by a combination of scanning electron microscopy and image analysis, increases with increasing ageing time, leading to significant increase in the hardness. The x-ray diffraction (XRD) and energy dispersive x-ray (EDX) was employed to investigate the element distribution and phase identification. Wear characterstics of the aged super duplex stainless steel were measured by varying normal loads, sliding speeds, sliding distance and compared with solution treated (as-cast) specimens. Scanning electron microscopy was used to assist in analysis of worn out surfaces. The outcomes suggested that the increase in percentage of sigma phase increases hardness and wear resistance in heat-treated specimens compared to solution treated specimens (as-cast).

Confocal Raman and electronic microscopy studies on the topotactic conversion of calcium carbonate from Pomacea lineate shells into hydroxyapatite bioceramic materials in phosphate media.

PubMed

dePaula, S M; Huila, M F G; Araki, K; Toma, H E

2010-12-01

Conversion of Pomacea lineate shells into hydroxyapatite (HA) bioceramic materials was investigated by their in vitro treatment with phosphate solutions, at room temperature. Confocal Raman microscopy revealed that the conversion proceeds at distinct rates through the nacreous or periostracum sides of the shell. The conversion can be accelerated using powdered samples, yielding biocompatible materials of great interest in biomedicine. Copyright © 2010 Elsevier Ltd. All rights reserved.

Solid-solution CrCoCuFeNi high-entropy alloy thin films synthesized by sputter deposition

DOE PAGES

An, Zhinan; Jia, Haoling; Wu, Yueying; ...

2015-05-04

The concept of high configurational entropy requires that the high-entropy alloys (HEAs) yield single-phase solid solutions. However, phase separations are quite common in bulk HEAs. A five-element alloy, CrCoCuFeNi, was deposited via radio frequency magnetron sputtering and confirmed to be a single-phase solid solution through the high-energy synchrotron X-ray diffraction, energy-dispersive spectroscopy, wavelength-dispersive spectroscopy, and transmission electron microscopy. The formation of the solid-solution phase is presumed to be due to the high cooling rate of the sputter-deposition process.

Anomalous Growth Rate of Ag Nanocrystals Revealed by in situ STEM

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

Ge, Mingyuan; Lu, Ming; Chu, Yong

In situ microscopy of colloidal nanocrystal growth offers a unique opportunity to acquire direct and straightforward data for assessing classical growth models. For this study, we observe the growth trajectories of individual Ag nanoparticles in solution using in situ scanning transmission electron microscopy. For the first time, we provide experimental evidence of growth rates of Ag nanoparticles in the presence of Pt in solution that are significantly faster than predicted by Lifshitz-Slyozov-Wagner theory. We attribute these observed anomalous growth rates to the synergistic effects of the catalytic properties of Pt and the electron beam itself. Transiently reduced Pt atoms servemore » as active sites for Ag ions to grow, thereby playing a key role in controlling the growth kinetics. Electron beam illumination greatly increases the local concentration of free radicals, thereby strongly influencing particle growth rate and the resulting particle morphology. Through a systematic investigation, we demonstrate the feasibility of utilizing these synergistic effects for controlling the growth rates and particle morphologies at the nanoscale. Our findings not only expand the current scope of crystal growth theory, but may also lead to a broader scientific application of nanocrystal synthesis.« less

3,4-Ethylenedioxythiophene functionalized graphene with palladium nanoparticles for enhanced electrocatalytic oxygen reduction reaction

NASA Astrophysics Data System (ADS)

Choe, Ju Eun; Ahmed, Mohammad Shamsuddin; Jeon, Seungwon

2015-05-01

Poly(3,4-ethylenedioxythiophene) functionalized graphene with palladium nanoparticles (denoted as Pd/PEDOT/rGO) has been synthesized for electrochemical oxygen reduction reaction (ORR) in alkaline solution. The structural features of catalyst are characterized by scanning electron microscopy, transmission electron microscopy (TEM), energy-dispersive X-ray spectroscopy and X-ray photoelectron spectroscopy. The TEM images suggest a well dispersed PdNPs onto PEDOT/rGO film. The ORR activity of Pd/PEDOT/rGO has been investigated via cyclic voltammetry (CV), rotating disk electrode (RDE) and rotating ring disk electrode (RRDE) techniques in 0.1 M KOH aqueous solution. Comparative CV analysis suggests a general approach of intermolecular charge-transfer in between graphene sheet and PdNPs via PEDOT which leads to the better PdNPs dispersion and subsequently superior ORR kinetics. The results from ORR measurements show that Pd/PEDOT/rGO has remarkable electrocatalytic activity and stability compared to Pd/rGO and state-of-the-art Pt/C. The Koutecky-Levich and Tafel analysis suggest that the proposed main path in the ORR mechanism has direct four-electron transfer process with faster transfer kinetic rate on the Pd/PEDOT/rGO.

Anomalous Growth Rate of Ag Nanocrystals Revealed by in situ STEM

DOE PAGES

Ge, Mingyuan; Lu, Ming; Chu, Yong; ...

2017-11-27

In situ microscopy of colloidal nanocrystal growth offers a unique opportunity to acquire direct and straightforward data for assessing classical growth models. For this study, we observe the growth trajectories of individual Ag nanoparticles in solution using in situ scanning transmission electron microscopy. For the first time, we provide experimental evidence of growth rates of Ag nanoparticles in the presence of Pt in solution that are significantly faster than predicted by Lifshitz-Slyozov-Wagner theory. We attribute these observed anomalous growth rates to the synergistic effects of the catalytic properties of Pt and the electron beam itself. Transiently reduced Pt atoms servemore » as active sites for Ag ions to grow, thereby playing a key role in controlling the growth kinetics. Electron beam illumination greatly increases the local concentration of free radicals, thereby strongly influencing particle growth rate and the resulting particle morphology. Through a systematic investigation, we demonstrate the feasibility of utilizing these synergistic effects for controlling the growth rates and particle morphologies at the nanoscale. Our findings not only expand the current scope of crystal growth theory, but may also lead to a broader scientific application of nanocrystal synthesis.« less

Facile preparation of dendritic Ag-Pd bimetallic nanostructures on the surface of Cu foil for application as a SERS-substrate

NASA Astrophysics Data System (ADS)

Yi, Zao; Tan, Xiulan; Niu, Gao; Xu, Xibin; Li, Xibo; Ye, Xin; Luo, Jiangshan; Luo, Binchi; Wu, Weidong; Tang, Yongjian; Yi, Yougen

2012-05-01

Dendritic Ag-Pd bimetallic nanostructures have been synthesized on the surface of Cu foil via a multi-stage galvanic replacement reaction (MGRR) of Ag dendrites in a Na2PdCl4 solution. After five stages of replacement reaction, one obtained structures with protruding Ag-Pd flakes; these will mature into many porous structures with a few Ag atoms that are left over dendrites. The dendritic Ag-Pd bimetallic nanostructures were characterized by transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM), field emission scanning electron microscopy (FESEM), energy-dispersive X-ray (EDX), selected area electron diffraction (SAED) and X-ray photoelectron spectroscopy (XPS). The morphology of the products strongly depended on the stage of galvanic replacement reaction and reaction temperature. The morphology and composition-dependent surface-enhanced Raman scattering (SERS) of the as-synthesized Ag-Pd bimetallic nanostructures were investigated. The effectiveness of these dendritic Ag-Pd bimetallic nanostructures on the surface of Cu foil as substrates toward SERS detection was evaluated by using rhodamine 6G (R6G) as a probe molecule. The results indicate that as-synthesized dendritic Ag-Pd bimetallic nanostructures are good candidates for SERS spectroscopy.

Acceptor Percolation Determines How Electron-Accepting Additives Modify Transport of Ambipolar Polymer Organic Field-Effect Transistors.

PubMed

Ford, Michael J; Wang, Ming; Bustillo, Karen C; Yuan, Jianyu; Nguyen, Thuc-Quyen; Bazan, Guillermo C

2018-06-18

Organic field-effect transistors (OFETs) that utilize ambipolar polymer semiconductors can benefit from the ability of both electron and hole conduction, which is necessary for complementary circuits. However, simultaneous hole and electron transport in organic field-effect transistors result in poor ON/OFF ratios, limiting potential applications. Solution processing methods have been developed to control charge transport properties and transform ambipolar conduction to hole-only conduction. The electron-acceptor phenyl-C61-butyric acid methyl ester (PC 61 BM), when mixed in solution with an ambipolar semiconducting polymer, can reduce electron conduction. Unipolar p-type OFETs with high, well-defined ON/OFF ratios and without detrimental effects on hole conduction are achieved for a wide range of blend compositions, from 95:5 to 5:95 wt % semiconductor polymer:PC 61 BM. When introducing the alternative acceptor N, N'-bis(1-ethylpropyl)-3,4:9,10-perylenediimide (PDI), high ON/OFF ratios are achieved for 95:5 wt % semiconductor polymer:PDI; however, electron conduction increases for 50:50 and 5:95 wt % semiconductor polymer:PDI. As described within, we show that electron conduction is practically eliminated when additive domains do not percolate across the OFET channel, that is, electrons are "morphologically trapped". Morphologies were characterized by optical, electron, and atomic force microscopy as well as X-ray scattering techniques. PC 61 BM was substituted with an endohedral Lu 3 N fullerene, which enhanced contrast in electron microscopy and allowed for more detailed insight into the blend morphologies. Blends with alternative, nonfullerene acceptors further emphasize the importance of morphology and acceptor percolation, providing insights for such blends that control ambipolar transport and ON/OFF ratios.

Synthesis of Al₂Ca Dispersoids by Powder Metallurgy Using a Mg-Al Alloy and CaO Particles.

PubMed

Fujita, Junji; Umeda, Junko; Kondoh, Katsuyoshi

2017-06-28

The elemental mixture of Mg-6 wt %Al-1 wt %Zn-0.3 wt %Mn (AZ61B) alloy powder and CaO particles was consolidated by an equal-channel angular bulk mechanical alloying (ECABMA) process to form a composite precursor. Subsequently, the precursor was subjected to a heat treatment to synthesize fine Al₂Ca particles via a solid-state reaction between the Mg-Al matrix and CaO additives. Scanning electron microscopy-energy-dispersive spectroscopy (SEM-EDS) and electron probe micro-analysis on the precursor indicated that 4.7-at % Al atoms formed a supersaturated solid solution in the α-Mg matrix. Transmission electron microscopy-EDS and X-ray diffraction analyses on the AZ61B composite precursor with 10-vol % CaO particles obtained by heat treatment confirmed that CaO additives were thermally decomposed in the Mg-Al alloy, and the solid-soluted Ca atoms diffused along the α-Mg grain boundaries. Al atoms also diffused to the grain boundaries because of attraction to the Ca atoms resulting from a strong reactivity between Al and Ca. As a result, needle-like (Mg,Al)₂Ca intermetallics were formed as intermediate precipitates in the initial reaction stage during the heat treatment. Finally, the precipitates were transformed into spherical Al₂Ca particles by the substitution of Al atoms for Mg atoms in (Mg,Al)₂Ca after a long heat treatment.

A comparative study of the effect of α-, β-, and γ-cyclodextrins as stabilizing agents in the synthesis of silver nanoparticles using a green chemistry method.

PubMed

Suárez-Cerda, Javier; Nuñez, Gabriel Alonso; Espinoza-Gómez, Heriberto; Flores-López, Lucía Z

2014-10-01

This paper describes the effect of different types of cyclodextrins (CDs) in the synthesis of silver nanoparticles (Ag-NPs), using an easy green chemistry method. The Ag-NPs were obtained using an aqueous silver nitrate solution (AgNO3) with α-, β-, or γ-CDs (aqueous solutions) as stabilizing agents, employing the chemical reduction method with citric acid as a reducing agent. A comparative study was done to determine which cyclodextrin (CD) was the best stabilizing agent, and we found out that β-CD was the best due to the number of glucopyranose units in its structure. The formation of the Ag-NPs was demonstrated by analysis of UV-vis spectroscopy, atomic force microscopy (AFM), scanning electron microscopy-energy dispersive spectroscopy (SEM-EDS) and transmission electron microscopy (TEM). SEM-EDS showed the formation of a cluster with a significant amount of silver, for β-CD-Ag-NPs, spherical agglomerates can be observed. However, for α-, γ-CD, the agglomerates do not have a specific form, but their appearance is porous. TEM analysis shows spherical nanoparticles in shape and size between ~0.5 to 7 nm. The clear lattice fringes in TEM images and the typical selected area electron diffraction (SAED) pattern, showed that the Ag-NPs obtained were highly crystalline with a face cubic center structure (FCC). Copyright © 2014 Elsevier B.V. All rights reserved.

Direct Observation of Protein Microcrystals in Crystallization Buffer by Atmospheric Scanning Electron Microscopy

PubMed Central

Maruyama, Yuusuke; Ebihara, Tatsuhiko; Nishiyama, Hidetoshi; Konyuba, Yuji; Senda, Miki; Numaga-Tomita, Takuro; Senda, Toshiya; Suga, Mitsuo; Sato, Chikara

2012-01-01

X-ray crystallography requires high quality crystals above a given size. This requirement not only limits the proteins to be analyzed, but also reduces the speed of the structure determination. Indeed, the tertiary structures of many physiologically important proteins remain elusive because of the so-called “crystallization bottleneck”. Once microcrystals have been obtained, crystallization conditions can be optimized to produce bigger and better crystals. However, the identification of microcrystals can be difficult due to the resolution limit of optical microscopy. Electron microscopy has sometimes been utilized instead, with the disadvantage that the microcrystals usually must be observed in vacuum, which precludes the usage for crystal screening. The atmospheric scanning electron microscope (ASEM) allows samples to be observed in solution. Here, we report the use of this instrument in combination with a special thin-membrane dish with a crystallization well. It was possible to observe protein crystals of lysozyme, lipase B and a histone chaperone TAF-Iβ in crystallization buffers, without the use of staining procedures. The smallest crystals observed with ASEM were a few μm in width, and ASEM can be used with non-transparent solutions. Furthermore, the growth of salt crystals could be monitored in the ASEM, and the difference in contrast between salt and protein crystals made it easy to distinguish between these two types of microcrystals. These results indicate that the ASEM could be an important new tool for the screening of protein microcrystals. PMID:22949879

Direct observation of protein microcrystals in crystallization buffer by atmospheric scanning electron microscopy.

PubMed

Maruyama, Yuusuke; Ebihara, Tatsuhiko; Nishiyama, Hidetoshi; Konyuba, Yuji; Senda, Miki; Numaga-Tomita, Takuro; Senda, Toshiya; Suga, Mitsuo; Sato, Chikara

2012-01-01

X-ray crystallography requires high quality crystals above a given size. This requirement not only limits the proteins to be analyzed, but also reduces the speed of the structure determination. Indeed, the tertiary structures of many physiologically important proteins remain elusive because of the so-called "crystallization bottleneck". Once microcrystals have been obtained, crystallization conditions can be optimized to produce bigger and better crystals. However, the identification of microcrystals can be difficult due to the resolution limit of optical microscopy. Electron microscopy has sometimes been utilized instead, with the disadvantage that the microcrystals usually must be observed in vacuum, which precludes the usage for crystal screening. The atmospheric scanning electron microscope (ASEM) allows samples to be observed in solution. Here, we report the use of this instrument in combination with a special thin-membrane dish with a crystallization well. It was possible to observe protein crystals of lysozyme, lipase B and a histone chaperone TAF-Iβ in crystallization buffers, without the use of staining procedures. The smallest crystals observed with ASEM were a few μm in width, and ASEM can be used with non-transparent solutions. Furthermore, the growth of salt crystals could be monitored in the ASEM, and the difference in contrast between salt and protein crystals made it easy to distinguish between these two types of microcrystals. These results indicate that the ASEM could be an important new tool for the screening of protein microcrystals.

Enhancing the stability of colloidal silver nanoparticles using polyhydroxyalkanoates (PHA) from Bacillus circulans (MTCC 8167) isolated from crude oil contaminated soil.

PubMed

Phukon, Pinkee; Saikia, Jyoti Prasad; Konwar, Bolin Kumar

2011-09-01

Polyhydroxyalkanoate (PHA) was produced by growing Bacillus circulans (MTCC 8167) in the specific detection medium. The identification of the polymer as PHA was confirmed by fluorescence microscopy. The PHA was purified and characterized using FT-IR. The silver nanoparticles (SNP) were synthesized from AgNO3 in the dispersed colloids of PHA (0.085%) using NaBH4 (sodium borohydrate as reducing agent). The stability was tested using wave length scanning with a UV-Vis spectrophotometer and finally with transmission electron microscopy. The PHA stabilized solution was found to be stable for 30 days as against the low stability of silver nanoparticles (SNP) solution alone. Copyright © 2011 Elsevier B.V. All rights reserved.

Hydrostatic Extrusion and Nano-Hardness of Nanocrystalline Grade 2 Titanium.

PubMed

Sitek, Ryszard; Kaminski, Janusz; Spychalski, Maciej; Garbacz, Halina; Pachla, Waclaw; Kurzydlowski, Krzysztof Jan

2015-07-01

The structure and corrosion resistance of Grade 2 titanium subjected to the hydroextrusion processes were examined. The microstructure was characterized using optical microscopy and transmission electron microscopy. The corrosion resistance was determined using the impedance and potentiodynamic methods, in 0.1 M H2SO4 solutions and an acidified 0.1 M NaCl solution with a pH of 4.2, at ambient temperature. Nanohardness tests were performed under a load of 100 mN. It has been demonstrated that the hydroextrusion method makes it possible to obtain relatively homogeneous nanocrystalline titanium Grade 2 with an increased hardness, the elastic modulus almost unchanged with respect to that of the initial structure and a lower corrosion resistance.

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

Chen, Limiao, E-mail: chenlimiao@csu.edu.cn; Jing, Qifeng; Chen, Jun

Silver nanostructures with dendritic, flower-like and irregular morphologies were controllably deposited on a silicon substrate in an aqueous hydrogen fluoride solution at room temperature. The morphology of the Ag nanostructures changed from dendritic to urchin-like, flowerlike and pinecone-like with increasing the concentration of polyvinyl pyrrolidone (MW = 55,000) from 2 to 10 mM. The Ag nanostructures were characterized by transmission electron microscopy, high-resolution transmission electron microscopy, scanning electron microscopy, energy-dispersive X-ray, and X-ray diffraction. Through a series of time-dependent morphological evolution studies, the growth processes of Ag nanostructures have been systematically investigated and the corresponding growth mechanisms have been discussed.more » In addition, the morphology-dependent surface-enhanced Raman scattering of as-synthesized Ag nanostructures were investigated. The results indicated that flower-like Ag nanostructure had the highest activity than the other Ag nanostructures for Rhodamine 6G probe molecules. Highlights: • A simple method was developed to prepare dendritic and flower-like Ag nanostructures. • The flower-like Ag nanoparticles exhibit highest SERS activity. • The SERS substrate based on flower-like Ag particles can be used to detect melamine.« less

Functional biocompatible magnetite-cellulose nanocomposite fibrous networks: Characterization by fourier transformed infrared spectroscopy, X-ray powder diffraction and field emission scanning electron microscopy analysis.

PubMed

Habibi, Neda

2015-02-05

The preparation and characterization of functional biocompatible magnetite-cellulose nano-composite fibrous material is described. Magnetite-cellulose nano-composite was prepared by a combination of the solution-based formation of magnetic nano-particles and subsequent coating with amino celluloses. Characterization was accomplished using X-ray powder diffraction (XRD), fourier transformed infrared (FTIR) and field emission scanning electron microscopy (FESEM) analysis. The peaks of Fe3O4 in the XRD pattern of nanocomposite confirm existence of the nanoparticles in the amino cellulose matrix. Magnetite-cellulose particles exhibit an average diameter of roughly 33nm as demonstrated by field emission scanning electron microscopy. Magnetite nanoparticles were irregular spheres dispersed in the cellulose matrix. The vibration corresponding to the NCH3 functional group about 2850cm(-1) is assigned in the FTIR spectra. Functionalized magnetite-cellulose nano-composite polymers have a potential range of application as targeted drug delivery system in biomedical field. Copyright © 2014 Elsevier B.V. All rights reserved.

Synthesis and characterization of nano TiO2-SiO2: PVA composite - a novel route

NASA Astrophysics Data System (ADS)

Venckatesh, Rajendran; Balachandaran, Kartha; Sivaraj, Rajeshwari

2012-07-01

A novel, simple, less time consuming and cost-effective sol-gel method has been developed to synthesize nano titania-silica with polyvinyl alcohol (PVA) composite relatively at low temperature in acidic pH. Titania sol is prepared by hydrolysis of titanium tetrachloride and was mixed with silicic acid and tetrahydrofuran mixture. The reaction was carried out under vigorous stirring for 6 h and dried at room temperature with the addition of PVA solution. The resulting powders were characterized by X-ray diffraction, scanning electron microscopy, transmission electron microscopy, Fourier transform infrared (FT-IR), UV-visible spectroscopy and thermal techniques. The grain size of the particles was calculated by X-ray diffraction; surface morphology and chemical composition were determined from scanning electron microscopy-energy dispersive spectroscopy; metal oxide stretching was confirmed from FT-IR spectroscopy; bandgap was calculated using UV-visible spectroscopy, and thermal stability of the prepared composite was determined by thermogravimetric/differential thermal analysis. Since TiO2 got agglomerated on the surface of SiO2, effective absorptive sites increase which in turn increase the photocatalytic efficiency of the resulting composite.

In situ microscopy of the self-assembly of branched nanocrystals in solution

DOE PAGES

Sutter, Eli; Tkachenko, Alexei V.; Sutter, Peter; ...

2016-04-04

Here, solution-phase self-assembly of nanocrystals into mesoscale structures is a promising strategy for constructing functional materials from nanoscale components. Liquid environments are key to self-assembly since they allow suspended nanocrystals to diffuse and interact freely, but they also complicate experiments. Real-time observations with single-particle resolution could have transformative impact on our understanding of nanocrystal self-assembly. Here we use real-time in situ imaging by liquid-cell electron microscopy to elucidate the nucleation and growth mechanism and properties of linear chains of octapod-shaped nanocrystals in their native solution environment. Statistical mechanics modelling based on these observations and using the measured chain-length distribution clarifiesmore » the relative importance of dipolar and entropic forces in the assembly process and gives direct access to the interparticle interaction. Our results suggest that monomer-resolved in situ imaging combined with modelling can provide unprecedented quantitative insight into the microscopic processes and interactions that govern nanocrystal self-assembly in solution.« less

In situ microscopy of the self-assembly of branched nanocrystals in solution

NASA Astrophysics Data System (ADS)

Sutter, Eli; Sutter, Peter; Tkachenko, Alexei V.; Krahne, Roman; de Graaf, Joost; Arciniegas, Milena; Manna, Liberato

2016-04-01

Solution-phase self-assembly of nanocrystals into mesoscale structures is a promising strategy for constructing functional materials from nanoscale components. Liquid environments are key to self-assembly since they allow suspended nanocrystals to diffuse and interact freely, but they also complicate experiments. Real-time observations with single-particle resolution could have transformative impact on our understanding of nanocrystal self-assembly. Here we use real-time in situ imaging by liquid-cell electron microscopy to elucidate the nucleation and growth mechanism and properties of linear chains of octapod-shaped nanocrystals in their native solution environment. Statistical mechanics modelling based on these observations and using the measured chain-length distribution clarifies the relative importance of dipolar and entropic forces in the assembly process and gives direct access to the interparticle interaction. Our results suggest that monomer-resolved in situ imaging combined with modelling can provide unprecedented quantitative insight into the microscopic processes and interactions that govern nanocrystal self-assembly in solution.

Atom probe trajectory mapping using experimental tip shape measurements.

PubMed

Haley, D; Petersen, T; Ringer, S P; Smith, G D W

2011-11-01

Atom probe tomography is an accurate analytical and imaging technique which can reconstruct the complex structure and composition of a specimen in three dimensions. Despite providing locally high spatial resolution, atom probe tomography suffers from global distortions due to a complex projection function between the specimen and detector which is different for each experiment and can change during a single run. To aid characterization of this projection function, this work demonstrates a method for the reverse projection of ions from an arbitrary projection surface in 3D space back to an atom probe tomography specimen surface. Experimental data from transmission electron microscopy tilt tomography are combined with point cloud surface reconstruction algorithms and finite element modelling to generate a mapping back to the original tip surface in a physically and experimentally motivated manner. As a case study, aluminium tips are imaged using transmission electron microscopy before and after atom probe tomography, and the specimen profiles used as input in surface reconstruction methods. This reconstruction method is a general procedure that can be used to generate mappings between a selected surface and a known tip shape using numerical solutions to the electrostatic equation, with quantitative solutions to the projection problem readily achievable in tens of minutes on a contemporary workstation. © 2011 The Authors Journal of Microscopy © 2011 Royal Microscopical Society.

Optical Fluorescence Microscopy for Spatially Characterizing Electron Transfer across a Solid-Liquid Interface on Heterogeneous Electrodes.

PubMed

Choudhary, Eric; Velmurugan, Jeyavel; Marr, James M; Liddle, James A; Szalai, Veronika

2016-01-01

Heterogeneous catalytic materials and electrodes are used for (electro)chemical transformations, including those important for energy storage and utilization. 1, 2 Due to the heterogeneous nature of these materials, activity measurements with sufficient spatial resolution are needed to obtain structure/activity correlations across the different surface features (exposed facets, step edges, lattice defects, grain boundaries, etc.). These measurements will help lead to an understanding of the underlying reaction mechanisms and enable engineering of more active materials. Because (electro)catalytic surfaces restructure with changing environments, 1 it is important to perform measurements in operando . Sub-diffraction fluorescence microscopy is well suited for these requirements because it can operate in solution with resolution down to a few nm. We have applied sub-diffraction fluorescence microscopy to a thin cell containing an electrocatalyst and a solution containing the redox sensitive dye p-aminophenyl fluorescein to characterize reaction at the solid-liquid interface. Our chosen dye switches between a nonfluorescent reduced state and a one-electron oxidized bright state, a process that occurs at the electrode surface. This scheme is used to investigate the activity differences on the surface of polycrystalline Pt, in particular to differentiate reactivity at grain faces and grain boundaries. Ultimately, this method will be extended to study other dye systems and electrode materials.

Eco-synthesis of graphene and its use in dihydronicotinamide adenine dinucleotide sensing.

PubMed

Amouzadeh Tabrizi, Mahmoud; Jalilzadeh Azar, Somayeh; Nadali Varkani, Javad

2014-09-01

In this paper, we report a green and eco-friendly approach to synthesize reduced graphene oxide (rGO) via a mild hydrothermal process using malt as a reduced agent. The proposed method is based on the reduction of graphene oxide (GO) in malt solution by making use of the reducing capability of phenolic compounds contained in malt solution. The obtained rGO was characterized by atomic force microscopy (AFM), ultraviolet-visible (UV-vis) absorption spectroscopy, X-ray diffraction spectroscopy (XRD), Raman spectroscopy, Fourier transform infrared (FTIR) spectroscopy, scanning electron microscopy (SEM), and transmission electron microscopy (TEM). Electrochemical impedance spectroscopy analysis revealed that the charge transfer resistance of rGO modified glassy carbon (GC) electrode was much lower than that of the GC electrode. The electrochemical behavior of dihydronicotinamide adenine dinucleotide (NADH) on rGO modified GC electrode was investigated by cyclic voltammetry and amperometry. Electrochemical experiments indicated that rGO/GC electrode exhibited excellent electrocatalytic activity toward the NADH, which can be attributed to excellent electrical conductivity and high specific surface area of the rGO composite. The resulting biosensor showed highly sensitive amperometric response to NADH with a low detection limit (0.33μM). Copyright © 2014 Elsevier Inc. All rights reserved.

Development of a physical and electronic model for RuO 2 nanorod rectenna devices

NASA Astrophysics Data System (ADS)

Dao, Justin

Ruthenium oxide (RuO2) nanorods are an emergent technology in nanostructure devices. As the physical size of electronics approaches a critical lower limit, alternative solutions to further device miniaturization are currently under investigation. Thin-film nanorod growth is an interesting technology, being investigated for use in wireless communications, sensor systems, and alternative energy applications. In this investigation, self-assembled RuO2 nanorods are grown on a variety of substrates via a high density plasma, reactive sputtering process. Nanorods have been found to grow on substrates that form native oxide layers when exposed to air, namely silicon, aluminum, and titanium. Samples were analyzed with Scanning Electron Microscopy (SEM) and Transmission Electron Microscopy (TEM) techniques. Conductive Atomic Force Microscopy (C-AFM) measurements were performed on single nanorods to characterize structure and electrical conductivity. The C-AFM probe tip is placed on a single nanorod and I-V characteristics are measured, potentially exhibiting rectifying capabilities. An analysis of these results using fundamental semiconductor physics principles is presented. Experimental data for silicon substrates was most closely approximated by the Simmons model for direct electron tunneling, whereas that of aluminum substrates was well approximated by Fowler-Nordheim tunneling. The native oxide of titanium is regarded as a semiconductor rather than an insulator and its ability to function as a rectifier is not strong. An electronic model for these nanorods is described herein.

Determination of precursor sites for pitting corrosion of polycrystalline titanium by using different techniques

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

Garfias-Mesias, L.F.; Alodan, M.; James, P.I.

1998-06-01

Scanning electrochemical microscopy (SECM) in ferrocyanide and bromide solutions was used to locate active sites (pitting precursors) on polycrystalline Ti where oxidation of Br{sup {minus}} and Fe(CN){sub 6}{sup 4{minus}} was possible. Analysis of the electrochemically active sites was done by using electron microscopy (SEM), energy dispersive X-ray analysis (EDX), atomic force microscopy (AFM), and in situ confocal laser scanning microscopy (CLSM). In most cases, the active sites were found to be associated with particles (inclusions) which contained mainly Al and Si; however, some other areas not associated with particles were also found to be active. Although the size of themore » inclusions was normally smaller than 20 {micro}m, as revealed by SEM and AFM imaging, in some cases larger particles were also found. Pitting corrosion tests in bromide solution at potentials above 1.5 V{sub SCE} followed by EDX analysis inside the pits and in situ CLSM observation, confirmed that most of the localized attack started in the areas where particles had been located.« less

Room temperature synthesis of rutile nanorods and their applications on cloth

NASA Astrophysics Data System (ADS)

Fei, Bin; Deng, Zhaoxiang; Xin, John H.; Zhang, Yihe; Pang, Geoffrey

2006-04-01

In order to achieve better photocatalytic performance, rutile nanorods dispersed in anatase and brookite phases were synthesized from titanium isopropoxide (TIP) in a concentrated HNO3 solution at room temperature (23 °C). X-ray diffraction results indicated that the percentage of rutile increased with increasing peptization time. Scanning electron microscopy and and high-resolution transmission electron microscopy measurements revealed that the nanosized titania particles mainly consisted of granular anatase and brookite, and rod-like rutile. It was interesting that the stability of the colloid increased with increasing nanoparticle concentration, and the tricrystalline titania showed a photocatalytic activity higher than that of pure anatase. These nanocrystals were applied onto cotton fabrics, and achieved a promising bactericidal photocatalytic activity and excellent protection against UV radiation.

Synthesis of TiO2 nanoparticles by hydrolysis and peptization of titanium isopropoxide solution

NASA Astrophysics Data System (ADS)

Mahata, S.; Mahato, S. S.; Nandi, M. M.; Mondal, B.

2012-07-01

Here we report the synthesis and characterization of a stable suspension of modified titania nanoparticles. Phase-pure TiO2 nanocrystallites with narrow particle-size distributions were selectively prepared by hydrolysis-peptization of modified alkoxide followed by hydrothermal treatment. Autoclaving modified TiO2 in the presence of HNO3 as cooperative catalysts led to the formation of crystalline TiO2 with narrow-sized distribution. Following the hydrothermal treatment at 150°C, X-ray diffraction shows the particles to be exclusively anatase. Synthesized powder is characterized by FT-IR, scanning electron microscopy (FESEM) and transmission electron microscopy (HRTEM). The photocatalytic activity in the degradation of orange-II is quite comparable to good anatase and rutile nanocrystallites.

Synthesis of noble metal/carbon nanotube composites in supercritical methanol.

PubMed

Sun, Zhenyu; Fu, Lei; Liu, Zhimin; Han, Buxing; Liu, Yunqi; Du, Jimin

2006-03-01

A simple and efficient route has been employed to deposit noble metal nanoparticles (Pt, Ru, Pt-Ru, Rh, Ru-Sn) onto carbon nanotubes (CNTs) in supercritical methanol solution. In this method, the inorganic metallic salts acted as metal precursors, and methanol as solvent as well as reductant for the precursors. The as-prepared nanocomposites were structurally and morphologically characterized by X-ray diffraction spectroscopy, transmission electron microscopy (TEM), scanning electron microscopy, and X-ray photoelectron spectroscopy analyses. It was demonstrated that the CNTs were decorated by crystalline metal nanoparticles with uniform sizes and a narrow particle size distribution. The size and loading content of the nanoparticles on CNTs could be tuned by manipulating reaction parameters. Furthermore, the formation mechanism of the composites was also discussed.

Biosynthesis and characterization of silver nanoparticles prepared from two novel natural precursors by facile thermal decomposition methods

NASA Astrophysics Data System (ADS)

Goudarzi, Mojgan; Mir, Noshin; Mousavi-Kamazani, Mehdi; Bagheri, Samira; Salavati-Niasari, Masoud

2016-09-01

In this work, two natural sources, including pomegranate peel extract and cochineal dye were employed for the synthesis of silver nanoparticles. The natural silver complex from pomegranate peel extract resulted in nano-sized structures through solution-phase method, but this method was not efficient for cochineal dye-silver precursor and the as-formed products were highly agglomerated. Therefore, an alternative facile solid-state approach was investigated as for both natural precursors and the results showed successful production of well-dispersed nanoparticles with narrow size distribution for cochineal dye-silver precursor. The products were characterized by X-ray diffraction (XRD), Scanning Electron Microscopy (SEM), Energy dispersive X-ray microanalysis (EDX), and Transmission Electron Microscopy (TEM).

Three-dimensional nanoscale imaging by plasmonic Brownian microscopy

NASA Astrophysics Data System (ADS)

Labno, Anna; Gladden, Christopher; Kim, Jeongmin; Lu, Dylan; Yin, Xiaobo; Wang, Yuan; Liu, Zhaowei; Zhang, Xiang

2017-12-01

Three-dimensional (3D) imaging at the nanoscale is a key to understanding of nanomaterials and complex systems. While scanning probe microscopy (SPM) has been the workhorse of nanoscale metrology, its slow scanning speed by a single probe tip can limit the application of SPM to wide-field imaging of 3D complex nanostructures. Both electron microscopy and optical tomography allow 3D imaging, but are limited to the use in vacuum environment due to electron scattering and to optical resolution in micron scales, respectively. Here we demonstrate plasmonic Brownian microscopy (PBM) as a way to improve the imaging speed of SPM. Unlike photonic force microscopy where a single trapped particle is used for a serial scanning, PBM utilizes a massive number of plasmonic nanoparticles (NPs) under Brownian diffusion in solution to scan in parallel around the unlabeled sample object. The motion of NPs under an evanescent field is three-dimensionally localized to reconstruct the super-resolution topology of 3D dielectric objects. Our method allows high throughput imaging of complex 3D structures over a large field of view, even with internal structures such as cavities that cannot be accessed by conventional mechanical tips in SPM.

Reclamation of niobium compounds from ionic liquid electrochemical polishing of superconducting radio frequency cavities

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

Wixtrom, Alex I.; Buhler, Jessica E.; Reece, Charles E.

2013-06-01

Recent research has shown that choline chloride (vitamin B4)-based solutions can be used as a greener alternative to acid-based electrochemical polishing solutions. This study demonstrated a successful method for electrochemical deposition of niobium compounds onto the surface of copper substrates using a novel choline chloride-based ionic liquid. Niobium ions present in the ionic liquid solution were dissolved into the solution prior to deposition via electrochemical polishing of solid niobium. A black coating was clearly visible on the surface of the Cu following deposition. This coating was analyzed using scanning electron microscopy (SEM), electron dispersive X-ray spectroscopy (EDX), atomic force microscopymore » (AFM), and X-ray fluorescence spectroscopy (XRF). This ionic liquid-based electrochemical deposition method effectively recycles previously dissolved niobium from electrochemical polishing of superconducting radio frequency (SRF) cavities.« less

Synthesis of oxocarbon-encapsulated gold nanoparticles with blue-shifted localized surface plasmon resonance by pulsed laser ablation in water with CO2 absorbers

NASA Astrophysics Data System (ADS)

Del Rosso, T.; Rey, N. A.; Rosado, T.; Landi, S.; Larrude, D. G.; Romani, E. C.; Freire Junior, F. L.; Quinteiro, S. M.; Cremona, M.; Aucelio, R. Q.; Margheri, G.; Pandoli, O.

2016-06-01

Colloidal suspensions of oxocarbon-encapsulated gold nanoparticles have been synthesized in a one-step procedure by pulsed-laser ablation (PLA) at 532 nm of a solid gold target placed in aqueous solution containing CO2 absorbers, but without any stabilizing agent. Multi-wavelength surface enhanced Raman spectroscopy allows the identification of adsorbed amorphous carbon and graphite, Au-carbonyl, Au coordinated CO2-derived bicarbonates/carbonates and hydroxyl groups around the AuNPs core. Scanning electron microscopy, energy dispersive x-ray analysis and high resolution transmission electron microscopy highlight the organic shell structure around the crystalline metal core. The stability of the colloidal solution of nanocomposites (NCs) seems to be driven by solvation forces and is achieved only in neutral or basic pH using monovalent hydroxide counter-ions (NaOH, KOH). The NCs are characterized by a blue shift of the localized surface plasmon resonance (LSPR) band typical of metal-ligand stabilization by terminal π-back bonding, attributed to a core charging effect caused by Au-carbonyls. Total organic carbon measurements detect the final content of organic carbon in the colloidal solution of NCs that is about six times higher than the value of the water solution used to perform PLA. The colloidal dispersions of NCs are stable for months and are applied as analytical probes in amino glycoside antibiotic LSPR based sensing.

Synthesis of oxocarbon-encapsulated gold nanoparticles with blue-shifted localized surface plasmon resonance by pulsed laser ablation in water with CO2 absorbers.

PubMed

Del Rosso, T; Rey, N A; Rosado, T; Landi, S; Larrude, D G; Romani, E C; Junior, F L Freire; Quinteiro, S M; Cremona, M; Aucelio, R Q; Margheri, G; Pandoli, O

2016-06-24

Colloidal suspensions of oxocarbon-encapsulated gold nanoparticles have been synthesized in a one-step procedure by pulsed-laser ablation (PLA) at 532 nm of a solid gold target placed in aqueous solution containing CO2 absorbers, but without any stabilizing agent. Multi-wavelength surface enhanced Raman spectroscopy allows the identification of adsorbed amorphous carbon and graphite, Au-carbonyl, Au coordinated CO2-derived bicarbonates/carbonates and hydroxyl groups around the AuNPs core. Scanning electron microscopy, energy dispersive x-ray analysis and high resolution transmission electron microscopy highlight the organic shell structure around the crystalline metal core. The stability of the colloidal solution of nanocomposites (NCs) seems to be driven by solvation forces and is achieved only in neutral or basic pH using monovalent hydroxide counter-ions (NaOH, KOH). The NCs are characterized by a blue shift of the localized surface plasmon resonance (LSPR) band typical of metal-ligand stabilization by terminal π-back bonding, attributed to a core charging effect caused by Au-carbonyls. Total organic carbon measurements detect the final content of organic carbon in the colloidal solution of NCs that is about six times higher than the value of the water solution used to perform PLA. The colloidal dispersions of NCs are stable for months and are applied as analytical probes in amino glycoside antibiotic LSPR based sensing.

Polymer Self-Assembly into Unique Fractal Nanostructures in Solution by a One-Shot Synthetic Procedure.

PubMed

Shin, Suyong; Gu, Ming-Long; Yu, Chin-Yang; Jeon, Jongseol; Lee, Eunji; Choi, Tae-Lim

2018-01-10

A fractal nanostructure having a high surface area is potentially useful in sensors, catalysts, functional coatings, and biomedical and electronic applications. Preparation of fractal nanostructures on solid substrates has been reported using various inorganic or organic compounds. However, achieving such a process using polymers in solution has been extremely challenging. Here, we report a simple one-shot preparation of polymer fractal nanostructures in solution via an unprecedented assembly mechanism controlled by polymerization and self-assembly kinetics. This was possible only because one monomer was significantly more reactive than the other, thereby easily forming a diblock copolymer microstructure. Then, the second insoluble block containing poly(p-phenylenevinylene) (PPV) without any side chains spontaneously underwent self-assembly during polymerization by an in situ nanoparticlization of conjugated polymers (INCP) method. The formation of fractal structures in solution was confirmed by various imaging techniques such as atomic force microscopy, transmission electron microscopy (TEM), and cryogenic TEM. The diffusion-limited aggregation theory was adopted to explain the branching patterns of the fractal nanostructures according to the changes in polymerization conditions such as the monomer concentration and the presence of additives. Finally, after detailed kinetic analyses, we proposed a plausible mechanism for the formation of unique fractal nanostructures, where the gradual formation and continuous growth of micelles in a chain-growth-like manner were accounted for.

Simple glucose reduction route for one-step synthesis of copper nanofluids

NASA Astrophysics Data System (ADS)

Shenoy, U. Sandhya; Shetty, A. Nityananda

2014-01-01

One-step method has been employed in the synthesis of copper nanofluids. Copper nitrate is reduced by glucose in the presence of sodium lauryl sulfate. The synthesized particles are characterized by X-ray diffraction technique for the phase structure; electron diffraction X-ray analysis for chemical composition; transmission electron microscopy and field emission scanning electron microscopy for the morphology; Fourier-transform infrared spectroscopy and ultraviolet-visible spectroscopy for the analysis of ingredients of the solution. Thermal conductivity, sedimentation and rheological measurements have also been carried out. It is found that the reaction parameters have considerable effect on the size of the particle formed and rate of the reaction. The techniques confirm that the synthesized particles are copper. The reported method showed promising increase in the thermal conductivity of the base fluid and is found to be reliable, simple and cost-effective method for preparing heat transfer fluids with higher stability.

Synthesis and characterization of nanocrystalline Co-Fe-Nb-Ta-B alloy

NASA Astrophysics Data System (ADS)

Raanaei, Hossein; Fakhraee, Morteza

2017-09-01

In this research work, structural and magnetic evolution of Co57Fe13Nb8Ta4B18 alloy, during mechanical alloying process, have been investigated by using, X-ray diffraction, scanning electron microscopy, transmission electron microscopy, electron dispersive X-ray spectroscopy, differential thermal analysis and also vibrating sample magnetometer. It is observed that at 120 milling time, the crystallite size reaches to about 7.8 nm. Structural analyses show that, the solid solution of the initial powder mixture occurs at160 h milling time. The coercivity behavior demonstrates a rise, up to 70 h followed by decreasing tendency up to final stage of milling process. Thermal analysis of 160 h milling time sample reveals two endothermic peaks. The characterization of annealed milled sample for 160 h milling time at 427 °C shows crystallite size growth accompanied by increasing in saturation magnetization.

Rare earth ions doped ZnO: Synthesis, characterization and preliminary photoactivity assessment

NASA Astrophysics Data System (ADS)

Cerrato, Erik; Gionco, Chiara; Berruti, Ilaria; Sordello, Fabrizio; Calza, Paola; Paganini, Maria Cristina

2018-08-01

This work reports the effect of doping zinc oxide with lanthanide ions on structural, EPR and UV visible properties. Bare and doped samples were synthesized using the simple and green hydrothermal process. Different rare earth ions (RE = La, Ce, Pr, Er and Yb) with 1% molar ratio RE/Zn were used. The samples have been studied using X Ray Diffraction, Scanning Electron Microscopy (SEM), Transmission Electron Microscopy (TEM) and UV visible diffuse reflectance spectroscopy. Finally, electron paramagnetic resonance (EPR) spectroscopy, was used to assess the materials photoactivity under UV irradiation, both in solid state, to see the charge carriers' generation and in solution, evaluating the OH• radical formation using the DMPO (5,5-Dimethyl-1-Pyrroline-N-Oxide) spin trapping technique. The results suggest that the synthesized materials could be interesting systems for the photocatalytic abatement of emerging organic persistent pollutants in wastewater treatment plants.

Surface alloying of aluminum with molybdenum by high-current pulsed electron beam

NASA Astrophysics Data System (ADS)

Xia, Han; Zhang, Conglin; Lv, Peng; Cai, Jie; Jin, Yunxue; Guan, Qingfeng

2018-02-01

The surface alloying of pre-coated molybdenum (Mo) film on aluminum (Al) substrate by high-current pulsed electron beam (HCPEB) was investigated. The microstructure and phase analysis were conducted by X-ray diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The results show that Mo particles were dissolved into Al matrix to form alloying layer, which was composed of Mo, Al and acicular or equiaxed Al5Mo phases after surface alloying. Meanwhile, various structure defects such as dislocation loops, high-density dislocations and dislocation walls were observed in the alloying surface. The corrosion resistance was tested by using potentiodynamic polarization curves and electrochemical impedance spectra (EIS). Electrochemical results indicate that all the alloying samples had better corrosion resistance in 3.5 wt% NaCl solution compared to initial sample. The excellent corrosion resistance is mainly attributed to the combined effect of the structure defects and the addition of Mo element to form a more stable passive film.

Phase change in CoTi2 induced by MeV electron irradiation

NASA Astrophysics Data System (ADS)

Zensho, Akihiro; Sato, Kazuhisa; Yasuda, Hidehiro; Mori, Hirotaro

2018-07-01

The phase change induced by MeV electron irradiation in the intermetallic compound E93-CoTi2 was investigated using high-voltage electron microscopy. Under MeV electron irradiation, CoTi2 was first transformed into an amorphous phase and, with continued irradiation, crystallite formation in the amorphous phase (i.e. formation of crystallites of a solid-solution phase within the amorphous phase) was induced. The critical temperature for amorphisation was around 250 K. The total dose (dpa) required for crystallite formation (i.e. that required for partial crystallisation) was high (i.e. 27-80 dpa) and, even after prolonged irradiation, the amorphous phase was retained in the irradiated sample. Such partial crystallisation behaviour of amorphous Co33Ti67 was clearly different from the crystallisation behaviour (i.e. amorphous-to-solid solution, polymorphous transformation) of amorphous Cr67Ti33 reported in the literature. A possible cause of the difference is discussed.

New methods allowing the detection of protein aggregates

PubMed Central

Demeule, Barthélemy; Palais, Caroline; Machaidze, Gia; Gurny, Robert

2009-01-01

Aggregation compromises the safety and efficacy of therapeutic proteins. According to the manufacturer, the therapeutic immunoglobulin trastuzumab (Herceptin®) should be diluted in 0.9% sodium chloride before administration. Dilution in 5% dextrose solutions is prohibited. The reason for the interdiction is not mentioned in the Food and Drug Administration (FDA) documentation, but the European Medicines Agency (EMEA) Summary of Product Characteristics states that dilution of trastuzumab in dextrose solutions results in protein aggregation. In this paper, asymmetrical flow field-flow fractionation (FFF), fluorescence spectroscopy, fluorescence microscopy and transmission electron microscopy (TEM) have been used to characterize trastuzumab samples diluted in 0.9% sodium chloride, a stable infusion solution, as well as in 5% dextrose (a solution prone to aggregation). When trastuzumab samples were injected in the FFF channel using a standard separation method, no difference could be seen between trastuzumab diluted in sodium chloride and trastuzumab diluted in dextrose. However, during FFF measurements made with appropriate protocols, aggregates were detected in 5% dextrose. The parameters enabling the detection of reversible trastuzumab aggregates are described. Aggregates could also be documented by fluorescence microscopy and TEM. Fluorescence spectroscopy data were indicative of conformational changes consistent with increased aggregation and adsorption to surfaces. The analytical methods presented in this study were able to detect and characterize trastuzumab aggregates. PMID:20061815

Solid state amorphization of metastable Al 0.5TiZrPdCuNi high entropy alloy investigated by high voltage electron microscopy

DOE PAGES

Nagase, Takeshi; Takeuchi, Akira; Amiya, Kenji; ...

2017-07-18

Here, the phase stability of high entropy alloy (HEA), Al 0.5TiZrPdCuNi, under fast electron irradiation was studied by in-situ high voltage electron microscopy (HVEM). The initial phase of this alloy quenched from the melt was dependent on cooling rate. At high cooling rates an amorphous phase was obtained, whereas a body-centered cubic ( b.c.c.) phase were obtained at low cooling rates. By thermal crystallization of the amorphous phase b.c.c. phase nano-crystals were formed. Upon fast electron irradiation solid state amorphization (SSA) was observed in b.c.c. phase regardless of the initial microstructure (i.e., “coarse crystalline structure” or “nano-crystalline structure with grainmore » boundaries as a sink for point defects”). SSA behavior in the Al 0.5TiZrPdCuNi HEAs was investigated by in-situ transmission electron microscopy observations. Because the amorphization is very rarely achieved in a solid solution phase under fast electron irradiation in common metallic materials, this result suggests that the Al 0.5TiZrPdCuNi HEA from other common alloys and the other HEAs. The differences in phase stability against the irradiation between the Al 0.5TiZrPdCuNi HEA and the other HEAs were discussed. This is the first experimental evidence of SSA in HEAs stimulated by fast electron irradiation.« less

Growth and characterization of organic layers deposited on porous-patterned Si surface

NASA Astrophysics Data System (ADS)

Gorbach, Tamara Ya.; Smertenko, Petro S.; Olkhovik, G. P.; Wisz, Grzegorz

2017-01-01

The organic layers with the thickness from a few nanometers up to few micrometers have been deposited from the chemical solution at room temperature on porous patterned Si surfaces using two medical solutions: thiamine diphosphide (pH=1÷2) and metamizole sodium (pH=6÷7). Based on evolution of morphology, structural and compositional features obtained by scanning electron microscopy, X-ray analysis, reflectance high energy electron diffraction the grown mechanisms in thin organic layers are discussed in the terms of terrace-step-kink model whereas self-organized assemblies evaluated more thick layers. Transport mechanism features and possible photovoltaic properties are discussed on the base of differential current-voltage characteristics.

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

NASA Astrophysics Data System (ADS)

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

2014-09-01

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

Platinum blue as an alternative to uranyl acetate for staining in transmission electron microscopy.

PubMed

Inaga, Sumire; Katsumoto, Tetsuo; Tanaka, Keiichi; Kameie, Toshio; Nakane, Hironobu; Naguro, Tomonori

2007-04-01

This paper introduces an aqueous solution of platinum blue (Pt-blue) as an alternative to uranyl acetate (UA) for staining in transmission electron microscopy (TEM). Pt-blue was prepared from a reaction of cis-dichlorodiamine-platinum (II) (cis-platin) with thymidine. When Pt-blue was dried on a microgrid and observed by TEM it showed a uniform appearance with tiny particles less than 1 nm in diameter. The effect of Pt-blue as an electron stain was then examined not only for positive staining of conventional ultrathin resin sections and counterstaining of post-embedding immuno-electron microscopy but also for negative staining. In ultrathin sections of the rat liver and renal glomerulus, Pt-blue provided good contrast images, especially in double staining combined with a lead stain (Pb). Almost all cell organelles were clearly observed with high contrast in these sections. Glycogen granules in the hepatic parenchymal cells were particularly electron dense in Pt-blue stained sections compared with those treated with UA. In longitudinal and transverse sections of budding influenza A viruses, a specific arrangement of rod-like structures, which correspond to the ribonucleoprotein complexes, was clearly shown in each virion stained with Pt-blue and Pb. When post-embedding immunoelectron microscopy was performed in ultrathin sections of HeLa cells embedded in Lowicryl K4M, the localization of Ki-67 protein was sufficiently detected even after Pt-blue and Pb staining. The present study also revealed that Pt-blue could be used for the negative staining of E. coli, allowing the visualization of a flagellum. These findings indicate that Pt-blue is a useful, safe, and easily obtainable electron stain that is an alternative to UA for TEM preparations.

Iodine Vapor Staining for Atomic Number Contrast in Backscattered Electron and X-ray Imaging

PubMed Central

Boyde, Alan; Mccorkell, Fergus A; Taylor, Graham K; Bomphrey, Richard J; Doube, Michael

2014-01-01

Iodine imparts strong contrast to objects imaged with electrons and X-rays due to its high atomic number (53), and is widely used in liquid form as a microscopic stain and clinical contrast agent. We have developed a simple technique which exploits elemental iodine's sublimation-deposition state-change equilibrium to vapor stain specimens with iodine gas. Specimens are enclosed in a gas-tight container along with a small mass of solid I2. The bottle is left at ambient laboratory conditions while staining proceeds until empirically determined completion (typically days to weeks). We demonstrate the utility of iodine vapor staining by applying it to resin-embedded tissue blocks and whole locusts and imaging them with backscattered electron scanning electron microscopy (BSE SEM) or X-ray microtomography (XMT). Contrast is comparable to that achieved with liquid staining but without the consequent tissue shrinkage, stain pooling, or uneven coverage artefacts associated with immersing the specimen in iodine solutions. Unmineralized tissue histology can be read in BSE SEM images with good discrimination between tissue components. Organs within the locust head are readily distinguished in XMT images with particularly useful contrast in the chitin exoskeleton, muscle and nerves. Here, we have used iodine vapor staining for two imaging modalities in frequent use in our laboratories and on the specimen types with which we work. It is likely to be equally convenient for a wide range of specimens, and for other modalities which generate contrast from electron- and photon-sample interactions, such as transmission electron microscopy and light microscopy. Microsc. Res. Tech. 77:1044–1051, 2014. © 2014 The Authors. Microscopy Research Technique published by Wiley Periodocals, Inc. PMID:25219801

[The corrosion of pure iron in five different mediums].

PubMed

Xu, Li; Zhu, Shengfa; Huang, Nan; Li, Xinchang; Zhang, Yu

2009-08-01

The sectional test was adopted in this study to investigate the corrosion of pure iron in 0.15 mol/L NaCl solution, Ringer solution, PBS(-) solution, SBF solution and M199 cell culture medium at three different times. The result shows that different mediums have different corrosion effects on pure iron. The arrangement according to the medium's corrosion ability from the strongest to weakest is 0.15 mol/L NaCl solution (Ringer solution), PBS(-) solution, SBF solution and M199 cell culture medium. The results of scanning electron microscopy and energy dispersive X-ray spectrum analyses show that the addition of HPO4(2-), H2POC4-, Ca2+, Mg2+, SO4(2-) and the organic component can inhibit the corrosion to some degree.

Deposition of tetracene thin films on SiO2/Si substrates by rapid expansion of supercritical solutions using carbon dioxide

NASA Astrophysics Data System (ADS)

Fujii, Tatsuya; Takahashi, Yuta; Uchida, Hirohisa

2015-03-01

We report on a novel deposition technique of tetracene (naphthacene) thin films on SiO2/Si substrates by rapid expansion of supercritical solutions (RESS) using CO2. Optical microscopy and scanning electron microscopy show that the thin films consist of a high density of submicron-sized grains. The growth mode of the grains followed the Volmer-Weber mode. X-ray diffraction shows that the thin films have regularly arranged structures in both the horizontal and vertical directions of the substrate. A fabricated top-contacted organic thin-film transistor with the tetracene active layer showed p-type transistor characteristics with a field-effect mobility of 5.1 × 10-4 cm2 V-1 s-1.

Investigation of manifestation of optical properties of butterfly wings with nanoscale zinc oxide incorporation

NASA Astrophysics Data System (ADS)

Aideo, Swati N.; Mohanta, Dambarudhar

2016-10-01

In this work, microstructural and optical characteristics nanoparticles of wings of Tailed Jay (Graphium Agamemnon) butterfly were studied before and after treating it in a precursor solution of zinc acetate and ethanol. We speculate that the butterfly scales are infiltrated with ZnO nanoparticles owing to reduction of Zinc hydroxide under ambient condition. The ZnO butterfly scales so produced were characterised using optical microscopy, UV-Vis reflectance spectroscopy, and electron microscopy etc. From the reflectance spectra, we could see that after treating it in the solution, optical properties vary. We anticipate that this change may be due to the formation of ZnO nanoparticles as well as the loss in periodicity due to the chemical treatments, which could be assessed from the SEM micrographs.

Microstructure and properties of ultrafine grain nickel 200 after hydrostatic extrusion processes

NASA Astrophysics Data System (ADS)

Sitek, R.; Krajewski, C.; Kamiński, J.; Spychalski, M.; Garbacz, H.; Pachla, W.; Kurzydłowski, K. J.

2012-09-01

This paper presents the results of the studies of the structure and properties of ultrafine grained nickel 200 obtained by hydrostatic extrusion processes. Microstructure was characterized by means of optical microscopy and electron transmission microscopy. Corrosion resistance was studied by impedance and potentiodynamic methods using an AutoLab PGSTAT 100 potentiostat in 0.1 M Na2SO4 solution and in acidified (by addition of H2SO4) 0.1 M NaCl solution at pH = 4.2 at room temperature. Microhardness tests were also performed. The results showed that hydrostatic extrusion produces a heterogeneous, ultrafine-grained microstructure in nickel 200. The corrosive resistance tests showed that the grain refinement by hydrostatic extrusion is accompanied by a decreased corrosive resistance of nickel 200.

Aberration corrected STEM by means of diffraction gratings

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

Linck, Martin; Ercius, Peter A.; Pierce, Jordan S.

In the past 15 years, the advent of aberration correction technology in electron microscopy has enabled materials analysis on the atomic scale. This is made possible by precise arrangements of multipole electrodes and magnetic solenoids to compensate the aberrations inherent to any focusing element of an electron microscope. In this paper, we describe an alternative method to correct for the spherical aberration of the objective lens in scanning transmission electron microscopy (STEM) using a passive, nanofabricated diffractive optical element. This holographic device is installed in the probe forming aperture of a conventional electron microscope and can be designed to removemore » arbitrarily complex aberrations from the electron's wave front. In this work, we show a proof-of-principle experiment that demonstrates successful correction of the spherical aberration in STEM by means of such a grating corrector (GCOR). Our GCOR enables us to record aberration-corrected high-resolution high-angle annular dark field (HAADF-) STEM images, although yet without advancement in probe current and resolution. Finally, improvements in this technology could provide an economical solution for aberration-corrected high-resolution STEM in certain use scenarios.« less

Aberration corrected STEM by means of diffraction gratings

DOE PAGES

Linck, Martin; Ercius, Peter A.; Pierce, Jordan S.; ...

2017-06-12

In the past 15 years, the advent of aberration correction technology in electron microscopy has enabled materials analysis on the atomic scale. This is made possible by precise arrangements of multipole electrodes and magnetic solenoids to compensate the aberrations inherent to any focusing element of an electron microscope. In this paper, we describe an alternative method to correct for the spherical aberration of the objective lens in scanning transmission electron microscopy (STEM) using a passive, nanofabricated diffractive optical element. This holographic device is installed in the probe forming aperture of a conventional electron microscope and can be designed to removemore » arbitrarily complex aberrations from the electron's wave front. In this work, we show a proof-of-principle experiment that demonstrates successful correction of the spherical aberration in STEM by means of such a grating corrector (GCOR). Our GCOR enables us to record aberration-corrected high-resolution high-angle annular dark field (HAADF-) STEM images, although yet without advancement in probe current and resolution. Finally, improvements in this technology could provide an economical solution for aberration-corrected high-resolution STEM in certain use scenarios.« less

Effect of Cooling Rates on γ → α Transformation and Metastable States in Fe-Cu Alloys with Addition of Ni

NASA Astrophysics Data System (ADS)

Crozet, C.; Verdier, M.; Lay, S.; Antoni-Zdziobek, A.

2018-07-01

α/γ phase transformations occurring in Fe-10Cu-xNi alloys (0 ≤ x ≤ 15 in mass%) were studied using X-ray diffraction, scanning electron microscopy, electron back scattered diffraction, transmission electron microscopy and chemical analysis, combining X-ray microanalysis with energy dispersive spectrometry in the scanning electron microscope and electron microprobe analysis with wavelength dispersive spectrometry. The influence of cooling rate on the microstructure was investigated using ice-brine quenching and 2 °C/min slow cooling rate performed with dilatometry. Ni addition induces metastable transformations on cooling: massive and bainitic ferrite are formed depending on the alloy composition and cooling rate. Moreover, most of the Cu phase precipitates on cooling giving rise to a fine distribution of Cu particles in the ferrite grains. For both cooling conditions, the hardness increases with increasing Ni content and a higher hardness is obtained in the quenched alloy for each composition. The change in hardness is correlated to the effect of Ni solid solution, transformation structure and size of Cu particles.

Reinforcing Natural Rubber with Cellulose Nanofibrils Extracted from Bleached Eucalyptus Kraft Pulp

Treesearch

Chunmei Zhang; Tianliang Zhai; Ronald Sabo; Craig Clemons; Yi Dan; Lih-Sheng Turng

2014-01-01

Reinforced natural rubber (NR) nanocomposites were prepared by solution mixing, casting, and evaporation of pre-vulcanized natural rubber latex and an aqueous suspension of cellulose nanofibrils (CNFs) extracted from bleached eucalyptus kraft pulp. Scanning electron microscopy (SEM) images showed that there were no micro-scaled aggregates observed in the nanocomposites...

Scanning tunneling microscopy of atomically precise graphene nanoribbons exfoliated onto H:Si(100)

NASA Astrophysics Data System (ADS)

Radocea, Adrian; Mehdi Pour, Mohammad; Vo, Timothy; Shekhirev, Mikhail; Sinitskii, Alexander; Lyding, Joseph

Atomically precise graphene nanoribbons (GNRs) are promising materials for next generation transistors due to their well-controlled bandgaps and the high thermal conductivity of graphene. The solution synthesis of graphene nanoribbons offers a pathway towards scalable manufacturing. While scanning tunneling microscopy (STM) can access size scales required for characterization, solvent residue increases experimental difficulty and precludes band-gap determination via scanning tunneling spectroscopy (STS). Our work addresses this challenge through a dry contact transfer method that cleanly transfers solution-synthesized GNRs onto H:Si(100) under UHV using a fiberglass applicator. The semiconducting silicon surface avoids problems with image charge screening enabling intrinsic bandgap measurements. We characterize the nanoribbons using STM and STS. For chevron GNRs, we find a 1.6 eV bandgap, in agreement with computational modeling, and map the electronic structure spatially with detailed spectra lines and current imaging tunneling spectroscopy. Mapping the electronic structure of graphene nanoribbons is an important step towards taking advantage of the ability to form atomically precise nanoribbons and finely tune their properties.

Simple solution-combustion synthesis of Ni-NiO@C nanocomposites with highly electrocatalytic activity for methanol oxidation

NASA Astrophysics Data System (ADS)

Yu, Jie; Ni, Yonghong; Zhai, Muheng

2018-01-01

Transition metal and its oxide composite nanomaterials are attracting increasing research interest due to their superior properties and extensive applications in many fields. In this paper, Ni-NiO@C nanocomposites were successfully synthesized in one step via a simple solution-combustion route, employing NiCl2 as the Ni source, oxygen in the atmosphere as the oxygen source, and ethanol as the solvent. The final product was characterized by powder X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM), energy dispersive X-ray spectrometry (EDS), (high resolution) transmission electron microscopy (TEM/HRTEM), and Raman spectra. N2 gas sorption-desorption experiments uncovered that the BET surface area of Ni-NiO@C nanocomposites reached 161.9 m2 g-1, far higher than 34.2 m2 g-1 of Ni-NiO. The electrochemical measurement showed that the as-produced Ni-NiO@C nanocomposites presented better catalytic activity for the electro-oxidation of methanol than Ni-NiO and NiO, which provides a new catalyst selection for the electro-oxidation of methanol.

Bulk Heterojunction Solar Cell with Nitrogen-Doped Carbon Nanotubes in the Active Layer: Effect of Nanocomposite Synthesis Technique on Photovoltaic Properties

PubMed Central

Keru, Godfrey; Ndungu, Patrick G.; Mola, Genene T.; Nyamori, Vincent O.

2015-01-01

Nanocomposites of poly(3-hexylthiophene) (P3HT) and nitrogen-doped carbon nanotubes (N-CNTs) have been synthesized by two methods; specifically, direct solution mixing and in situ polymerization. The nanocomposites were characterized by means of transmission electron microscopy (TEM), scanning electron microscopy (SEM), X-ray dispersive spectroscopy, UV-Vis spectrophotometry, photoluminescence spectrophotometry (PL), Fourier transform infrared spectroscopy (FTIR), Raman spectroscopy, thermogravimetric analysis, and dispersive surface energy analysis. The nanocomposites were used in the active layer of a bulk heterojunction organic solar cell with the composition ITO/PEDOT:PSS/P3HT:N-CNTS:PCBM/LiF/Al. TEM and SEM analysis showed that the polymer successfully wrapped the N-CNTs. FTIR results indicated good π-π interaction within the nanocomposite synthesized by in situ polymerization as opposed to samples made by direct solution mixing. Dispersive surface energies of the N-CNTs and nanocomposites supported the fact that polymer covered the N-CNTs well. J-V analysis show that good devices were formed from the two nanocomposites, however, the in situ polymerization nanocomposite showed better photovoltaic characteristics.

Sorption potential of alkaline treated straw and a soil for sulfonylurea herbicide removal from aqueous solutions: An environmental management strategy.

PubMed

Cara, Irina-Gabriela; Rusu, Bogdan-George; Raus, Lucian; Jitareanu, Gerard

2017-11-01

The adsorption potential of alkaline treated straw (wheat and corn) in mixture with soil, has been investigated for the removal of sulfonylurea molecules from an aqueous solutions. The surface characteristics were investigated by scanning electron microscopy and Fourier Transform Infrared - FTIR, while the adsorbent capacity was evaluated using batch sorption tests and liquid chromatography coupled with mass spectrometry. Surface analysis of alkaline treated straw samples by scanning electron microscopy - SEM showed the increasing of the surface roughness improving their functional surface activity. An increase (337.22 mg g -1 ) of adsorption capacity of sulfonylurea molecules was obtained for all studied straw. The Langmuir isotherm model was the best model for the mathematical description of the adsorption process indicating the forming of a surface sorption monolayer with a finite number of identical sites. The kinetics of sulfonylurea herbicide followed the pseudo-second order mechanism corresponding to strong chemical interactions. The results sustained that the alkaline treated straw have biosorption characteristics, being suitable adsorbent materials. Copyright © 2017 Elsevier Ltd. All rights reserved.

Flower-like and hollow sphere-like WO{sub 3} porous nanostructures: Selective synthesis and their photocatalysis property

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

Huang, Jiarui, E-mail: jrhuang@mail.anhu.edu.cn; Xu, Xiaojuan; Gu, Cuiping, E-mail: cpgu2008@mail.anhu.edu.cn

Graphical abstract: -- Abstract: Nanoflake-based flower-like and hollow microsphere-like hydrated tungsten oxide architectures were selectively synthesized by acidic precipitation of sodium tungstate solution at mild temperature. Several techniques, such as X-ray diffraction, scanning electron microscopy, thermogravimetric-differential thermalgravimetric analysis, transmission electron microscopy, and Brunauer–Emmett–Teller N{sub 2} adsorption–desorption analyses, were used to characterize the structure and morphology of the products. The experimental results show that the nanoflake-based flower-like and hollow sphere-like WO{sub 3}·H{sub 2}O architectures can be obtained by changing the concentration of sodium tungstate solution. The possible formation process based on the aggregation–recrystallization mechanism is proposed. The corresponding tungsten oxide three-dimensionalmore » architectures were obtained after calcination at 450 °C. Finally, the obtained WO{sub 3} three-dimensional architectures were used as photocatalyst in the experiments. Compared with WO{sub 3} microflowers, the as-prepared WO{sub 3} hollow microspheres exhibit superior photocatalytic property on photocatalytic decomposition of Rhodamine B due to their hollow porous hierarchical structures.« less

Preparation of alpha-alumina-supported mesoporous bentonite membranes for reverse osmosis desalination of aqueous solutions.

PubMed

Li, Liangxiong; Dong, Junhang; Lee, Robert

2004-05-15

In this study, mesoporous bentonite clay membranes approximately 2 microm thick were prepared on porous alpha-alumina substrates by a sol-gel method. Nanosized clay particles were obtained from commercial Na-bentonite powders (Wyoming) by a process of sedimentation, washing, and freeze-drying. X-ray diffraction, scanning electron microscopy, transmission electron microscopy, and nitrogen adsorption-desorption were employed for membrane characterization. It was found that the content of solids, concentration of polymer binder, and pH value of the clay colloidal suspension had critical influences on membrane formation during the dip-coating process. The membranes were tested for reverse osmosis separation of a 0.1 M NaCl solution. Both water permeability and Na(+) rejection rate of the supported membranes were comparable to those of the compacted thick membranes reported in the literature. However, due to the drastically reduced membrane thickness, water permeance and flux of the supported membranes were significantly higher than those of the compacted thick membranes. It was also observed that the calcination temperature played a critical role in determining structural stability in water and desalination performance of the clay membrane.

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.

Precipitation phases at different processes and heat treat ments as well as their effects on the mechanical properties of super-austenitic stainless steel

NASA Astrophysics Data System (ADS)

Sun, Hunying; Zhou, Zhangjian; Wang, Man; Li, Shaofu; Zhang, Liwei; Zou, Lei

2013-03-01

A new type lCr30Ni30Mo2TiZr super-austenitic stainless steel has been developed. The microstructures, precipitation phases and mechanical properties of the steel under different deformation processes and heat treatment (solution, stabilized treatment) were investigated using X-ray Diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) as well as mechanical tests. The results indicate that coarse carbides such as Cr-rich M23C6, sigma (σ), and little chi (χ) phases were formed in the steel, and large α' -Cr phases were also detected at three joint grain boundaries, and they were promoted by large strain. The precipitate phases were dissolved or transformed to intermetallic phase even at higher elevated temperature, and influenced the mechanical property obviously. These intermetallic compounds seriously reduced elongation of the rolled steel at room temperature and 700 °C, but increased the forged one at 700 °C. Impact absorbed energies of the stabilized specimens were lower than half of that solution status.

Hydrogels Synthesized by Electron Beam Irradiation for Heavy Metal Adsorption

PubMed Central

Manaila, Elena; Craciun, Gabriela; Ighigeanu, Daniel; Cimpeanu, Catalina; Barna, Catalina; Fugaru, Viorel

2017-01-01

Poly(acrylamide co-acrylic acid) hydrogels were prepared by free-radical copolymerization of acrylamide and acrylic acid in aqueous solutions using electron beam irradiation in the dose range of 2.5 kGy to 6 kGy in atmospheric conditions and at room temperature. The influence of the absorbed dose, the amount of cross-linker (trimethylolpropane trimethacrylate) and initiator (potassium persulfate) on the swelling properties and the diffusion coefficient and network parameters of hydrogels were investigated. The structure and morphology of hydrogels were characterized by Fourier Transform Infrared Spectroscopy (FTIR) and Scanning Electron Microscopy (SEM). The use of the obtained hydrogels by the removal of Cu2+ and Cr6+ from aqueous solutions was investigated at room temperature. During the adsorption of metal ions on hydrogels, the residual metal ion concentration in the solution was measured by an atomic absorption spectrophotometer (AAS). It has been established that the use of a relatively small amount of trimethylolpropane trimethacrylate for hydrogel preparation has led to the increasing of swelling up to 8500%. PMID:28772904

Hydrogels Synthesized by Electron Beam Irradiation for Heavy Metal Adsorption.

PubMed

Manaila, Elena; Craciun, Gabriela; Ighigeanu, Daniel; Cimpeanu, Catalina; Barna, Catalina; Fugaru, Viorel

2017-05-18

Poly(acrylamide co-acrylic acid) hydrogels were prepared by free-radical copolymerization of acrylamide and acrylic acid in aqueous solutions using electron beam irradiation in the dose range of 2.5 kGy to 6 kGy in atmospheric conditions and at room temperature. The influence of the absorbed dose, the amount of cross-linker (trimethylolpropane trimethacrylate) and initiator (potassium persulfate) on the swelling properties and the diffusion coefficient and network parameters of hydrogels were investigated. The structure and morphology of hydrogels were characterized by Fourier Transform Infrared Spectroscopy (FTIR) and Scanning Electron Microscopy (SEM). The use of the obtained hydrogels by the removal of Cu 2+ and Cr 6+ from aqueous solutions was investigated at room temperature. During the adsorption of metal ions on hydrogels, the residual metal ion concentration in the solution was measured by an atomic absorption spectrophotometer (AAS). It has been established that the use of a relatively small amount of trimethylolpropane trimethacrylate for hydrogel preparation has led to the increasing of swelling up to 8500%.

Nickel recovery from electronic waste II electrodeposition of Ni and Ni-Fe alloys from diluted sulfate solutions.

PubMed

Robotin, B; Ispas, A; Coman, V; Bund, A; Ilea, P

2013-11-01

This study focuses on the electrodeposition of Ni and Ni-Fe alloys from synthetic solutions similar to those obtained by the dissolution of electron gun (an electrical component of cathode ray tubes) waste. The influence of various parameters (pH, electrolyte composition, Ni(2+)/Fe(2+) ratio, current density) on the electrodeposition process was investigated. Scanning electron microscopy (SEM) and X-ray fluorescence analysis (XRFA) were used to provide information about the obtained deposits' thickness, morphology, and elemental composition. By controlling the experimental parameters, the composition of the Ni-Fe alloys can be tailored towards specific applications. Complementarily, the differences in the nucleation mechanisms for Ni, Fe and Ni-Fe deposition from sulfate solutions have been evaluated and discussed using cyclic voltammetry and potential step chronoamperometry. The obtained results suggest a progressive nucleation mechanism for Ni, while for Fe and Ni-Fe, the obtained data points are best fitted to an instantaneous nucleation model. Copyright © 2013 Elsevier Ltd. All rights reserved.

In situ growth of hollow gold-silver nanoshells within porous silica offers tunable plasmonic extinctions and enhanced colloidal stability.

PubMed

Li, Chien-Hung; Jamison, Andrew C; Rittikulsittichai, Supparesk; Lee, Tai-Chou; Lee, T Randall

2014-11-26

Porous silica-coated hollow gold-silver nanoshells were successfully synthesized utilizing a procedure where the porous silica shell was produced prior to the transformation of the metallic core, providing enhanced control over the structure/composition of the bimetallic hollow core. By varying the reaction time and the precise amount of gold salt solution added to a porous silica-coated silver-core template solution, composite nanoparticles were tailored to reveal a readily tunable surface plasmon resonance that could be centered across the visible and near-IR spectral regions (∼445-800 nm). Characterization by X-ray photoelectron spectroscopy, energy-dispersive X-ray spectroscopy, scanning electron microscopy, and transmission electron microscopy revealed that the synthetic methodology afforded particles having uniform composition, size, and shape. The optical properties were evaluated by absorption/extinction spectroscopy. The stability of colloidal solutions of our composite nanoparticles as a function of pH was also investigated, revealing that the nanoshells remain intact over a wide range of conditions (i.e., pH 2-10). The facile tunability, enhanced stability, and relatively small diameter of these composite particles (∼110 nm) makes them promising candidates for use in tumor ablation or as photothermal drug-delivery agents.

Chelant Enhanced Solution Processing for Wafer Scale Synthesis of Transition Metal Dichalcogenide Thin Films.

PubMed

Ionescu, Robert; Campbell, Brennan; Wu, Ryan; Aytan, Ece; Patalano, Andrew; Ruiz, Isaac; Howell, Stephen W; McDonald, Anthony E; Beechem, Thomas E; Mkhoyan, K Andre; Ozkan, Mihrimah; Ozkan, Cengiz S

2017-07-25

It is of paramount importance to improve the control over large area growth of high quality molybdenum disulfide (MoS 2 ) and other types of 2D dichalcogenides. Such atomically thin materials have great potential for use in electronics, and are thought to make possible the first real applications of spintronics. Here in, a facile and reproducible method of producing wafer scale atomically thin MoS 2 layers has been developed using the incorporation of a chelating agent in a common organic solvent, dimethyl sulfoxide (DMSO). Previously, solution processing of a MoS 2 precursor, ammonium tetrathiomolybdate ((NH 4 ) 2 MoS 4 ), and subsequent thermolysis was used to produce large area MoS 2 layers. Our work here shows that the use of ethylenediaminetetraacetic acid (EDTA) in DMSO exerts superior control over wafer coverage and film thickness, and the results demonstrate that the chelating action and dispersing effect of EDTA is critical in growing uniform films. Raman spectroscopy, photoluminescence (PL), x-ray photoelectron spectroscopy (XPS), Fourier transform infrared spectroscopy (FTIR), atomic force microscopy (AFM) and high-resolution scanning transmission electron microscopy (HR-STEM) indicate the formation of homogenous few layer MoS 2 films at the wafer scale, resulting from the novel chelant-in-solution method.

Isomorphism and solid solutions among Ag- and Au-selenides

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

Palyanova, Galina A.; Seryotkin, Yurii V.; Novosibirsk State University

Au-Ag selenides were synthesized by heating stoichiometric mixtures of elementary substances of initial compositions Ag{sub 2−x}Au{sub x}Se with a step of x=0.25 (0≤x≤2) to 1050 °C and annealing at 500 °C. Scanning electron microscopy, optical microscopy, electron microprobe analysis and X-ray powder diffraction methods have been applied to study synthesized samples. Results of studies of synthesized products revealed the existence of three solid solutions with limited isomorphism Ag↔Au: naumannite Ag{sub 2}Se – Ag{sub 1.94}Au{sub 0.06}Se, fischesserite Ag{sub 3}AuSe{sub 2} - Ag{sub 3.2}Au{sub 0.8}Se{sub 2} and gold selenide AuSe - Au{sub 0.94}Ag{sub 0.06}Se. Solid solutions and AgAuSe phases were added tomore » the phase diagram of Ag-Au-Se system. Crystal-chemical interpretation of Ag-Au isomorphism in selenides was made on the basis of structural features of fischesserite, naumannite, and AuSe. - Highlights: • Au-Ag selenides were synthesized. • Limited Ag-Au isomorphism in the selenides is affected by structural features. • Some new phases were introduced to the phase diagram Ag-Au-Se.« less

Influence of low concentration acid treatment on lithium disilicate core/veneer ceramic bond strength

PubMed Central

Garcia, Rudan P.; Conti, Paulo CR.; Pereira, Jefferson R.; Valle, Accácio Ld.

2013-01-01

Objective: This study evaluated the influence of low concentration acid treatment on the shear bond strength between lithium disilicate (LD) infrastructure and veneering porcelain. The surface morphology characteristic after this acid treatment was also examined. Study Design: LD reinforced ceramic cylinders (n=10) (IPS e.max Press, Ivoclar-Vivadent, Schaan, Liechtenstein) were treated (LD-treated) with a low concentration acid solution (Invex Liquid – Ivoclar-Vivadent, Schaan, Liechtenstein) or not treated with the acid solution (LD-untreated). They were veneered with a glass ceramic (IPS e.max Ceram, Ivoclar-Vivadent, Schaan, Liechtenstein). A metal ceramic group (CoCr) was tested as control. Shear bond strength (SBS) was conducted using a universal testing machine at 0.5 mm/min. Surface morphology characteristics after acid treatment were analyzed using scanning electron microscopy. Results: The acid treatment at low concentrations did not influence the SBS of the LD/veneering porcelain interface. The CoCr group showed the significant higher SBS value (35.59 ± 5.97 MPa), followed by LD-untreated group (27.76 ± 3.59 MPa) and LD-treated (27.02 ± 4.79 MPa). The fracture modes were predominantly adhesive for CoCr group and cohesive within the infrastructure for DL groups. Scanning Electron Microscopy (SEM) analysis showed no morphological differences between treated and untreated LD surfaces. Conclusions: Low concentration acid treatment did not improved SBS of veneering ceramic to LD and did not cause morphological changes on the LD surface. Key words:Lithium disilicate, glass ceramics, acid etching, shear bond strength, scanning electron microscopy. PMID:24455073

A pseudo-tetragonal tungsten bronze superstructure: a combined solution of the crystal structure of K6.4(Nb,Ta)(36.3)O94 with advanced transmission electron microscopy and neutron diffraction.

PubMed

Paria Sena, Robert; Babaryk, Artem A; Khainakov, Sergiy; Garcia-Granda, Santiago; Slobodyanik, Nikolay S; Van Tendeloo, Gustaaf; Abakumov, Artem M; Hadermann, Joke

2016-01-21

The crystal structure of the K6.4Nb28.2Ta8.1O94 pseudo-tetragonal tungsten bronze-type oxide was determined using a combination of X-ray powder diffraction, neutron diffraction and transmission electron microscopy techniques, including electron diffraction, high angle annular dark field scanning transmission electron microscopy (HAADF-STEM), annular bright field STEM (ABF-STEM) and energy-dispersive X-ray compositional mapping (STEM-EDX). The compound crystallizes in the space group Pbam with unit cell parameters a = 37.468(9) Å, b = 12.493(3) Å, c = 3.95333(15) Å. The structure consists of corner sharing (Nb,Ta)O6 octahedra forming trigonal, tetragonal and pentagonal tunnels. All tetragonal tunnels are occupied by K(+) ions, while 1/3 of the pentagonal tunnels are preferentially occupied by Nb(5+)/Ta(5+) and 2/3 are occupied by K(+) in a regular pattern. A fractional substitution of K(+) in the pentagonal tunnels by Nb(5+)/Ta(5+) is suggested by the analysis of the HAADF-STEM images. In contrast to similar structures, such as K2Nb8O21, also parts of the trigonal tunnels are fractionally occupied by K(+) cations.

Light, electron microscopic and immunohistochemical study of the effect of low-dose aspirin during the proestrus phase on rat endometrium in the preimplantation period.

PubMed

Ateş, Utku; Baka, Meral; Turgut, Mehmet; Uyanikgil, Yiğit; Ulker, Sibel; Yilmaz, Ozlem; Tavmergen, Erol; Yurtseven, Mine

2007-04-01

To evaluate structural alterations in rat endometrium at preimplantation following treatment with aspirin beginning from proestrus by light microscopy, electron microscopy and immunohistochemical techniques. Twenty rats were divided into control (n = 10) and experimental (n = 10) groups. Experimental rats were treated with low-dose aspirin daily (2 mg/kg/day) during estrus, beginning from the proestrus phase, mated at end of cycle and treated with aspirin. Untreated pregnant rats were the control group. Rats in both groups were sacrificed at the 84th pregnancy hour; the uterus was rapidly removed and dissected free of surrounding adipose tissue. Uteri specimens from nonpregnant rats were transferred into fixative solution and processed for light, electron microscopic and immunohistochemical study. Light and electron microscopy of endometrium from control rats conformed to mid-diestrus phase; endometrial histology of the aspirin-treated group conformed to late diestrus phase. The endometrial layer was significantly thicker in the aspirin-treated group compared to the untreated control group (p <0.001). No significant difference was found in vessel number between groups. Staining with alphaV integrin was more dense in the aspirin-treated group. Based on histologic findings, we suggest low-dose aspirin has positive effects on preparing endometrium before implantation.

Electrocrystallization and Properties of Supersaturated Solid Solutions of Copper

NASA Astrophysics Data System (ADS)

Povetkin, V. V.; Ivanova, T. E.; Ismagilova, A. V.

2018-03-01

The role of the alloying element in the formation of the structure and properties of electrolytic copper alloys has been determined. The X-ray diffraction analysis (XRD) and scanning electron microscopy (SEM) have shown that electrochemical alloying of copper with low-melting metals leads to the formation of supersaturated solid solutions (SSS) on the cathode, crushing of the crystal structure, smoothing of the surface relief, hardening of the deposits obtained, increasing their solderability and corrosive resistance to acidic media.

A general route for the rapid synthesis of one-dimensional nanostructured single-crystal Te, Se and Se Te alloys directly from Te or/and Se powders

NASA Astrophysics Data System (ADS)

Zhou, Bo; Zhu, Jun-Jie

2006-03-01

A general and template-free 'disproportionation and reversal' route was developed to synthesize one-dimensional (1D) nanostructures of Te, Se and Se-Te alloys directly from Te or/and Se powders. The products were characterized by x-ray diffraction (XRD), transmission electron microscopy (TEM), selected area electron diffraction (SAED), and scanning electron microscopy (SEM). Te nanorods and nanowires with a width varying from about 40 nm to about 300 nm, Se nanowires with a width of 60-100 nm and a length of 4-6 µm, and SexTe100-x alloy nanorods with x in a wide range, and with a width of 30-70 nm and an aspect ratio of three to five, were prepared. The mechanism of formation of the nanorods and nanowires and the effects of the experimental conditions, such as solution concentration, cooling rate, solvent nature and heating process, on the morphology and size of the products have been discussed. We believe that this general route and some other proper reversible processes between solid state and solution state can be extended to the transformations from various bulk materials into nanosized materials with various morphologies.

Graphene-Supported Spinel CuFe2O4 Composites: Novel Adsorbents for Arsenic Removal in Aqueous Media

PubMed Central

La, Duong Duc; Nguyen, Tuan Anh; Jones, Lathe A.; Bhosale, Sheshanath V.

2017-01-01

A graphene nanoplate-supported spinel CuFe2O4 composite (GNPs/CuFe2O4) was successfully synthesized by using a facile thermal decomposition route. Scanning electron microscopy (SEM), high resolution transmission electron microscopy (HRTEM), Electron Dispersive Spectroscopy (EDS), X-ray diffraction (XRD) and X-ray Photoelectron Spectroscopy (XPS) were employed to characterize the prepared composite. The arsenic adsorption behavior of the GNPs/CuFe2O4 composite was investigated by carrying out batch experiments. Both the Langmuir and Freundlich models were employed to describe the adsorption isotherm, where the sorption kinetics of arsenic adsorption by the composite were found to be pseudo-second order. The selectivity of the adsorbent toward arsenic over common metal ions in water was also demonstrated. Furthermore, the reusability and regeneration of the adsorbent were investigated by an assembled column filter test. The GNPs/CuFe2O4 composite exhibited significant, fast adsorption of arsenic over a wide range of solution pHs with exceptional durability, selectivity, and recyclability, which could make this composite a very promising candidate for effective removal of arsenic from aqueous solution. The highly sensitive adsorption of the material toward arsenic could be potentially employed for arsenic sensing. PMID:28587257

Evaluation of hemocompatibility and in vitro immersion on microwave-assisted hydroxyapatite-alumina nanocomposites.

PubMed

Radha, G; Balakumar, S; Venkatesan, Balaji; Vellaichamy, Elangovan

2015-05-01

This study reports the microwave-assisted synthesis and characterization of nHAp (nano-hydroxyapatite)-alumina composites. The crystalline phase and interaction of alumina with nHAp was analyzed using X-ray diffraction (XRD) and Raman microscopy analysis, respectively. High resolution transmission electron microscopy (HRTEM) micrographs exhibit morphological changes of nHAp composites with increasing alumina concentrations. Microhardness studies reveal the enhanced mechanical strength of nHAp10 and nHAp20 nanocomposites than pure nHAp. In vitro bioactivity of the nanocomposites was studied by immersing samples in simulated body fluid (Hank's solution) for 21 days. The surface of biomineralized samples were analyzed using field emission scanning electron microscopy (FESEM) and energy dispersive X-ray spectroscopy (EDX). Hemolytic assay revealed acceptable compatibility for varying concentrations of all the samples. Cell proliferation assay was systematically investigated for 1 day and 3 days on Saos-2 osteoblast-like cell lines and it was found that nHAp nanocomposites improved the proliferation. Copyright © 2015 Elsevier B.V. All rights reserved.

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

NASA Astrophysics Data System (ADS)

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

2018-05-01

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

PMMA/PS coaxial electrospinning: core-shell fiber morphology as a function of material parameters

NASA Astrophysics Data System (ADS)

Rahmani, Shahrzad; Arefazar, Ahmad; Latifi, Masoud

2017-03-01

Core-shell fibers of polymethyl methacrylate (PMMA) and polystyrene (PS) have been successfully electrospun by coaxial electrospinning. To evaluate the influence of the solvent on the final fiber morphology, four types of organic solvents were used in the shell solution while the core solvent was preserved. Morphological observations with scanning electron microscopy, transmission electron microscopy and optical microscopy revealed that both core and shell solvent properties were involved in the final fiber morphology. To explain this involvement, alongside a discussion of the Bagley solubility graph of PS and PMMA, a novel criterion based on solvent physical properties was introduced. A theoretical model based on the momentum conservation principle was developed and applied for describing the dependence of the core and shell diameters to their solvent combinations. Different concentrations of core and shell were also investigated in the coaxial electrospinning of PMMA/PS. The core-shell fiber morphologies with different core and shell concentrations were compared with their single electrospun fibers.

Mesoporous activated carbon from corn stalk core for lithium ion batteries

NASA Astrophysics Data System (ADS)

Li, Yi; Li, Chun; Qi, Hui; Yu, Kaifeng; Liang, Ce

2018-04-01

A novel mesoporous activated carbon (AC) derived from corn stalk core is prepared via a facile and effective method which including the decomposition and carbonization of corn stalk core under an inert gas atmosphere and further activation process with KOH solution. The mesoporous activated carbon (AC) is characterized by X-ray diffraction (XRD), Raman spectroscopy, scanning electron microscopy (SEM), transmission electron microscopy (TEM) and Brunauer-Emmett-Teller (BET) measurements. These biomass waste derived from activated carbon is proved to be promising anode materials for high specific capacity lithium ion batteries. The activated carbon anode possesses excellent reversible capacity of 504 mAh g-1 after 100 cycles at 0.2C. Compared with the unactivated carbon (UAC), the electrochemical performance of activated carbon is significantly improved due to its mesoporous structure.

An Open-Source Storage Solution for Cryo-Electron Microscopy Samples.

PubMed

Ultee, Eveline; Schenkel, Fred; Yang, Wen; Brenzinger, Susanne; Depelteau, Jamie S; Briegel, Ariane

2018-02-01

Cryo-electron microscopy (cryo-EM) enables the study of biological structures in situ in great detail and to solve protein structures at Ångstrom level resolution. Due to recent advances in instrumentation and data processing, the field of cryo-EM is a rapidly growing. Access to facilities and national centers that house the state-of-the-art microscopes is limited due to the ever-rising demand, resulting in long wait times between sample preparation and data acquisition. To improve sample storage, we have developed a cryo-storage system with an efficient, high storage capacity that enables sample storage in a highly organized manner. This system is simple to use, cost-effective and easily adaptable for any type of grid storage box and dewar and any size cryo-EM laboratory.

Synthesis and photocatalytic properties of TiO{sub 2} nanostructures

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

Xia, X.H.; Liang, Y.; Wang, Z.

2008-08-04

TiO{sub 2} particles, rods, flowers and sheets were prepared by hydrothermal method via adjusting the temperature, the pressure and the concentration of TiCl{sub 4}. The as-prepared TiO{sub 2} powders were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS), UV-vis diffuse reflectance spectra and N{sub 2} adsorption-desorption measurements. It was found that pressure is the most important factor influencing the morphology of TiO{sub 2}. The photocatalytic activity of the products was evaluated by the photodegradation of aqueous brilliant red X-3B solution under UV light. Among the as-prepared nanostructures, the flower-like TiO{sub 2}more » exhibited the highest photocatalytic activity.« less

Synthesis of silver nanoparticles using reducing agents obtained from natural sources (Rumex hymenosepalus extracts)

PubMed Central

2013-01-01

We have synthesized silver nanoparticles from silver nitrate solutions using extracts of Rumex hymenosepalus, a plant widely found in a large region in North America, as reducing agent. This plant is known to be rich in antioxidant molecules which we use as reducing agents. Silver nanoparticles grow in a single-step method, at room temperature, and with no addition of external energy. The nanoparticles have been characterized by ultraviolet-visible spectroscopy and transmission electron microscopy, as a function of the ratio of silver ions to reducing agent molecules. The nanoparticle diameters are in the range of 2 to 40 nm. High-resolution transmission electron microscopy and fast Fourier transform analysis show that two kinds of crystal structures are obtained: face-centered cubic and hexagonal. PMID:23841946

Corrosion resistance evaluation of Pd-free Ag-Au-Pt-Cu dental alloys.

PubMed

Fujita, Takeshi; Shiraishi, Takanobu; Takuma, Yasuko; Hisatsune, Kunihiro

2011-01-01

The corrosion resistance of nine experimental Pd-free Ag-Au-Pt-Cu dental alloys in a 0.9% NaCl solution was investigated using cyclic voltammetry (CV), optical microscopy, and scanning electron microscopy (SEM). CV measurements revealed that the breakdown potential (E(bd)) and zero current potential (E(zc)) increased with increasing Au/(Au+Ag) atomic ratio. Thus, the Au/(Au+Ag) atomic ratio, but not the Cu content, influenced the corrosion resistance of Ag-Au-Pt-Cu alloys. After the forward scan of CV, both optical and scanning electron microscope images showed that in all the experimental alloys, the matrix phase was corroded but not the second phase. From corrosion resistance viewpoint, the Ag-Au-Pt-Cu alloys seemed to be suitable for clinical application.

Extremely strong self-assembly of a bimetallic salen complex visualized at the single-molecule level.

PubMed

Salassa, Giovanni; Coenen, Michiel J J; Wezenberg, Sander J; Hendriksen, Bas L M; Speller, Sylvia; Elemans, Johannes A A W; Kleij, Arjan W

2012-04-25

A bis-Zn(salphen) structure shows extremely strong self-assembly both in solution as well as at the solid-liquid interface as evidenced by scanning tunneling microscopy, competitive UV-vis and fluorescence titrations, dynamic light scattering, and transmission electron microscopy. Density functional theory analysis on the Zn(2) complex rationalizes the very high stability of the self-assembled structures provoked by unusual oligomeric (Zn-O)(n) coordination motifs within the assembly. This coordination mode is strikingly different when compared with mononuclear Zn(salphen) analogues that form dimeric structures having a typical Zn(2)O(2) central unit. The high stability of the multinuclear structure therefore holds great promise for the development of stable self-assembled monolayers with potential for new opto-electronic materials.

Synthesis of TiO{sub 2} nanoparticles by hydrolysis and peptization of titanium isopropoxide solution

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

Mahata, S.; Mahato, S. S.; Nandi, M. M.

2012-07-23

Here we report the synthesis and characterization of a stable suspension of modified titania nanoparticles. Phase-pure TiO{sub 2} nanocrystallites with narrow particle-size distributions were selectively prepared by hydrolysis-peptization of modified alkoxide followed by hydrothermal treatment. Autoclaving modified TiO{sub 2} in the presence of HNO3 as cooperative catalysts led to the formation of crystalline TiO{sub 2} with narrow-sized distribution. Following the hydrothermal treatment at 150 Degree-Sign C, X-ray diffraction shows the particles to be exclusively anatase. Synthesized powder is characterized by FT-IR, scanning electron microscopy (FESEM) and transmission electron microscopy (HRTEM). The photocatalytic activity in the degradation of orange-II is quitemore » comparable to good anatase and rutile nanocrystallites.« less

Development of regenerated cellulose/halloysites nanocomposites via ionic liquids.

PubMed

Hanid, Nurbaiti Abdul; Wahit, Mat Uzir; Guo, Qipeng; Mahmoodian, Shaya; Soheilmoghaddam, Mohammad

2014-01-01

In this study, regenerated cellulose/halloysites (RC/HNT) nanocomposites with different nanofillers loading were fabricated by dissolving the cellulose in 1-ethyl-3-methylimidazolium chloride (EMIMCl) ionic liquid. The films were prepared via solution casting method and were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The mechanical properties were investigated by tensile testing. It clearly displayed a good enhancement of both tensile strength and Young's modulus with HNT loading up to 5 wt%. As the HNT loadings increased to 5 wt%, the thermal behaviour and water resistance rate was also increased. The TEM and SEM images also depicted even dispersion of the HNT and a good intertubular interaction between the HNT and the cellulose matrix. Copyright © 2013 Elsevier Ltd. All rights reserved.

Calibration-free quantitative surface topography reconstruction in scanning electron microscopy.

PubMed

Faber, E T; Martinez-Martinez, D; Mansilla, C; Ocelík, V; Hosson, J Th M De

2015-01-01

This work presents a new approach to obtain reliable surface topography reconstructions from 2D Scanning Electron Microscopy (SEM) images. In this method a set of images taken at different tilt angles are compared by means of digital image correlation (DIC). It is argued that the strength of the method lies in the fact that precise knowledge about the nature of the rotation (vector and/or magnitude) is not needed. Therefore, the great advantage is that complex calibrations of the measuring equipment are avoided. The paper presents the necessary equations involved in the methods, including derivations and solutions. The method is illustrated with examples of 3D reconstructions followed by a discussion on the relevant experimental parameters. Copyright © 2014 Elsevier B.V. All rights reserved.

Degradation of Methylammonium Lead Iodide Perovskite Structures through Light and Electron Beam Driven Ion Migration

PubMed Central

2016-01-01

Organometal halide perovskites show promising features for cost-effective application in photovoltaics. The material instability remains a major obstacle to broad application because of the poorly understood degradation pathways. Here, we apply simultaneous luminescence and electron microscopy on perovskites for the first time, allowing us to monitor in situ morphology evolution and optical properties upon perovskite degradation. Interestingly, morphology, photoluminescence (PL), and cathodoluminescence of perovskite samples evolve differently upon degradation driven by electron beam (e-beam) or by light. A transversal electric current generated by a scanning electron beam leads to dramatic changes in PL and tunes the energy band gaps continuously alongside film thinning. In contrast, light-induced degradation results in material decomposition to scattered particles and shows little PL spectral shifts. The differences in degradation can be ascribed to different electric currents that drive ion migration. Moreover, solution-processed perovskite cuboids show heterogeneity in stability which is likely related to crystallinity and morphology. Our results reveal the essential role of ion migration in perovskite degradation and provide potential avenues to rationally enhance the stability of perovskite materials by reducing ion migration while improving morphology and crystallinity. It is worth noting that even moderate e-beam currents (86 pA) and acceleration voltages (10 kV) readily induce significant perovskite degradation and alter their optical properties. Therefore, attention has to be paid while characterizing such materials using scanning electron microscopy or transmission electron microscopy techniques. PMID:26804213

Extra and Intracellular Synthesis of Nickel Oxide Nanoparticles Mediated by Dead Fungal Biomass

PubMed Central

Salvadori, Marcia Regina; Ando, Rômulo Augusto; Oller Nascimento, Cláudio Augusto; Corrêa, Benedito

2015-01-01

The use of dead biomass of the fungus Hypocrea lixii as a biological system is a new, effective and environmentally friendly bioprocess for the production and uptake of nickel oxide nanoparticles (NPs), which has become a promising field in nanobiotechnology. Dead biomass of the fungus was successfully used to convert nickel ions into nickel oxide NPs in aqueous solution. These NPs accumulated intracellularly and extracellularly on the cell wall surface through biosorption. The average size, morphology and location of the NPs were characterized by transmission electron microscopy, high-resolution transmission electron microscopy, scanning electron microscopy, and energy dispersive X-ray spectroscopy. The NPs were mainly spherical and extra and intracellular NPs had an average size of 3.8 nm and 1.25 nm, respectively. X-ray photoelectron spectroscopy analysis confirmed the formation of nickel oxide NPs. Infrared spectroscopy detected the presence of functional amide groups, which are probable involved in particle binding to the biomass. The production of the NPs by dead biomass was analyzed by determining physicochemical parameters and equilibrium concentrations. The present study opens new perspectives for the biosynthesis of nanomaterials, which could become a potential biosorbent for the removal of toxic metals from polluted sites. PMID:26043111

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

NASA Astrophysics Data System (ADS)

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

2017-11-01

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

Surface-induced polymerization of actin.

PubMed Central

Renault, A; Lenne, P F; Zakri, C; Aradian, A; Vénien-Bryan, C; Amblard, F

1999-01-01

Living cells contain a very large amount of membrane surface area, which potentially influences the direction, the kinetics, and the localization of biochemical reactions. This paper quantitatively evaluates the possibility that a lipid monolayer can adsorb actin from a nonpolymerizing solution, induce its polymerization, and form a 2D network of individual actin filaments, in conditions that forbid bulk polymerization. G- and F-actin solutions were studied beneath saturated Langmuir monolayers containing phosphatidylcholine (PC, neutral) and stearylamine (SA, a positively charged surfactant) at PC:SA = 3:1 molar ratio. Ellipsometry, tensiometry, shear elastic measurements, electron microscopy, and dark-field light microscopy were used to characterize the adsorption kinetics and the interfacial polymerization of actin. In all cases studied, actin follows a monoexponential reaction-limited adsorption with similar time constants (approximately 10(3) s). At a longer time scale the shear elasticity of the monomeric actin adsorbate increases only in the presence of lipids, to a 2D shear elastic modulus of mu approximately 30 mN/m, indicating the formation of a structure coupled to the monolayer. Electron microscopy shows the formation of a 2D network of actin filaments at the PC:SA surface, and several arguments strongly suggest that this network is indeed causing the observed elasticity. Adsorption of F-actin to PC:SA leads more quickly to a slightly more rigid interface with a modulus of mu approximately 50 mN/m. PMID:10049338

Microstructural Characteristics and Mechanical Properties of an Electron Beam-Welded Ti/Cu/Ni Joint

NASA Astrophysics Data System (ADS)

Zhang, Feng; Wang, Ting; Jiang, Siyuan; Zhang, Binggang; Feng, Jicai

2018-04-01

Electron beam welding experiments of TA15 titanium alloy to GH600 nickel superalloy with and without a copper sheet interlayer were carried out. Surface appearance, microstructure and phase constitution of the joint were examined by optical microscopy, scanning electron microscopy and x-ray diffraction analysis. Mechanical properties of Ti/Ni and Ti/Cu/Ni joint were evaluated based on tensile strength and microhardness tests. The results showed that cracking occurred in Ti/Ni electron beam weldment for the formation of brittle Ni-Ti intermetallics, while a crack-free electron beam-welded Ti/Ni joint can be obtained by using a copper sheet as filler metal. The addition of copper into the weld affected the welding metallurgical process of the electron beam-welded Ti/Ni joint significantly and was helpful for restraining the formation of Ti-Ni intermetallics in Ti/Ni joint. The microstructure of the weld was mainly characterized by a copper-based solid solution and Ti-Cu interfacial intermetallic compounds. Ti-Ni intermetallic compounds were almost entirely suppressed. The hardness of the weld zone was significantly lower than that of Ti/Ni joint, and the tensile strength of the joint can be up to 282 MPa.

Microstructural Characteristics and Mechanical Properties of an Electron Beam-Welded Ti/Cu/Ni Joint

NASA Astrophysics Data System (ADS)

Zhang, Feng; Wang, Ting; Jiang, Siyuan; Zhang, Binggang; Feng, Jicai

2018-05-01

Electron beam welding experiments of TA15 titanium alloy to GH600 nickel superalloy with and without a copper sheet interlayer were carried out. Surface appearance, microstructure and phase constitution of the joint were examined by optical microscopy, scanning electron microscopy and x-ray diffraction analysis. Mechanical properties of Ti/Ni and Ti/Cu/Ni joint were evaluated based on tensile strength and microhardness tests. The results showed that cracking occurred in Ti/Ni electron beam weldment for the formation of brittle Ni-Ti intermetallics, while a crack-free electron beam-welded Ti/Ni joint can be obtained by using a copper sheet as filler metal. The addition of copper into the weld affected the welding metallurgical process of the electron beam-welded Ti/Ni joint significantly and was helpful for restraining the formation of Ti-Ni intermetallics in Ti/Ni joint. The microstructure of the weld was mainly characterized by a copper-based solid solution and Ti-Cu interfacial intermetallic compounds. Ti-Ni intermetallic compounds were almost entirely suppressed. The hardness of the weld zone was significantly lower than that of Ti/Ni joint, and the tensile strength of the joint can be up to 282 MPa.

Effect of superoxidized water and sodium hypochlorite, associated or not with EDTA, on organic and inorganic components of bovine root dentin.

PubMed

Ghisi, Alexandre Corrêa; Kopper, Patrícia Maria Poli; Baldasso, Flávia E R; Stürmer, Caroline P; Rossi-Fedele, Giampiero; Steier, Liviu; de Figueiredo, José Antonio Poli; Morgental, Renata Dornelles; Vier-Pelisser, Fabiana Vieira

2015-06-01

This study aimed to evaluate the effects of Sterilox (Sx), a superoxidized water, 5% and 2% sodium hypochlorite (5NaOCl and 2NaOCl), and 17% EDTA (E) on the organic and inorganic components of bovine dentin. Eighty bovine incisors were randomly divided into 8 groups (n = 10): 5NaOCl, 5NaOCl + E, 2NaOCl, 2NaOCl + E, Sx, Sx + E, E alone, and distilled water (H2O). Root canal instrumentation was performed by using the corresponding irrigant. The apical 15 mm was longitudinally sectioned into 2 fragments, one for light microscopy analysis in slides stained with picrosirius red (organic component) and the other for scanning electron microscopy analysis (inorganic component). Scores data obtained in the light microscopy analysis were submitted to the Kruskal-Wallis test, followed by multiple comparisons test (P < .05). Scanning electron microscopy images were analyzed descriptively. The chemical solution 5NaOCl had a greater effect on the organic component of dentin in area and depth than 2NaOCl. The chemical solutions 5NaOCl + E, 5NaOCl and 2NaOCl + E caused the greatest change in the collagenous organic matrix near the root canal lumen. The chemical solution 2NaOCl showed similar behavior to Sx, associated or not with E, promoting more superficial disorganization of collagen in a smaller area. Demineralization was observed in all groups in which E was used. However, areas of erosion and open dentinal tubules were detected only when it was combined with NaOCl. Five percent NaOCl promoted the most extensive damage to the organic component of dentin, and when associated to EDTA, dentinal erosion could be seen. Considering these specific aspects, 2% NaOCl and Sx had milder effects on bovine root dentin. Copyright © 2015 American Association of Endodontists. Published by Elsevier Inc. All rights reserved.

Au-nanoparticle-embedded cross-linked gelatin films synthesized on aqueous solution in contact with dielectric barrier discharge

NASA Astrophysics Data System (ADS)

Shirafuji, Tatsuru; Nakamura, Yusuke; Azuma, Shiori; Sotoda, Naoya; Isshiki, Toshiyuki

2018-01-01

A wine-red free-standing thin film has been formed by irradiating dielectric barrier discharge plasma on an aqueous solution containing HAuCl4 and gelatin. The film has a fibrous structure with an inhomogeneous thickness profile and is composed of cross-linked gelatin, as confirmed by optical microscopy and infrared absorption spectroscopy. The film has embedded Au nanoparticles (GNPs), as confirmed by transmission electron microscopy. In the region with a relatively small film thickness, the number density of GNPs is relatively low, and the sizes of GNPs range from 5.3 to 34.3 nm. In the region with a relatively large film thickness, on the other hand, GNPs are highly accumulated, and the sizes of GNPs range from 10.0 to 26.7 nm. The aqueous solution remains transparent even after the film growth process, which indicates that the plasma-induced processes involving GNP formation and film growth are confined near the surface of the aqueous solution. A possible film growth mechanism is discussed on the basis of the experimental results of this study.

Peering at Brain Polysomes with Atomic Force Microscopy

PubMed Central

Lunelli, Lorenzo; Bernabò, Paola; Bolner, Alice; Vaghi, Valentina; Marchioretto, Marta; Viero, Gabriella

2016-01-01

The translational machinery, i.e., the polysome or polyribosome, is one of the biggest and most complex cytoplasmic machineries in cells. Polysomes, formed by ribosomes, mRNAs, several proteins and non-coding RNAs, represent integrated platforms where translational controls take place. However, while the ribosome has been widely studied, the organization of polysomes is still lacking comprehensive understanding. Thus much effort is required in order to elucidate polysome organization and any novel mechanism of translational control that may be embedded. Atomic force microscopy (AFM) is a type of scanning probe microscopy that allows the acquisition of 3D images at nanoscale resolution. Compared to electron microscopy (EM) techniques, one of the main advantages of AFM is that it can acquire thousands of images both in air and in solution, enabling the sample to be maintained under near physiological conditions without any need for staining and fixing procedures. Here, a detailed protocol for the accurate purification of polysomes from mouse brain and their deposition on mica substrates is described. This protocol enables polysome imaging in air and liquid with AFM and their reconstruction as three-dimensional objects. Complementary to cryo-electron microscopy (cryo-EM), the proposed method can be conveniently used for systematically analyzing polysomes and studying their organization. PMID:27023752

Organic nanofibers from squarylium dyes: local morphology, optical, and electrical properties

NASA Astrophysics Data System (ADS)

Balzer, Frank; Schiek, Manuela; Osadnik, Andreas; Lützen, Arne; Rubahn, Horst-Günter

2012-02-01

Environmentally stable, non-toxic squarylium dyes with strong absorption maxima in the red and near infrared spectral region are known for almost fifty years. Despite the fact that their optoelectronic properties distinguish them as promising materials for organics based photovoltaic cells, they have regained attention only very recently. For their application in heterojunction solar cells knowledge of their nanoscopic morphology as well as nanoscopic electrical properties is paramount. In this paper thin films from two different squarylium dyes, from squarylium (SQ) and from hydroxy-squarylium (SQOH) are investigated. The thin films are either solution casted or vacuum sublimed onto substrates such as muscovite mica, which are known to promote self-assembly into oriented, crystalline nanostructures such as nanofibers. Local characterization is performed via (polarized) optical microscopy, scanning electron microscopy (SEM), atomic force microscopy (AFM), and Kelvin probe force microscopy (KPFM).

From micelle supramolecular assemblies in selective solvents to isoporous membranes.

PubMed

Nunes, Suzana P; Karunakaran, Madhavan; Pradeep, Neelakanda; Behzad, Ali Reza; Hooghan, Bobby; Sougrat, Rachid; He, Haoze; Peinemann, Klaus-Viktor

2011-08-16

The supramolecular assembly of PS-b-P4VP copolymer micelles induced by selective solvent mixtures was used to manufacture isoporous membranes. Micelle order in solution was confirmed by cryo-scanning electron microscopy in casting solutions, leading to ordered pore morphology. When dioxane, a solvent that interacts poorly with the micelle corona, was added to the solution, polymer-polymer segment contact was preferential, increasing the intermicelle contact. Immersion in water gave rise to asymmetric porous membranes with exceptional pore uniformity and high porosity. The introduction of a small number of carbon nanotubes to the casting solution improved the membrane stability and the reversibility of the gate response in the presence of different pH values.

Solvothermal synthesis of nanocrystalline TiO 2 in toluene with surfactant

NASA Astrophysics Data System (ADS)

Kim, Chung-Sik; Moon, Byung Kee; Park, Jong-Ho; Choi, Byung-Chun; Seo, Hyo-Jin

2003-10-01

Synthesis of narrow-dispersed nanocrystalline TiO 2 was investigated by surfactant-aided solvothermal synthetic method in toluene solutions. Titanium isopropoxide (TIP) was used as precursor, which was decomposed at high temperature in the surfactant-dissolved solution. After the solution was thermally treated at 250°C for 20 h in an autoclave, low-dispersed TiO 2 nanocrystalline particles with average size of <6 nm were synthesized. When sufficient amount of TIP or surfactant was added in the solution, long dumbbell-shaped nanorods were formed, which may be due to the oriented growth of particles along [0 0 1] axis. Characterization of products was investigated by X-ray diffraction and transmission electron microscopy.

Stability of core-shell nanowires in selected model solutions

NASA Astrophysics Data System (ADS)

Kalska-Szostko, B.; Wykowska, U.; Basa, A.; Zambrzycka, E.

2015-03-01

This paper presents the studies of stability of magnetic core-shell nanowires prepared by electrochemical deposition from an acidic solution containing iron in the core and modified surface layer. The obtained nanowires were tested according to their durability in distilled water, 0.01 M citric acid, 0.9% NaCl, and commercial white wine (12% alcohol). The proposed solutions were chosen in such a way as to mimic food related environment due to a possible application of nanowires as additives to, for example, packages. After 1, 2 and 3 weeks wetting in the solutions, nanoparticles were tested by Infrared Spectroscopy, Atomic Absorption Spectroscopy, Transmission Electron Microscopy and X-ray diffraction methods.

SRB seawater corrosion project

NASA Technical Reports Server (NTRS)

Bozack, M. J.

1991-01-01

The corrosion behavior of 2219 aluminum when exposed to seawater was characterized. Controlled corrosion experiments at three different temperatures (30, 60 and 100 C) and two different environments (seawater and 3.5 percent salt solution) were designed to elucidate the initial stages in the corrosion process. It was found that 2219 aluminum is an active catalytic surface for growth of Al2O3, NaCl, and MgO. Formation of Al2O3 is favored at lower temperatures, while MgO is favored at higher temperatures. Visible corrosion products are formed within 30 minutes after seawater exposure. Corrosion characteristics in 3.5 percent salt solution are different than corrosion in seawater. Techniques utilized were: (1) scanning electron microscopy, (2) energy dispersive x-ray spectroscopy, and (3) Auger electron spectroscopy.

Hollow Polycaprolactone Microspheres with/without a Single Surface Hole by Co-Electrospraying

PubMed Central

2017-01-01

We describe the co-electrospraying of hollow microspheres from a polycaprolactone (PCL) shell solution and various core solutions including water, cyclohexane, poly(ethylene oxide) (PEO), and polyethylene glycol (PEG), using different collectors. The morphologies of the resultant microspheres were characterized by scanning electron microscopy (SEM), confocal microscopy, and nano-X-ray computed tomography (nano-XCT). The core/shell solution miscibility played an important role in the co-electrospraying process and the formation of microsphere structures. Spherical particles were more likely to be produced from miscible combinations of core/shell solutions than from immiscible ones. Hollow PCL microspheres with a single hole in their surfaces were produced when an ethanol bath was used as the collector. The mechanism by which the core/shell structure is transformed into single-hole hollow microspheres is proposed to be primarily based on the evaporation through the shell and extraction by ethanol of the core solution and is described in detail. Additionally, we present a 3D macroscopic tubular structure composed of hollow PCL microspheres, directly assembled on a copper wire collector during co-electrospraying. SEM and nano-XCT confirm that microspheres in the 3D bulk structure remain hollow. PMID:28901145

Electron-beam generated porous dextran gels: experimental and quantum chemical studies.

PubMed

Naumov, Sergej; Knolle, Wolfgang; Becher, Jana; Schnabelrauch, Matthias; Reichelt, Senta

2014-06-01

The aim of this work was to investigate the reaction mechanism of electron-beam generated macroporous dextran cryogels by quantum chemical calculation and electron paramagnetic resonance measurements. Electron-beam radiation was used to initiate the cross-linking reaction of methacrylated dextran in semifrozen aqueous solutions. The pore morphology of the resulting cryogels was visualized by scanning electron microscopy. Quantum chemical calculations and electron paramagnetic resonance studies provided information on the most probable reaction pathway and the chain growth radicals. The most probable reaction pathway was a ring opening reaction and the addition of a C-atom to the double-bond of the methacrylated dextran molecule. First detailed quantum chemical calculation on the reaction mechanism of electron-beam initiated cross-linking reaction of methacrylated dextran are presented.

Stimulated parametric emission microscopy.

PubMed

Isobe, Keisuke; Kataoka, Shogo; Murase, Rena; Watanabe, Wataru; Higashi, Tsunehito; Kawakami, Shigeki; Matsunaga, Sachihiro; Fukui, Kiichi; Itoh, Kazuyoshi

2006-01-23

We propose a novel microscopy technique based on the four-wave mixing (FWM) process that is enhanced by two-photon electronic resonance induced by a pump pulse along with stimulated emission induced by a dump pulse. A Ti:sapphire laser and an optical parametric oscillator are used as light sources for the pump and dump pulses, respectively. We demonstrate that our proposed FWM technique can be used to obtain a one-dimensional image of ethanol-thinned Coumarin 120 solution sandwiched between a hole-slide glass and a cover slip, and a two-dimensional image of a leaf of Camellia sinensis.

Doxorubicin-loaded Zein in situ gel for interstitial chemotherapy.

PubMed

Cao, Xiaoying; Geng, Jianning; Su, Suwen; Zhang, Linan; Xu, Qian; Zhang, Li; Xie, Yinghua; Wu, Shaomei; Sun, Yongjun; Gao, Zibin

2012-01-01

A novel drug delivery system of doxorubicin (DOX)-loaded Zein in situ gel for interstitial chemotherapy was investigated in this study. The possible mechanisms of drug release were described according to morphological analysis by optical microscopy and scanning electronic microscope (SEM). In vitro and in vivo anti-tumor activity studies showed that DOX-loaded Zein in situ gel was superior to DOX solution. Local pharmacokinetics in tumor tissue was studied by quantitative analysis with confocal laser scanning microscopy (CLSM) combined with microdialysis technology. A pharmacokinetics mathematical model of DOX-loaded Zein in situ gel in tumors was then built.

Covalent conjugation of graphene oxide with methotrexate and its antitumor activity

NASA Astrophysics Data System (ADS)

Wojtoniszak, M.; Urbas, K.; Perużyńska, M.; Kurzawski, M.; Droździk, M.; Mijowska, E.

2013-05-01

Here, we have functionalized graphene oxide with anticancer drug methotrexate through amide bonding. A kinetics of the drug release from graphene oxide in physiological solution - phosphate buffered saline (PBS) containing different biocompatible polymers have been investigated. Dispersion of MTX-GO in poly sodium-4-styrene sulfonate and poly ethylene glycol resulted in increase of the release time. The material was characterized with transmission electron microscopy, atomic force microscopy, Raman spectroscopy, Fourier transform infrared spectroscopy and UV-vis spectroscopy. Furthermore, antineoplastic action against human breast adenocarcinoma cell line MCF7 of MTX-GO and empty graphene oxide was explored.

Electron Tomography: A Three-Dimensional Analytic Tool for Hard and Soft Materials Research

DOE PAGES

Ercius, Peter; Alaidi, Osama; Rames, Matthew J.; ...

2015-06-18

Three-dimensional (3D) structural analysis is essential to understand the relationship between the structure and function of an object. Many analytical techniques, such as X-ray diffraction, neutron spectroscopy, and electron microscopy imaging, are used to provide structural information. Transmission electron microscopy (TEM), one of the most popular analytic tools, has been widely used for structural analysis in both physical and biological sciences for many decades, in which 3D objects are projected into two-dimensional (2D) images. In many cases, 2D-projection images are insufficient to understand the relationship between the 3D structure and the function of nanoscale objects. Electron tomography (ET) is amore » technique that retrieves 3D structural information from a tilt series of 2D projections, and is gradually becoming a mature technology with sub-nanometer resolution. Distinct methods to overcome sample-based limitations have been separately developed in both physical and biological science, although they share some basic concepts of ET. Here, this review discusses the common basis for 3D characterization, and specifies difficulties and solutions regarding both hard and soft materials research. It is hoped that novel solutions based on current state-of-the-art techniques for advanced applications in hybrid matter systems can be motivated. Electron tomography produces quantitative 3D reconstructions for biological and physical sciences from sets of 2D projections acquired at different tilting angles in a transmission electron microscope. Finally, state-of-the-art techniques capable of producing 3D representations such as Pt-Pd core-shell nanoparticles and IgG1 antibody molecules are reviewed.« less

Solvent-like ligand-coated ultrasmall cadmium selenide nanocrystals: strong electronic coupling in a self-organized assembly.

PubMed

Lawrence, Katie N; Johnson, Merrell A; Dolai, Sukanta; Kumbhar, Amar; Sardar, Rajesh

2015-07-21

Strong inter-nanocrystal electronic coupling is a prerequisite for delocalization of exciton wave functions and high conductivity. We report 170 meV electronic coupling energy of short chain poly(ethylene glycol) thiolate-coated ultrasmall (<2.5 nm in diameter) CdSe semiconductor nanocrystals (SNCs) in solution. Cryo-transmission electron microscopy analysis showed the formation of a pearl-necklace assembly of nanocrystals in solution with regular inter-nanocrystal spacing. The electronic coupling was studied as a function of CdSe nanocrystal size where the smallest nanocrystals exhibited the largest coupling energy. The electronic coupling in spin-cast thin-film (<200 nm in thickness) of poly(ethylene glycol) thiolate-coated CdSe SNCs was studied as a function of annealing temperature, where an unprecedentedly large, ∼400 meV coupling energy was observed for 1.6 nm diameter SNCs, which were coated with a thin layer of poly(ethylene glycol) thiolates. Small-angle X-ray scattering measurements showed that CdSe SNCs maintained an order array inside the films. The strong electronic coupling of SNCs in a self-organized film could facilitate the large-scale production of highly efficient electronic materials for advanced optoelectronic device application.

Physicochemical characterization and water vapor sorption of organic solution advanced spray-dried inhalable trehalose microparticles and nanoparticles for targeted dry powder pulmonary inhalation delivery.

PubMed

Li, Xiaojian; Mansour, Heidi M

2011-12-01

Novel advanced spray-dried inhalable trehalose microparticulate/nanoparticulate powders with low water content were successfully produced by organic solution advanced spray drying from dilute solution under various spray-drying conditions. Laser diffraction was used to determine the volumetric particle size and size distribution. Particle morphology and surface morphology was imaged and examined by scanning electron microscopy. Hot-stage microscopy was used to visualize the presence/absence of birefringency before and following particle engineering design pharmaceutical processing, as well as phase transition behavior upon heating. Water content in the solid state was quantified by Karl Fisher (KF) coulometric titration. Solid-state phase transitions and degree of molecular order were examined by differential scanning calorimetry (DSC) and powder X-ray diffraction, respectively. Scanning electron microscopy showed a correlation between particle morphology, surface morphology, and spray drying pump rate. All advanced spray-dried microparticulate/nanoparticulate trehalose powders were in the respirable size range and exhibited a unimodal distribution. All spray-dried powders had very low water content, as quantified by KF. The absence of crystallinity in spray-dried particles was reflected in the powder X-ray diffractograms and confirmed by thermal analysis. DSC thermal analysis indicated that the novel advanced spray-dried inhalable trehalose microparticles and nanoparticles exhibited a clear glass transition (T(g)). This is consistent with the formation of the amorphous glassy state. Spray-dried amorphous glassy trehalose inhalable microparticles and nanoparticles exhibited vapor-induced (lyotropic) phase transitions with varying levels of relative humidity as measured by gravimetric vapor sorption at 25°C and 37°C.

Microstructure and Phase Evolution in Mg-Gd and Mg-Gd-Nd Alloys With Additions of Zn, Y and Zr

NASA Astrophysics Data System (ADS)

Khawaled, S.; Bamberger, M.; Katsman, A.

Microstructure and phase evolution in Mg-Gd and Mg-Gd-Nd based alloys with additions of Zn, Zr and Y were analyzed in the as-cast, solution treated and aged conditions. Alloys has been investigated after solution treatment at 540°C for 24hr followed by isothermal aging at 175°C up to 32 days by using of Vickers hardness, optical microscopy, scanning electron microscopy equipped with EDS, X-ray diffraction and transmission electron microscopy. It was found that the as-cast alloys contained primary α-Mg matrix, eutecticlike structures, cuboid-like phases and Zr-rich clusters. The homogenized and quenched alloys contained primary α-Mg solid solution, smaller amount of divorced eutectic compounds, enlarged cuboid-like particles and Zr-rich clusters. The eutectic phase was Mg5Gd prototype with the composition Mg5(GdxNd1-x, x≈0.2). The compositions of the cuboid shaped particles are characterized by enlarged amount of Gd and can be written as Mg2(Gd x Y1-x) with x≈0.85 in the Mg-5Gd based alloy, and Gd4(YxNd1-x) with x≈0.5 in the Mg-6Gd-3.7Nd based alloy. The cuboid shaped particles grew during aging and reached 3µm average size. Precipitation of ß″ and ß' phases during aging was observed. Mg-6Gd-3.7Nd based alloy reached a maximum value of microhardness after 16 days of aging; in Mg-Gd based alloy, microhardness increased more slowly and reached a maximum value after 32 days of aging.

Population and size distribution of solute-rich mesospecies within mesostructured aqueous amino acid solutions.

PubMed

Jawor-Baczynska, Anna; Moore, Barry D; Lee, Han Seung; McCormick, Alon V; Sefcik, Jan

2013-01-01

Aqueous solutions of highly soluble substances such as small amino acids are usually assumed to be essentially homogenous systems with some degree of short range local structuring due to specific interactions on the sub-nanometre scale (e.g. molecular clusters, hydration shells), usually not exceeding several solute molecules. However, recent theoretical and experimental studies have indicated the presence of much larger supramolecular assemblies or mesospecies in solutions of small organic and inorganic molecules as well as proteins. We investigated both supersaturated and undersaturated aqueous solutions of two simple amino acids (glycine and DL-alanine) using Dynamic Light Scattering (DLS), Brownian Microscopy/Nanoparticles Tracking Analysis (NTA) and Cryogenic Transmission Electron Microscopy (Cryo-TEM). Colloidal scale mesospecies (nanodroplets) were previously reported in supersaturated solutions of these amino acids and were implicated as intermediate species on non-classical crystallization pathways. Surprisingly, we have found that the mesospecies are also present in significant numbers in undersaturated solutions even when the solute concentration is well below the solid-liquid equilibrium concentration (saturation limit). Thus, mesopecies can be observed with mean diameters ranging from 100 to 300 nm and a size distribution that broadens towards larger size with increasing solute concentration. We note that the mesospecies are not a separate phase and the system is better described as a thermodynamically stable mesostructured liquid containing solute-rich domains dispersed within bulk solute solution. At a given temperature, solute molecules in such a mesostructured liquid phase are subject to equilibrium distribution between solute-rich mesospecies and the surrounding bulk solution.

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.

Hydrothermal synthesis of NiCo2O4 nanowires/nitrogen-doped graphene for high-performance supercapacitor

NASA Astrophysics Data System (ADS)

Yu, Mei; Chen, Jianpeng; Ma, Yuxiao; Zhang, Jingdan; Liu, Jianhua; Li, Songmei; An, Junwei

2014-09-01

NiCo2O4 nanowires/nitrogen-doped graphene (NCO/NG) composite materials were synthesized by hydrothermal treatment in a water-glycerol mixed solvent and subsequent thermal transformation. The obtained materials were characterized by X-ray diffraction, scanning electron microscopy, transmission electron microscopy, Fourier transform infrared spectroscopy and Raman spectroscopy. The electrochemical performance of the composites was evaluated by cyclic voltammetry, galvanostatic charge/discharge and electrochemical impedance spectrum techniques. NiCo2O4 nanowires are densely coated by nitrogen-doped graphene and the composite displays good electrochemical performance. The maximum specific capacitance of NCO/NG is 1273.13 F g-1 at 0.5 A g-1 in 6 M KOH aqueous solution, and it exhibits good capacity retention without noticeable degradation after 3000 cycles at 4 A g-1.

A review of advantages of high-efficiency X-ray spectrum imaging for analysis of nanostructured ferritic alloys

DOE PAGES

Parish, Chad M.; Miller, Michael K.

2014-12-09

Nanostructured ferritic alloys (NFAs) exhibit complex microstructures consisting of 100-500 nm ferrite grains, grain boundary solute enrichment, and multiple populations of precipitates and nanoclusters (NCs). Understanding these materials' excellent creep and radiation-tolerance properties requires a combination of multiple atomic-scale experimental techniques. Recent advances in scanning transmission electron microscopy (STEM) hardware and data analysis methods have the potential to revolutionize nanometer to micrometer scale materials analysis. The application of these methods is applied to NFAs as a test case and is compared to both conventional STEM methods as well as complementary methods such as scanning electron microscopy and atom probe tomography.more » In this paper, we review past results and present new results illustrating the effectiveness of latest-generation STEM instrumentation and data analysis.« less

Green synthesis of silver nanoparticles using Alternanthera dentata leaf extract at room temperature and their antimicrobial activity

NASA Astrophysics Data System (ADS)

Kumar, Deenadayalan Ashok; Palanichamy, V.; Roopan, Selvaraj Mohana

2014-06-01

A green rapid biogenic synthesis of silver nanoparticles AgNPs using Alternanthera dentata (A. dentata) aqueous extract was demonstrated in this present study. The formation of silver nanoparticles was confirmed by Surface Plasmon Resonance (SPR) at 430 nm using UV-visible spectrophotometer. The reduction of silver ions to silver nanoparticles by A. dentata extract was completed within 10 min. Synthesized nanoparticles were characterized using UV-visible spectroscopy; Fourier transformed infrared spectroscopy (FT-IR), X-ray diffraction (XRD), scanning electron microscopy and transmission electron microscopy (TEM). The extracellular silver nanoparticles synthesis by aqueous leaf extract demonstrates rapid, simple and inexpensive method comparable to chemical and microbial methods. The colloidal solution of silver nanoparticles were found to exhibit antibacterial activity against Escherichia coli, Pseudomonas aeruginosa, Klebsiella pneumonia and, Enterococcus faecalis.

Sixty years from discovery to solution: crystal structure of bovine liver catalase form III

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

Foroughi, Leila M.; Kang, You-Na; Matzger, Adam J.

2012-03-27

The crystallization and structural characterization of bovine liver catalase (BLC) has been intensively studied for decades. Forms I and II of BLC have previously been fully characterized using single-crystal X-ray diffraction. Form III has previously been analyzed by electron microscopy, but owing to the thinness of this crystal form an X-ray crystal structure had not been determined. Here, the crystal structure of form III of BLC is presented in space group P212121, with unit-cell parameters a = 68.7, b = 173.7, c = 186.3 {angstrom}. The asymmetric unit is composed of the biological tetramer, which is packed in a tetrahedronmore » motif with three other BLC tetramers. This higher resolution structure has allowed an assessment of the previously published electron-microscopy studies.« less

Quantitative Description of Crystal Nucleation and Growth from in Situ Liquid Scanning Transmission Electron Microscopy.

PubMed

Ievlev, Anton V; Jesse, Stephen; Cochell, Thomas J; Unocic, Raymond R; Protopopescu, Vladimir A; Kalinin, Sergei V

2015-12-22

Recent advances in liquid cell (scanning) transmission electron microscopy (S)TEM has enabled in situ nanoscale investigations of controlled nanocrystal growth mechanisms. Here, we experimentally and quantitatively investigated the nucleation and growth mechanisms of Pt nanostructures from an aqueous solution of K2PtCl6. Averaged statistical, network, and local approaches have been used for the data analysis and the description of both collective particles dynamics and local growth features. In particular, interaction between neighboring particles has been revealed and attributed to reduction of the platinum concentration in the vicinity of the particle boundary. The local approach for solving the inverse problem showed that particles dynamics can be simulated by a stationary diffusional model. The obtained results are important for understanding nanocrystal formation and growth processes and for optimization of synthesis conditions.

Microfluidic reactor synthesis and photocatalytic behavior of Cu@Cu2O nanocomposite

NASA Astrophysics Data System (ADS)

Xu, Lei; Srinivasakannan, C.; Peng, Jinhui; Yan, Mi; Zhang, Di; Zhang, Libo

2015-03-01

The Cu@Cu2O nanocomposites were synthesized by solution-phase synthesis of Cu nanoparticles in microfluidic reactor at room temperature, followed by controlling the oxidation process. The size, morphology, elemental compositions, and the chemical composition on the surface of Cu@Cu2O nanocomposite were characterized by transmission electron microscopy (TEM), scanning electron microscopy (SEM), X-ray diffraction (XRD), and X-ray photoelectron spectroscopy (XPS). Experimental results demonstrated that the surface of the Cu nanoparticles was oxidized to Cu2O which serves as the shell of nanoparticle. The amount of Cu2O can be controlled by varying the drying temperature. Additionally the binary Cu@Cu2O nanocomposite along with H2O2 exhibited its potential as an excellent photocatalyst for degradation of methylene blue (MB) under UV irradiation.

Nanostructure CdS/ZnO heterojunction configuration for photocatalytic degradation of Methylene blue

NASA Astrophysics Data System (ADS)

Velanganni, S.; Pravinraj, S.; Immanuel, P.; Thiruneelakandan, R.

2018-04-01

In the present manuscript, thin films of Zinc Oxide (ZnO) have been deposited on a FTO substrate using a simple successive ionic layer adsorption and reaction (SILAR) and chemical bath deposition (CBD) method. Cadmium Sulphide (CdS) nanoparticles are sensitized over ZnO thin films using SILAR method. The synthesized nanostructured CdS/ZnO heterojunction thin films was characterized by X-ray diffraction (XRD), Scanning electron microscopy (SEM), High resolution transmission electron microscopy (HR-TEM), X-ray photoelectron spectroscopy (XPS), UV-Vis spectroscopy and Raman spectroscopy techniques. The band gap of CdS nanoparticles over ZnO nanostructure was found to be about 3.20 eV. The photocatalytic activities of the deposited CdS/ZnO thin films were evaluated by the degradation of methylene blue (MB) in an aqueous solution under sun light irradiation.

Sonochemical fabrication of fluorinated mesoporous titanium dioxide microspheres

NASA Astrophysics Data System (ADS)

Yu, Changlin; Yu, Jimmy C.; Chan, Mui

2009-05-01

A sonochemical-hydrothermal method for preparing fluorinated mesoporous TiO 2 microspheres was developed. Formation of mesoporous TiO 2 and doping of fluorine was achieved by sonication and then hydrothermal treatment of a solution containing titanium isopropoxide, template, and sodium fluoride. The as-synthesized TiO 2 microspheres were characterized by X-ray diffraction (XRD), Fourier translation infrared spectroscopy (FT-IR), X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM), transmission electron microscopy (TEM), energy-dispersive X-ray (EDX) spectroscopy, photoluminescence spectroscopy (PL), and BET surface areas. The P123 template was removed completely during the hydrothermal and washing steps, which was different from the conventional calcination treatment. The as- synthesized TiO 2 microspheres had good crystallinity and high stability. Results from the photocatalytic degradation of methylene blue (MB) showed that fluorination could remarkably improve the photocatalytic activity of titanium dioxide.

Size-dependent microstructures in rapidly solidified uranium-niobium powder particles

DOE PAGES

McKeown, Joseph T.; Hsiung, Luke L.; Park, Jong M.; ...

2016-06-14

The microstructures of rapidly solidified U-6wt%Nb powder particles synthesized by centrifugal atomization were characterized using scanning electron microscopy and transmission electron microscopy. Observed variations in microstructure are related to particle sizes. All of the powder particles exhibited a two-zone microstructure. The formation of this two-zone microstructure is described by a transition from solidification controlled by internal heat flow and high solidification rate during recalescence (micro-segregation-free or partitionless growth) to solidification controlled by external heat flow with slower solidification rates (dendritic growth with solute redistribution). The extent of partitionless solidification increased with decreasing particle size due to larger undercoolings in smallermore » particles prior to solidification. The metastable phases that formed are related to variations in Nb concentration across the particles. Lastly, the microstructures of the powders were heavily twinned.« less

Synthesis, characterization, and photocatalytic properties of Ni12P5 hollow microspheres

NASA Astrophysics Data System (ADS)

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

2017-05-01

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

A simple and low temperature process for super-hydrophilic rutile TiO 2 thin films growth

NASA Astrophysics Data System (ADS)

Mane, R. S.; Joo, Oh-Shim; Min, Sun-Ki; Lokhande, C. D.; Han, Sung-Hwan

2006-11-01

We investigate an environmentally friendly aqueous solution system for rutile TiO2 violet color nanocrystalline thin films growth on ITO substrate at room temperature. Film shows considerable absorption in visible region with excitonic maxima at 434 nm. X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), selected area electron diffraction (SAED), UV-vis, water surface contact angle and energy dispersive X-ray analysis (EDX) techniques in addition to actual photo-image that shows purely rutile phase of TiO2 with violet color, super-hydrophilic and densely packed nanometer-sized spherical grains of approximate diameter 3.15 ± 0.4 nm, characterize the films. Band gap energy of 4.61 eV for direct transition was obtained for the rutile TiO2 films. Film surface shows super-hydrophilic behavior, as exhibited water contact angle was 7°. Strong visible absorption (not due to chlorine) leaves future challenge to use these films in extremely thin absorber (ETA) solar cells.

Robust forests of vertically aligned carbon nanotubes chemically assembled on carbon substrates.

PubMed

Garrett, David J; Flavel, Benjamin S; Shapter, Joseph G; Baronian, Keith H R; Downard, Alison J

2010-02-02

Forests of vertically aligned carbon nanotubes (VACNTs) have been chemically assembled on carbon surfaces. The structures show excellent stability over a wide potential range and are resistant to degradation from sonication in acid, base, and organic solvent. Acid-treated single-walled carbon nanotubes (SWCNTs) were assembled on amine-terminated tether layers covalently attached to pyrolyzed photoresist films. Tether layers were electrografted to the carbon substrate by reduction of the p-aminobenzenediazonium cation and oxidation of ethylenediamine. The amine-modified surfaces were incubated with cut SWCNTs in the presence of N,N'-dicyclohexylcarbodiimide (DCC), giving forests of vertically aligned carbon nanotubes (VACNTs). The SWCNT assemblies were characterized by scanning electron microscopy, atomic force microscopy, and electrochemistry. Under conditions where the tether layers slow electron transfer between solution-based redox probes and the underlying electrode, the assembly of VACNTs on the tether layer dramatically increases the electron-transfer rate at the surface. The grafting procedure, and hence the preparation of VACNTs, is applicable to a wide range of materials including metals and semiconductors.

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

NASA Astrophysics Data System (ADS)

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

2016-08-01

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

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.

Efficient fluorescence quenching in electrochemically exfoliated graphene decorated with gold nanoparticles

NASA Astrophysics Data System (ADS)

Hurtado-Morales, M.; Ortiz, M.; Acuña, C.; Nerl, H. C.; Nicolosi, V.; Hernández, Y.

2016-07-01

High surface area graphene sheets were obtained by electrochemical exfoliation of graphite in an acid medium under constant potential conditions. Filtration and centrifugation processes played an important role in order to obtain stable dispersions in water. Scanning electron microscopy and transmission electron microscopy imaging revealed highly exfoliated crystalline samples of ∼5 μm. Raman, Fourier transform infrared and x-ray photoelectron spectroscopy further confirmed the high quality of the exfoliated material. The electrochemically exfoliated graphene (EEG) was decorated with gold nanoparticles (AuNPs) using sodium cholate as a buffer layer. This approach allowed for a non-covalent functionalization without altering the desirable electronic properties of the EEG. The AuNP-EEG samples were characterized with various techniques including absorbance and fluorescence spectroscopy. These samples displayed a fluorescence signal using an excitation wavelength of 290 nm. The calculated quantum yield (Φ) for these samples was 40.04%, a high efficiency compared to previous studies using solution processable graphene.

Synthesis of MoS2/rGO nanosheets hybrid materials for enhanced visible light assisted photocatalytic activity

NASA Astrophysics Data System (ADS)

Pal, Shreyasi; Dutta, Shibsankar; De, Sukanta

2018-04-01

A facile hydrothermal method has been adopted to synthesize pure MoS2 nanosheets and MoS2/rGO nanosheets hybrid. The samples were characterized using field emission scanning electron microscopy (FESEM), transmission electron microscopy (HRTEM), X-ray diffraction spectroscopy (XRD), Brunauer-Emmett-Teller (BET). The photocatalytic performance and reusability of MoS2 nanosheets and MoS2/rGO hybrids was evaluated by discoloring of RhB under visible light irradiation. Results indicated that MoS2/rGO photocatalysts with large surface area of 69.5 m2 g-1 could completely degrade 50 mL of 8 mg L-1 RhB aqueous solution in 90 min with excellent recycling and structural stability as compared with pure MoS2 nanosheets (53%). Such enhanced performance could be explained due to the high surface area, enhanced light absorption and the increased dye adsorptivity and reduced electron-hole pair recombination with the presence of rGO.

Reversible Cryopreservation of Living Cells Using an Electron Microscopy Cryo-Fixation Method.

PubMed

Huebinger, Jan; Han, Hong-Mei; Grabenbauer, Markus

2016-01-01

Rapid cooling of aqueous solutions is a useful approach for two important biological applications: (I) cryopreservation of cells and tissues for long-term storage, and (II) cryofixation for ultrastructural investigations by electron and cryo-electron microscopy. Usually, both approaches are very different in methodology. Here we show that a novel, fast and easy to use cryofixation technique called self-pressurized rapid freezing (SPRF) is-after some adaptations-also a useful and versatile technique for cryopreservation. Sealed metal tubes with high thermal diffusivity containing the samples are plunged into liquid cryogen. Internal pressure builds up reducing ice crystal formation and therefore supporting reversible cryopreservation through vitrification of cells. After rapid rewarming of pressurized samples, viability rates of > 90% can be reached, comparable to best-performing of the established rapid cooling devices tested. In addition, the small SPRF tubes allow for space-saving sample storage and the sealed containers prevent contamination from or into the cryogen during freezing, storage, or thawing.

Phase constitution characteristics of the Fe-Al alloy layer in the HAZ of calorized steel pipe

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

Li Yajiang; Zou Zengda; Wei Xing

1997-09-01

Mechanical properties of the welding region and phase constitution characteristics in the iron-aluminum (Fe-Al) alloy layer of calorized steel pipes were researched by means of metallography, which included the use of scanning electron microscopy (SEM), transmission electron microscopy (TEM), electron probe microanalysis (EPMA) and an X-ray diffractometer. Experimental results indicated that the Fe-Al alloy layer of calorized steel pipe was mainly composed of an FeAl phase, an Fe{sub 3}Al phase and an {alpha}-Fe(Al) solid solution, and the microhardness in the Fe-Al coating was 600--310 HM from the surface layer to the inside. There were no higher aluminum content phases, suchmore » as brittle FeAl{sub 2}, Fe{sub 2}Al{sub 5} and FeAl{sub 3}. By controlling the aluminizing process parameters, the ability to bear deformation and weld-ability of the calorized steel pipe were remarkably improved.« less

Synthesis of ZnO-CuO/MCM-48 photocatalyst for the degradation of organic pollutions.

PubMed

Duan, Yongzheng; Shen, Yulian

2017-07-01

The photocatalytic properties of ZnO-CuO catalysts supported on siliceous MCM-48 (Mobil Composition of Matter No. 48) for the degradation of organic pollutions such as methylene blue and salicylic acid under UV light irradiation were investigated. These catalysts were prepared by impregnation of MCM-48 with a mixed aqueous solution of copper acetate and zinc acetate. X-ray diffraction, N 2 -physisorption, high resolution transmission electron microscopy, scanning electron microscopy, Fourier transform infrared spectroscopy, X-ray photoelectron spectroscopy and photoluminescence were used to characterize these samples. Results from characterizations showed that the addition of ZnO to CuO/MCM-48 could markedly improve the photocatalytic degradation properties. The enhanced photocatalytic behaviors of ZnO-CuO/MCM-48 may be due to the formation of p-n heterojunctions between ZnO and CuO, resulting in the effective separation of photogenerated electron-hole pairs. Moreover, the photocatalysts were easily recovered and reused for five cycles without considerable loss of activity.

Intermolecular and interfacial forces: Elucidating molecular mechanisms using chemical force microscopy

NASA Astrophysics Data System (ADS)

Ashby, Paul David

Investigation into the origin of forces dates to the early Greeks. Yet, only in recent decades have techniques for elucidating the molecular origin of forces been developed. Specifically, Chemical Force Microscopy uses the high precision and nanometer scale probe of Atomic Force Microscopy to measure molecular and interfacial interactions. This thesis presents the development of many novel Chemical Force Microscopy techniques for measuring equilibrium and time-dependant force profiles of molecular interactions, which led to a greater understanding of the origin of interfacial forces in solution. In chapter 2, Magnetic Feedback Chemical Force Microscopy stiffens the cantilever for measuring force profiles between self-assembled monolayer (SAM) surfaces. Hydroxyl and carboxyl terminated SAMs produce long-range interactions that extend one or three nanometers into the solvent, respectively. In chapter 3, an ultra low noise AFM is produced through multiple modifications to the optical deflection detection system and signal processing electronics. In chapter 4, Brownian Force Profile Reconstruction is developed for accurate measurement of steep attractive interactions. Molecular ordering is observed for OMCTS, 1-nonanol, and water near flat surfaces. The molecular ordering of the solvent produces structural or solvation forces, providing insight into the orientation and possible solidification of the confined solvent. Seven molecular layers of OMCTS are observed but the oil remains fluid to the last layer. 1-nonanol strongly orders near the surface and becomes quasi-crystalline with four layers. Water is oriented by the surface and symmetry requires two layers of water (3.7 A) to be removed simultaneously. In chapter 5, electronic control of the cantilever Q (Q-control) is used to obtain the highest imaging sensitivity. In chapter 6, Energy Dissipation Chemical Force Microscopy is developed to investigate the time dependence and dissipative characteristics of SAM interfacial interactions in solution. Long-range adhesive forces for hydroxyl and carboxyl terminated SAM surfaces arise from solvent, not ionic, interactions. Exclusion of the solvent and contact between the SAM surfaces leads to rearrangement of the SAM headgroups. The isolation of the chemical and physical interfacial properties from the topography by Energy Dissipation Chemical Force Microscopy produces a new quantitative high-sensitivity imaging mode.

Field modeling and ray-tracing of a miniature scanning electron microscope beam column.

PubMed

Loyd, Jody S; Gregory, Don A; Gaskin, Jessica A

2017-08-01

A miniature scanning electron microscope (SEM) focusing column design is introduced and its potential performance assessed through an estimation of parameters that affect the probe radius, to include source size, spherical and chromatic aberration, diffraction and space charge broadening. The focusing column, a critical component of any SEM capable of operating on the lunar surface, was developed by the NASA Marshall Space Flight Center and Advanced Research Systems. The ray-trace analysis presented uses a model of the electrostatic field (within the focusing column) that is first calculated using the boundary element method (BEM). This method provides flexibility in modeling the complex electrode shapes of practical electron lens systems. A Fourier series solution of the lens field is then derived within a cylindrical domain whose boundary potential is provided by the BEM. Used in this way, the Fourier series solution is an accuracy enhancement to the BEM solution, allowing sufficient precision to assess geometric aberrations through direct ray-tracing. Two modes of operation with distinct lens field solutions are described. © The Author 2017. Published by Oxford University Press on behalf of The Japanese Society of Microscopy. All rights reserved. For permissions, please e-mail: journals.permissions@oup.com.

Solution-processed flexible NiO resistive random access memory device

NASA Astrophysics Data System (ADS)

Kim, Soo-Jung; Lee, Heon; Hong, Sung-Hoon

2018-04-01

Non-volatile memories (NVMs) using nanocrystals (NCs) as active materials can be applied to soft electronic devices requiring a low-temperature process because NCs do not require a heat treatment process for crystallization. In addition, memory devices can be implemented simply by using a patterning technique using a solution process. In this study, a flexible NiO ReRAM device was fabricated using a simple NC patterning method that controls the capillary force and dewetting of a NiO NC solution at low temperature. The switching behavior of a NiO NC based memory was clearly observed by conductive atomic force microscopy (c-AFM).

A Calcium Enterolith in a Patient with Crohn's Disease and Its In Vitro Dissolubility in Citric Acid

PubMed Central

Urata, Haruo; Ohmori, Masayasu; Kondo, Yoshitaka; Kawahara, Yoshiro; Okada, Hiroyuki

2017-01-01

The microstructure and dissolubility of a calcified enterolith and enterolith pieces removed from a 26-year-old Japanese woman with Crohn's disease were analyzed using scanning electron microscopy and energy dispersive X-ray spectroscopy. The enterolith showed a multilayered structure with fatty acid calcium and magnesium phosphate. The amount of calcium, magnesium, and phosphate decreased after they were immersed in a citric acid solution, suggesting a potential contribution of acidic aqueous solution to elute inorganic substances contained in calcified enteroliths. This is the first study to investigate the in vitro dissolubility of calcified enteroliths induced by citric acid solution. PMID:29082049

Synthesis and characterization of RuS2 nanostructures.

PubMed

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

2005-12-08

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

Preparation of fluorinated Cr2O3 hexagonal prism and catalytic performance for the dehydrofluorination of 1,1-difluoroethane to vinyl fluoride

NASA Astrophysics Data System (ADS)

Han, Wenfeng; Li, Xiaojuan; Tang, Haodong; Wang, Zhikun; Xi, Miao; Li, Ying; Liu, Huazhang

2015-09-01

A Cr2O3 hexagonal prism structure synthesized via the reaction of aqueous CrCl3 solution with NaBH4 solution at room temperature followed by calcination of the precipitate in N2 atmosphere at 500 °C is investigated as an efficient catalyst for dehydrofluorination of 1,1-difluoroethane producing vinyl fluoride. With the assistance of scanning electron microscopy, transmission electron microscopy, and high-resolution transmission electron microscopy, experimental results revealed that the uniform hexagonal prism has a prism length of 285 ± 43 nm and width of 233 ± 33 nm. It is in the form of loose and net-like aggregation of nano-Cr2O3 with diameter less than 3-5 nm with polycrystalline structure. NH3 temperature programmed desorption and chlorodifluoromethane dismutation experiments confirm the existence of relatively abundant and strong acidic sites. As a catalyst for dehydrofluorination of 1,1-difluoroethane, compared with commercial Cr2O3, much higher activity and stability were observed due to the evolution of CrO x F y species and much higher surface area and mesoporous structure. No significant morphology changes or sintering of the catalyst are observed after 70-h reaction. Compared with the commercial Cr2O3, we suggest that the much smaller size of Cr2O3 crystalline which possesses higher surface energy, lower strength, and more abundant Lewis acidity and the formation of CrO x F y during reaction over hexagonal prism catalyst probably contributes to the activity and stability difference between these two catalysts.

The use of acetone to enhance the infiltration of HA nanoparticles into a demineralized dentin collagen matrix.

PubMed

Besinis, Alexandros; van Noort, Richard; Martin, Nicolas

2016-03-01

This study investigates the role of acetone, as a carrier for nano-hydroxyapatite (nano-HA) in solution, to enhance the infiltration of fully demineralized dentin with HA nanoparticles (NPs). Dentin specimens were fully demineralized and subsequently infiltrated with two types of water-based nano-HA solutions (one containing acetone and one without). Characterization of the dentin surfaces and nano-HA particles was performed using scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The surface wettability and infiltration capacity of the nano-HA solutions were quantified by means of contact angle measurements and energy dispersive X-ray spectroscopy (EDS), respectively. Contact angle measurements were taken at baseline and repeated at regular intervals to assess the effect of acetone. The P and Ca levels of infiltrated dentin specimens were measured and compared to sound dentin and non-infiltrated controls. The presence of acetone resulted in an eight-fold decrease in the contact angles of the nano-HA solutions recorded on the surface of demineralized dentin compared to nano-HA solutions without acetone (one-way ANOVA, p<0.05). Perfect wetting of the demineralized dentin surface was achieved 5min after the application of the nano-HA solution containing acetone. Infiltration of demineralized dentin with the nano-HA solution containing acetone restored the lost mineral content by 50%, whereas the mean mineralization values for P and Ca in dentin treated with the acetone-free nano-HA solution were less than 6%. Acetone was shown to act as a vehicle to enhance the capacity to infiltrate demineralized dentin with HA NPs. The successful infiltration of dentin collagen with HA NPs provides a suitable scaffold, whereby the infiltrated HA NPs have the potential to act as seeds that may initiate heterogenous mineral growth when exposed to an appropriate mineral-rich environment. Copyright © 2015 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Synthesis, Structural Characterization, and Growth Mechanism of Li 1+x V 3 O 8 Submicron Fibers for Lithium-Ion Batteries

DOE PAGES

Yue, Shiyu; Li, Jing; Wang, Lei; ...

2018-03-05

Here, we report on the synthesis of submicron Li 1+xV 3O 8 fibers through a facile mixed ethanol/water solution-mediated solvothermal route in the absence of surfactants. All the raw materials used are commercially available, relatively inexpensive, and low-toxic, and these can be handled in an ambient atmosphere, rendering this synthetic route as reasonably facile and efficient. To ensure a desirable and acceptable sample crystallinity and purity, we introduced a postannealing treatment at 500°C. The monoclinic phase formation of the fiber sample was probed in detail using a series of X-ray diffraction, scanning electron microscopy, transmission electron microscopy, infrared spectroscopy, X-raymore » photoelectron spectroscopy, high resolution transmission electron microscopy, and selected area electron diffraction measurements. Both morphology and chemical composition could be carefully and systematically tuned in terms of generating a class of novel, pure, and well-defined motifs of Li 1+xV 3O 8. A plausible mechanism for the formation of submicron-diameter fibers has been discussed in addition to the expected phase transformation within our Li-V-O materials. Our comprehensive study should provide for needed fundamental insights into putting forth a viable synthesis strategy for the generation of well-defined morphological variants of layered oxide materials for battery applications.« less

Synthesis, Structural Characterization, and Growth Mechanism of Li 1+x V 3 O 8 Submicron Fibers for Lithium-Ion Batteries

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

Yue, Shiyu; Li, Jing; Wang, Lei

Here, we report on the synthesis of submicron Li 1+xV 3O 8 fibers through a facile mixed ethanol/water solution-mediated solvothermal route in the absence of surfactants. All the raw materials used are commercially available, relatively inexpensive, and low-toxic, and these can be handled in an ambient atmosphere, rendering this synthetic route as reasonably facile and efficient. To ensure a desirable and acceptable sample crystallinity and purity, we introduced a postannealing treatment at 500°C. The monoclinic phase formation of the fiber sample was probed in detail using a series of X-ray diffraction, scanning electron microscopy, transmission electron microscopy, infrared spectroscopy, X-raymore » photoelectron spectroscopy, high resolution transmission electron microscopy, and selected area electron diffraction measurements. Both morphology and chemical composition could be carefully and systematically tuned in terms of generating a class of novel, pure, and well-defined motifs of Li 1+xV 3O 8. A plausible mechanism for the formation of submicron-diameter fibers has been discussed in addition to the expected phase transformation within our Li-V-O materials. Our comprehensive study should provide for needed fundamental insights into putting forth a viable synthesis strategy for the generation of well-defined morphological variants of layered oxide materials for battery applications.« less

Effect of organic fuels on surface area and photocatalytic activity of scheelite CaWO4 nanoparticles

NASA Astrophysics Data System (ADS)

Manjunath, Kusuma; Gujjarahalli Thimmanna, Chandrappa

2018-03-01

Discrete nanoscale calcium tungstate (CaWO4) nanoparticles with exquisite photocatalytic activities were synthesized through ultra-rapid solution combustion route. Here, we aim to study the effect of different fuels on the synthesis of CaWO4 nanoparticles which lead to improve the characteristic properties and morphological evolution of the powders. From BET surface area measurement, it is observed that CaWO4 nanoparticles synthesized by using citric acid as fuel exhibits relatively large surface area (31.78 m2 g‑1) as compared to other fuels. The powder x-ray diffraction (PXRD) studies reveal that CaWO4 nanoparticles belong to scheelite type tetragonal system. The morphology of CaWO4 nanoparticles investigated using scanning electron microscopy (SEM) reveals that the powders are highly porous and agglomerated. Transmission electron microscopy (TEM) and high-resolution transmission electron microscopy (HRTEM) images of the CaWO4 nanoparticles show that a well-dispersed nearly oval-shaped nanoparticles with variable dimensions and lattice spacing that depends on the type of fuels used in the synthesis. The selected area electron diffraction (SAED) patterns of CaWO4 nanoparticles exhibit several concentric rings with bright spots indicating the polycrystalline nature of the powders. Investigation on photocatalytic activity of CaWO4 nanoparticles synthesized using citric acid shows highest (∼93%) degradation of methylene blue (MB).

Stabilized antiferroelectricity in xBiScO3-(1-x)NaNbO3 lead-free ceramics with established double hysteresis loops

NASA Astrophysics Data System (ADS)

Gao, Lisheng; Guo, Hanzheng; Zhang, Shujun; Randall, Clive A.

2018-02-01

We previously reported various solid solution systems that demonstrated the stabilized antiferroelectric (P) phases in NaNbO3 through lowering the tolerance factor. However, all those reported modifications were achieved by adding A2+B4+O3 type solid solutions. A lead-free antiferroelectric (AFE) solid solution xBiScO3-(1-x)NaNbO3 was rationalized by adopting the tolerance factor design rule. Specifically, adding BiScO3 was found to effectively stabilize the AFE phase without changing the crystal symmetry of NaNbO3. Microstructure and electron zone axis diffraction patterns from transmission electron microscopy revealed the stabilized AFE (P) phase in this solid solution. Besides, the electric-field-induced polarization with a double-hysteresis loop was observed. The present results pointed out that the strategy could also be applied while adding A3+B3+O3 type solid solutions. In addition, it expanded the compositional design that can be applied to antiferroelectric materials.

Fabrication of carbon nanowires by pyrolysis of aqueous solution of sugar within asbestos nanofibers

NASA Astrophysics Data System (ADS)

Butko, V. Yu.; Fokin, A. V.; Nevedomskii, V. N.; Kumzerov, Yu. A.

2015-05-01

Carbon nanowires have been fabricated by pyrolysis of an aqueous solution of sugar in nanochannels of asbestos fibers. Electron microscopy demonstrates that the diameter of these nanochannels corresponds to the diameter of the thinnest of the carbon nanowires obtained. Some of these nanowires have a graphite crystal lattice and internal pores. After asbestos is etched out, the carbon nanowires can retain the original shape of the asbestos fibers. Heating in an inert atmosphere reduces the electrical resistivity of the carbon nanowires to ˜0.035 Ω cm.

Corrosion and degradation of a polyurethane/Co-Ni-Cr-Mo pacemaker lead

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

Sung, P.; Fraker, A.C.

1987-12-01

An investigation to study changes in the metal surfaces and the polyurethane insulation of heart pacemaker leads under controlled in vitro conditions was conducted. A polyurethane (Pellethane 2363-80A)/Co-Ni-Cr-Mo (MP35N) wire lead was exposed in Hanks' physiological saline solution for 14 months and then analyzed using scanning electron microscopy, x-ray energy dispersive analysis, and small angle x-ray scattering. Results showed that some leakage of solution into the lead had occurred and changes were present on both the metal and the polyurethane surfaces.

Preparation of tungsten oxide

DOEpatents

Bulian, Christopher J [Yankton, SD; Dye, Robert C [Los Alamos, NM; Son, Steven F [Los Alamos, NM; Jorgensen, Betty S [Jemez Springs, NM; Perry, W Lee [Jemez Springs, NM

2009-09-22

Tungsten trioxide hydrate (WO.sub.3.H.sub.2O) was prepared from a precursor solution of ammonium paratungstate in concentrated aqueous hydrochloric acid. The precursor solution was rapidly added to water, resulting in the crash precipitation of a yellow white powder identified as WO.sub.3.H.sub.2O nanosized platelets by x-ray diffraction and scanning electron microscopy. Annealing of the powder at 200.degree. C. provided cubic phase WO.sub.3 nanopowder, and at 400.degree. C. provided WO.sub.3 nanopowder as a mixture of monoclinic and orthorhombic phases.

Nanoparticle Immobilization for Controllable Experiments in Liquid-Cell Transmission Electron Microscopy.

PubMed

Robertson, Alex W; Zhu, Guomin; Mehdi, B Layla; Jacobs, Robert M J; De Yoreo, James; Browning, Nigel D

2018-06-22

We demonstrate that silanization can control the adhesion of nanostructures to the SiN windows compatible with liquid-cell transmission electron microscopy (LC-TEM). Formation of an (3-aminopropyl)triethoxysilane (APTES) self-assembled monolayer on a SiN window, producing a surface decorated with amino groups, permits strong adhesion of Au nanoparticles to the window. Many of these nanoparticles remain static, undergoing minimal translation or rotation during LC-TEM up to high electron beam current densities due to the strong interaction between the APTES amino group and Au. We then use this technique to perform a direct comparative LC-TEM study on the behavior of ligand and nonligand-coated Au nanoparticles in a Au growth solution. While the ligand coated nanoparticles remain consistent even under high electron beam current densities, the naked nanoparticles acted as sites for secondary Au nucleation. These nucleated particles decorated the parent nanoparticle surface, forming consecutive monolayer assemblies of ∼2 nm diameter nanoparticles, which sinter into the parent particle when the electron beam was shut off. This method for facile immobilization of nanostructures for LC-TEM study will permit more sophisticated and controlled in situ experiments into the properties of solid-liquid interfaces in the future.

Interfacial Microstructure and Its Influence on Resistivity of Thin Layers Copper Cladding Steel Wires

NASA Astrophysics Data System (ADS)

Li, Hongjuan; Ding, Zhimin; Zhao, Ruirong

2018-04-01

The interfacial microstructure and resistivity of cold-drawn and annealed thin layers copper cladding steel (CCS) wires have been systematically investigated by the methods of scanning electron microscopy (SEM), transmission electron microscopy (TEM), energy dispersive spectroscopy (EDS), and resistivity testing. The results showed that the Cu and Fe atoms near interface diffused into each other matrixes. The Fe atoms diffused into Cu matrixes and formed a solid solution. The mechanism of solid solution is of substitution type. When the quantity of Fe atoms exceeds the maximum solubility, the supersaturated solid solution would form Fe clusters and decompose into base Cu and α-Fe precipitated phases under certain conditions. A few of α-Fe precipitates was observed in the copper near Cu/Fe interfaces of cold-drawn CCS wires, with 1-5 nm in size. A number of α-Fe precipitates of 1-20 nm in size can be detected in copper near Cu/Fe interfaces of CCS wires annealed at 850°C. When annealing temperature was less than 750°C, the resistivity of CCS wires annealed was lower than that of cold-drawn CCS wires. However, when annealing temperature was above 750°C, the resistivity of CCS wires was greater than that of cold-drawn CCS wires and increased with rising the annealing temperature. The relationship between nanoscale α-Fe precipitation and resistivity of CCS wires has been well discussed.

Self-assembly behavior of pH- and thermosensitive amphiphilic triblock copolymers in solution: experimental studies and self-consistent field theory simulations.

PubMed

Cai, Chunhua; Zhang, Liangshun; Lin, Jiaping; Wang, Liquan

2008-10-09

We investigated, both experimentally and theoretically, the self-assembly behaviors of pH- and thermosensitive poly(L-glutamic acid)- b-poly(propylene oxide)-b-poly(L-glutamic acid) (PLGA-b-PPO-b-PLGA) triblock copolymers in aqueous solution by means of transmission electron microscopy (TEM), scanning electron microscopy (SEM), dynamic light scattering (DLS), circular dichroism (CD), and self-consistent field theory (SCFT) simulations. Vesicles were observed when the hydrophilic PLGA block length is shorter or the pH value of solution is lower. The vesicles were found to transform to spherical micelles when the PLGA block length increases or its conformation changes from helix to coil with increasing the pH value. In addition, increasing temperature gives rise to a decrease in the size of aggregates, which is related to the dehydration of the PPO segments at higher temperatures. The SCFT simulation results show that the vesicles transform to the spherical micelles with increasing the fraction or statistical length of A block in model ABA triblock copolymer, which corresponds to the increase in the PLGA length or its conformation change from helix to coil in experiments, respectively. The SCFT calculations also provide chain distribution information in the aggregates. On the basis of both experimental and SCFT results, the mechanism of the structure change of the PLGA- b-PPO- b-PLGA aggregates was proposed.

Evaluation and quantification of reprocessing modification in single-use devices in interventional cardiology

NASA Astrophysics Data System (ADS)

Tessarolo, Francesco; Ferrari, Paolo; Silvia, Bortoluzzi; Motta, Antonella; Migliaresi, Claudio; Zennaro, Lucio; Rigo, Adelio; Guarrera, Giovanni Maria; Nollo, Giandomenico

2004-11-01

The increasing demand in interventional cardiology urges for reprocessing of single-use-labelled medical devices. To fulfil this aim, accurate and validated regeneration protocols are mandatory to guarantee sterility, functionality and safeness. The reprocessing protocol was realized by decontamination with chloro-donors, cleaning with enzymatic solutions and hydrogen peroxide gas plasma sterilization. Reprocessing effects on ablation and electrophysiology catheters were evaluated by assessing physical-chemical changes on surfaces and bulks, as a function of the reprocessing cycles number. Conventional optical microscopy and environmental scanning electron microscopy (ESEM) underlined the presence of micro-scratches on the polyurethane shaft surface. A clear correlation was found between surface damages and number of reprocessing cycles. Atomic force microscopy (AFM) confirmed the occurrence of physical-chemical etching of the polyurethane shaft caused by the hydrogen peroxide plasma sterilization, with increasing of nano-roughness at increasing number of the reprocessing cycles. UV-Vis spectra performed on the incubation solution of polymeric shaft sample, showed an absorbance increase at about 208 nm. This fact could be attributed to the water elution from the polymer of low molecular weight oligomers. The presence of hydrolysis products of the polymeric shaft after incubation demands both the characterization of the products released in the solution and the chemical characterization of the water exposed surface.

Dimensions and Global Twist of Single-Layer DNA Origami Measured by Small-Angle X-ray Scattering.

PubMed

Baker, Matthew A B; Tuckwell, Andrew J; Berengut, Jonathan F; Bath, Jonathan; Benn, Florence; Duff, Anthony P; Whitten, Andrew E; Dunn, Katherine E; Hynson, Robert M; Turberfield, Andrew J; Lee, Lawrence K

2018-06-04

The rational design of complementary DNA sequences can be used to create nanostructures that self-assemble with nanometer precision. DNA nanostructures have been imaged by atomic force microscopy and electron microscopy. Small-angle X-ray scattering (SAXS) provides complementary structural information on the ensemble-averaged state of DNA nanostructures in solution. Here we demonstrate that SAXS can distinguish between different single-layer DNA origami tiles that look identical when immobilized on a mica surface and imaged with atomic force microscopy. We use SAXS to quantify the magnitude of global twist of DNA origami tiles with different crossover periodicities: these measurements highlight the extreme structural sensitivity of single-layer origami to the location of strand crossovers. We also use SAXS to quantify the distance between pairs of gold nanoparticles tethered to specific locations on a DNA origami tile and use this method to measure the overall dimensions and geometry of the DNA nanostructure in solution. Finally, we use indirect Fourier methods, which have long been used for the interpretation of SAXS data from biomolecules, to measure the distance between DNA helix pairs in a DNA origami nanotube. Together, these results provide important methodological advances in the use of SAXS to analyze DNA nanostructures in solution and insights into the structures of single-layer DNA origami.

Formation of Fluorohydroxyapatite with Silver Diamine Fluoride

PubMed Central

Mei, M.L.; Nudelman, F.; Marzec, B.; Walker, J.M.; Lo, E.C.M.; Walls, A.W.; Chu, C.H.

2017-01-01

Silver diamine fluoride (SDF) is found to promote remineralization and harden the carious lesion. Hydroxyapatite crystallization is a crucial process in remineralization; however, the role of SDF in crystal formation is unknown. We designed an in vitro experiment with calcium phosphate with different SDF concentrations (0.38, 1.52, 2.66, 3.80 mg/mL) to investigate the effect of this additive on the nucleation and growth of apatite crystals. Two control groups were also prepared—calcium phosphate (CaCl2·2H2O + K2HPO4 in buffer solution) and SDF (Ag[NH3]2F in buffer solution). After incubation at 37 oC for 24 h, the shape and organization of the crystals were examined by bright-field transmission electron microscopy and electron diffraction. Unit cell parameters of the obtained crystals were determined with powder X-ray diffraction. The vibrational and rotational modes of phosphate groups were analyzed with Raman microscopy. The transmission electron microscopy and selected-area electron diffraction confirmed that all solids precipitated within the SDF groups were crystalline and that there was a positive correlation between the increased percentage of crystal size and the concentration of SDF. The powder X-ray diffraction patterns indicated that fluorohydroxyapatite and silver chloride were formed in all the SDF groups. Compared with calcium phosphate control, a contraction of the unit cell in the a-direction but not the c-direction in SDF groups was revealed, which suggested that small localized fluoride anions substituted the hydroxyl anions in hydroxyapatite crystals. This was further evidenced by the Raman spectra, which displayed up-field shift of the phosphate band in all the SDF groups and confirmed that the chemical environment of the phosphate functionalities indeed changed. The results suggested that SDF reacted with calcium and phosphate ions and produced fluorohydroxyapatite. This preferential precipitation of fluorohydroxyapatite with reduced solubility could be one of the main factors for arrest of caries lesions treated with SDF. PMID:28521107

Elucidation of wear mechanisms by ferrographic analysis

NASA Technical Reports Server (NTRS)

Jones, W. R., Jr.

1981-01-01

The use of ferrographic analysis in conjunction with light and scanning electron microscopy is described for the elucidation of wear mechanisms taking place in operating equipment. Example of adhesive wear, abrasive wear, corrosive wear, rolling element fatigue, lubricant breakdown, and other wear modes are illustrated. In addition, the use of magnetic solutions to precipitate nonmagnetic debris from aqueous and nonaqueous fluids is described.

Chemistry of Non-Equilibrium Film Deposition.

DTIC Science & Technology

1985-12-01

titanium isopropoxide mixed with water solutions of lanthanum and lead nitrate. The gels were dehydrated, then fired to 600C to remove all organics...OW- ’so IRO $Va. ame Thin films; titanium dioxide; -PuZT,- ion beam deposition; annealing,’ trnmiso electron microscopy. 4 - . - S \\AISST 0A ZT *Can...Deposition....... . ... *.... .. ... .. ..... .. . .... 2 C. Nonequilibrium Physical Deposition.................... 3 1. Titanium Oxide Films

Synthesis, Characterization and Reactivity of Nanostructured Zero-Valent Iron Particles for Degradation of Azo Dyes

NASA Astrophysics Data System (ADS)

Mikhailov, Ivan; Levina, Vera; Leybo, Denis; Masov, Vsevolod; Tagirov, Marat; Kuznetsov, Denis

Nanostructured zero-valent iron (NSZVI) particles were synthesized by the method of ferric ion reduction with sodium borohydride with subsequent drying and passivation at room temperature in technical grade nitrogen. The obtained sample was characterized by means of X-ray powder diffraction, scanning electron microscopy, transmission electron microscopy and dynamic light scattering studies. The prepared NSZVI particles represent 100-200nm aggregates, which consist of 20-30nm iron nanoparticles in zero-valent oxidation state covered by thin oxide shell. The reactivity of the NSZVI sample, as the removal efficiency of refractory azo dyes, was investigated in this study. Two azo dye compounds, namely, orange G and methyl orange, are commonly detected in waste water of textile production. Experimental variables such as NSZVI dosage, initial dye concentration and solution pH were investigated. The kinetic rates of degradation of both dyes by NSZVI increased with the decrease of solution pH from 10 to 3 and with the increase of NSZVI dosage, but decreased with the increase of initial dye concentration. The removal efficiencies achieved for both orange G and methyl orange were higher than 90% after 80min of treatment.

Superior lithium-ion insertion/extraction properties of a novel LiFePO4/C/graphene material used as a cathode in aqueous solution.

PubMed

Duan, Wenyuan; Zhao, Mingshu; Shen, Junfang; Zhao, Suixin; Song, Xiaoping

2017-09-28

Herein, olivine LiFePO 4 covered with graphene and carbon layers is prepared via a sol-gel method, followed by calcination, and the resultant composite is used as a cathode material in aqueous rechargeable lithium-ion batteries (ARLBs). The phase structure and morphology of the composite are characterized via X-ray diffraction (XRD), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM) and specific surface area analysis (BET). The ARLB system is fabricated using LiFePO 4 /C/graphene as the cathode and a zinc anode in 1 mol L -1 ZnSO 4 ·7H 2 O and saturated LiNO 3 aqueous solution without dissolved oxygen, which delivers a capacity of 153 mA h g -1 at 0.5C rate. Even at a 50C rate, it maintains a capacity of 95 mA h g -1 after 200 cycles. The excellent rate capabilities show that this cathode material exhibits good electrochemical performance and this novel ARLB has great potential in the fields of energy storage and high power sources.

Preparation of NiCoP Hollow Quasi-Polyhedra and Their Electrocatalytic Properties for Hydrogen Evolution in Alkaline Solution.

PubMed

Li, Yapeng; Liu, Jindou; Chen, Chen; Zhang, Xiaohua; Chen, Jinhua

2017-02-22

Double metal phosphide (NiCoP) with hollow quasi-polyhedron structure was prepared by acidic etching and precipitation of ZIF-67 polyhedra and further phosphorization treatment with NaH 2 PO 2 . The morphology and microstructure of NiCoP quasi-polyhedron and its precursors were investigated by scanning electron microscopy, transmission electron microscopy, X-ray diffraction, and a micropore and chemisorption analyzer. Electrocatalytic properties were examined by typical electrochemical methods, such as linear sweep voltammetry, cyclic voltammetry, chronoamperometry, and electrochemical impedance spectroscopy in 1.0 M KOH aqueous solution. Results reveal that, compared with CoP hollow polyhedra, NiCoP hollow quasi-polyhedra exhibit better electrochemical properties for hydrogen evolution with a low onset overpotential of 74 mV and a small Tafel slope of 42 mV dec -1 . When the current density is 10 mA cm -2 , the corresponding overpotential is merely 124 mV, and 93% of its electrocatalytic activity can be maintained for 12 h. This indicates that NiCoP with hollow quasi-polyhedron structure, bimetallic merit, and low cost may be a good candidate as electrocatalyst in the practical application of hydrogen evolution.

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.

Simultaneous AuIII Extraction and In Situ Formation of Polymeric Membrane-Supported Au Nanoparticles: A Sustainable Process with Application in Catalysis.

PubMed

Mora-Tamez, Lucía; Esquivel-Peña, Vicente; Ocampo, Ana L; Rodríguez de San Miguel, Eduardo; Grande, Daniel; de Gyves, Josefina

2017-04-10

A polymeric membrane-supported catalyst with immobilized gold nanoparticles (AuNPs) was prepared through the extraction and in situ reduction of Au III salts in a one-step strategy. Polymeric inclusion membranes (PIMs) and polymeric nanoporous membranes (PNMs) were tested as different membrane-support systems. Transport experiments indicated that PIMs composed of cellulose triacetate, 2-nitrophenyloctyl ether, and an aliphatic tertiary amine (Adogen 364 or Alamine 336) were the most efficient supports for Au III extraction. The simultaneous extraction and reduction processes were proven to be the result of a synergic phenomenon in which all the membrane components were involved. Scanning electron microscopy characterization of cross-sectional samples suggested a distribution of AuNPs throughout the membrane. Transmission electron microscopy characterization of the AuNPs indicated average particle sizes of 36.7 and 2.9 nm for the PIMs and PNMs, respectively. AuNPs supported on PIMs allowed for >95.4 % reduction of a 0.05 mmol L -1 4-nitrophenol aqueous solution with 10 mmol L -1 NaBH 4 solution within 25 min. © 2017 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

Characterization of corrosion products of AB{sub 5}-type hydrogen storage alloys for nickel-metal hydride batteries

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

Maurel, F.; Knosp, B.; Backhaus-Ricoult, M.

2000-01-01

To better understand the decrease in storage capacity of AB{sub 5}-type alloys in rechargeable Ni/MH batteries undergoing repeated charge/discharge cycles, the corrosion of a MnNi{sub 3.55}Co{sub 0.75}Mn{sub 0.4}Al{sub 0.3} alloy in aqueous KOH electrolyte was studied. The crystal structure, chemical composition, and distribution of corrosion products were characterized by X-ray diffraction, scanning electron microscopy, and transmission electron microscopy. Hollow and filed needles of a mixed rare earth hydroxide Mn(OH){sub 3} were found to cover a continuous nanocrystalline corrosion scale composed of metal (Ni, Co) solid solution, oxide (Ni,Co)O solid solution and rare earth hydroxide, and a Mn-depleted alloy subscale. Corrosionmore » kinetics were measured for three different temperatures. Growth kinetics of the continuous corrosion scale and of the Mm(OH){sub 3} needles obeyed linear and parabolic rate laws, respectively. Models for the corrosion mechanism were developed on the basis of diffusional transport of Mn and OH through the hydroxide needles and subsequent diffusion along grain boundaries through the nanocrystalline scale.« less

Ultrasonic degradation of aqueous phenolsulfonphthalein (PSP) in the presence of nano-Fe/H2O2.

PubMed

Ayanda, Olushola S; Nelana, Simphiwe M; Naidoo, Eliazer B

2018-10-01

In this study, nano iron (nano-Fe) was successfully synthesized by sodium borohydride reduction of ferric chloride solution to enhance the ultrasonic degradation of phenolsulfonphthalein (PSP). The nano-Fe was characterized by scanning electron microscopy - energy dispersive spectroscopy (SEM-EDX), transmission electron microscopy (TEM), powder X-ray diffraction (XRD), attenuated total reflection - Fourier transform infrared spectroscopy (ATR-FTIR), and Brunauer, Emmett and Teller (BET) surface area determination. Experimental results demonstrated that a combined ultrasonic/nano-Fe/H 2 O 2 system was more effective for PSP removal in combination than they were individually and there was a significant difference between the combined and single processes. The ultrasonic/nano-Fe/H 2 O 2 degradation follows the Langmuir-Hinshelwood (L-H) kinetic model. The addition of nano-Fe and H 2 O 2 to the ultrasonic reactor greatly accelerated the degradation of PSP (25 mg/L) from 12.5% up to 96.5%. These findings indicated that ultrasonic degradation in the presence of nano-Fe and H 2 O 2 is a promising and efficient technique for the elimination of emerging micropollutants from aqueous solution. Copyright © 2018 Elsevier B.V. All rights reserved.

New SnO2/MgAl-layered double hydroxide composites as photocatalysts for cationic dyes bleaching.

PubMed

Dvininov, E; Ignat, M; Barvinschi, P; Smithers, M A; Popovici, E

2010-05-15

A new type of nanocomposite containing SnO(2) has been obtained by wet impregnation of dehydrated Mg/Al-hydrotalcite-type compounds with ethanolic solutions of SnCl(4).2H(2)O. Tin chloride hydrolysis was achieved using NaOH or NH(4)OH aqueous solutions, at pH around 9, followed by the conversion into corresponding hydroxides through calcinations. The powder X-ray diffraction (PXRD) and UV-Vis diffuse reflectance (UV-DR) methods confirmed the structure of as-synthesized solids. The chemical composition and morphology of the synthesized materials were investigated by energy dispersive X-ray analysis (EDX), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The as-synthesized materials were used for photocatalytic studies showing a good activity for methylene blue decolourization, which varies with SnO(2) content and used as a hydrolysing agent. The proposed mechanism is based on the shifting of flat band potential of SnO(2) due to the interaction with Mg/Al-LDH, this being energetically favourable to the formation of hydroxyl radicals responsible for methylene blue degradation. Copyright (c) 2009 Elsevier B.V. All rights reserved.

Ultratrace Detection of Nitroaromatics: Picric Acid Responsive Aggregation/Disaggregation of Self-Assembled p-Terphenylbenzimidazolium-Based Molecular Baskets.

PubMed

Sandhu, Sana; Kumar, Rahul; Singh, Prabhpreet; Mahajan, Aman; Kaur, Manmeet; Kumar, Subodh

2015-05-20

1-(p-Terphenyl)-benzimidazolium (TRIPOD-TP) molecules undergo self-assembly to form rodlike structures in aqueous medium, as shown by field-emission scanning electron microscopy, transmission electron microscopy, and dynamic light scattering studies. Upon gradual addition of picric acid (PA), these aggregates undergo an aggregation/disaggregation process to complex morphological structures (10(-12)-10(-10) M PA) and spherical aggregates (10(-9)-10(-8) M PA). These spherical aggregates undergo further dissolution to well-dispersed spheres between 10(-7)-10(-6) M PA. During fluorescence studies, these aggregates demonstrate superamplified fluorescence quenching (>97%) in the presence of 10(-5) to 0.2 equiv of the probe concentration, an unprecedented process with PA. The lowest detection limits by solution of TRIPOD-TP are 5 × 10(-13) PA, 50 × 10(-12) M 2,4-dinitrophenol, 200 × 10(-12) M 2,4,6-trinitrotoluene, and 1 nM 1-chloro-2,4-dinitrobenzene. Paper strips dipped in the solution of TRIPOD-TP demonstrate quantitative fluorescence quenching between 10(-17) and 10(-6) M PA using front-surface steady state studies and can measure as low as 2.29 × 10(-20) g/cm(2) PA.

Cell Adhesion Molecule L1 in Folded (Horseshoe) and Extended Conformations

PubMed Central

Schürmann, Gregor; Haspel, Jeffrey; Grumet, Martin; Erickson, Harold P.

2001-01-01

We have investigated the structure of the cell adhesion molecule L1 by electron microscopy. We were particularly interested in the conformation of the four N-terminal immunoglobulin domains, because x-ray diffraction showed that these domains are bent into a horseshoe shape in the related molecules hemolin and axonin-1. Surprisingly, rotary-shadowed specimens showed the molecules to be elongated, with no indication of the horseshoe shape. However, sedimentation data suggested that these domains of L1 were folded into a compact shape in solution; therefore, this prompted us to look at the molecules by an alternative technique, negative stain. The negative stain images showed a compact shape consistent with the expected horseshoe conformation. We speculate that in rotary shadowing the contact with the mica caused a distortion of the protein, weakening the bonds forming the horseshoe and permitting the molecule to extend. We have thus confirmed that the L1 molecule is primarily in the horseshoe conformation in solution, and we have visualized for the first time its opening into an extended conformation. Our study resolves conflicting interpretations from previous electron microscopy studies of L1. PMID:11408583

Enhanced Carrier Collection from CdS Passivated Grains in Solution-Processed Cu2ZnSn(S,Se)4 Solar Cells.

PubMed

Werner, Melanie; Keller, Debora; Haass, Stefan G; Gretener, Christina; Bissig, Benjamin; Fuchs, Peter; La Mattina, Fabio; Erni, Rolf; Romanyuk, Yaroslav E; Tiwari, Ayodhya N

2015-06-10

Solution processing of Cu2ZnSn(S,Se)4 (CZTSSe)-kesterite solar cells is attractive because of easy manufacturing using readily available metal salts. The solution-processed CZTSSe absorbers, however, often suffer from poor morphology with a bilayer structure, exhibiting a dense top crust and a porous bottom layer, albeit yielding efficiencies of over 10%. To understand whether the cell performance is limited by this porous layer, a systematic compositional study using (scanning) transmission electron microscopy ((S)TEM) and energy-dispersive X-ray spectroscopy of the dimethyl sulfoxide processed CZTSSe absorbers is presented. TEM investigation revealed a thin layer of CdS that is formed around the small CZTSSe grains in the porous bottom layer during the chemical bath deposition step. This CdS passivation is found to be beneficial for the cell performance as it increases the carrier collection and facilitates the electron transport. Electron-beam-induced current measurements reveal an enhanced carrier collection for this buried region as compared to reference cells with evaporated CdS.

Preparation of poly(methyl methacrylate) microcapsules by in situ polymerization on the surface of calcium carbonate particles.

PubMed

Sato, Katsuhiko; Nakajima, Tatsuya; Anzai, Jun-ichi

2012-12-01

Poly(methyl methacrylate) (PMMA) microcapsules were prepared by the in situ polymerization of methyl methacrylate (MMA) and N,N'-methylenebisacrylamide on the surface of calcium carbonate (CaCO(3)) particles, followed by the dissolution of the CaCO(3) core in ethylenediaminetetraacetic acid solution. The microcapsules were characterized using fluorescence microscopy, atomic force microscopy, scanning electron microscopy, and Fourier transform infrared spectroscopy. The average sizes of the CaCO(3) particles and PMMA capsules were 3.8±0.6 and 4.0±0.6 μm, respectively. A copolymer consisting of MMA and rhodamine B-bearing MMA was also used to prepare microcapsules for fluorescent microscopy observations. Fluorescein isothiocyanate-labeled bovine serum albumin was enclosed in the PMMA microcapsules and its release properties were studied. Copyright © 2012 Elsevier Inc. All rights reserved.

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

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

Li Yao; He Xiaoyan; Cao Minhua

2008-11-03

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

Intensive care unit environmental surfaces are contaminated by multidrug-resistant bacteria in biofilms: combined results of conventional culture, pyrosequencing, scanning electron microscopy, and confocal laser microscopy.

PubMed

Hu, H; Johani, K; Gosbell, I B; Jacombs, A S W; Almatroudi, A; Whiteley, G S; Deva, A K; Jensen, S; Vickery, K

2015-09-01

Hospital-associated infections cause considerable morbidity and mortality, and are expensive to treat. Organisms causing these infections can be sourced from the inanimate environment around a patient. Could the difficulty in eradicating these organisms from the environment be because they reside in dry surface biofilms? The intensive care unit (ICU) of a tertiary referral hospital was decommissioned and the opportunity to destructively sample clinical surfaces was taken in order to investigate whether multidrug-resistant organisms (MDROs) had survived the decommissioning process and whether they were present in biofilms. The ICU had two 'terminal cleans' with 500 ppm free chlorine solution; items from bedding, surrounds, and furnishings were then sampled with cutting implements. Sections were sonicated in tryptone soya broth and inoculated on to chromogenic plates to demonstrate MDROs, which were confirmed with the Vitek2 system. Genomic DNA was extracted directly from ICU samples, and subjected to polymerase chain reaction (PCR) for femA to detect Staphylococcus aureus and the microbiome by bacterial tag-encoded FLX amplicon pyrosequencing. Confocal laser scanning microscopy (CLSM) and scanning electron microscopy (SEM) were performed on environmental samples. Multidrug-resistant bacteria were cultured from 52% (23/44) of samples cultured. S. aureus PCR was positive in 50%. Biofilm was demonstrated in 93% (41/44) of samples by CLSM and/or SEM. Pyrosequencing demonstrated that the biofilms were polymicrobial and contained species that had multidrug-resistant strains. Dry surface biofilms containing MDROs are found on ICU surfaces despite terminal cleaning with chlorine solution. How these arise and how they might be removed requires further study. Copyright © 2015 The Healthcare Infection Society. Published by Elsevier Ltd. All rights reserved.

Synthesis and Characterisation of Hollow Spherical Nano- and Microparticles with Silica and Magnetite

NASA Astrophysics Data System (ADS)

Gorbyk, P. P.; Dubrovin, I. V.; Demchenko, Yu. A.

The main principles and methods of synthesis of hollow structures with inorganic nanomaterials are described. Synthesis of hollow spherical silica particles was based on hydrolysis of Si(CH3)2Cl2 and SiCl4 in nonpolar solvents at a surface of aerosol drops. To synthesise hollow magnetite nano- and microparticles with magnetite, saturated solution of iron chlorides in acetone was used. Phase and element composition, morphology and structure of samples were studied using XRD, Auger electron spectroscopy, scanning electron and atom force microscopies.

Microstructural and microchemical studies of phase stability in V-O solid solution

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

Ghosh, Chanchal, E-mail: chanchal@igcar.gov.in

2017-02-15

Over the last couple of decades vanadium and V-based alloys have received significant attention as a potential structural material for fusion power applications because of their favourable mechanical properties under irradiation and at elevated temperatures. They are also considered as the advanced options of storage materials for hydrogen and its isotopes. However, the higher affinity of V for O, C and N poses critical challenges in its engineering applications since they lead to degradation of mechanical properties. They can further interact with the matrix to produce metallic oxy-carbo-nitride precipitates. To a certain limit, these precipitates are beneficial and can bemore » exploited to enhance the mechanical behaviour of the alloy through suitable microstructural design. However, this requires a prior knowledge of the interaction between the alloy and the impurity solutes. In the present work vanadium specific experiments have been designed and carried out to bring out the V-interstitial solute interaction by charging oxygen in the near surface region of vanadium. Microstructural and microchemical behaviour of the V-O solid solution has been studied through HRTEM (high resolution transmission electron microscopy) and HAADF (high angle annular dark field) coupled with EELS. Quantitative electron microscopy has been carried out to study structural modification of the alloy in atomic level caused by O charging. - Highlights: •Controlled experiments were carried out in pulsed laser ablation set-up to promote V-O interaction. • As a consequence of O dissolution, V transformed into a bct structure which is otherwise a bcc structure. •In V-O solid solution, dissolved O in the V matrix introduces significant amount of lattice strain. • Present work can be extended for introducing interstitial O in other pure transition metals and their alloys.« less

Arresting simulated dentine caries with adjunctive application of silver nitrate solution and sodium fluoride varnish: an in vitro study.

PubMed

Zhao, Irene Shuping; Mei, May Lei; Li, Quan-Li; Lo, Edward Chin Man; Chu, Chun-Hung

2017-08-01

The aim of this in vitro study was to assess the ability of silver nitrate solution, followed by sodium fluoride varnish, to arrest caries. Dentine slices were prepared and demineralised. Each slice was cut into three specimens for three groups (SF, SDF and W). Specimens of the SF group received topical application of 25% silver nitrate solution followed by 5% sodium fluoride varnish. The SDF group received topical application of 38% silver diamine fluoride solution (positive control). Specimens of the W group received deionised water (negative control). All specimens were subjected to pH cycling for 8 days. Dentine surface morphology, crystal characteristics, carious lesion depth and collagen matrix degradation were evaluated by scanning electron microscopy, X-ray diffraction, X-ray microtomography and spectrophotometry with a hydroxyproline assay. Scanning electron microscopy showed that dentine collagen was exposed in group W, but not in groups SF and SDF, while clusters of granular spherical grains were formed in groups SF and SDF. The mean lesion depths (±standard deviation) of groups SF, SDF and W were 128 ± 19, 135 ± 24 and 258 ± 53 μm, respectively (SF, SDF < W; P < 0.001). The X-ray diffraction analysis indicated that silver chloride was formed in groups SF and SDF. The concentration of hydroxyproline released from the dentine matrix was significantly lower in groups SF and SDF than in group W (P < 0.05). The results of this in vitro study indicate that the use of silver nitrate solution and sodium fluoride varnish is effective in inhibiting dentine demineralisation and dentine collagen degradation. © 2017 FDI World Dental Federation.

Effects of Etching Time and NaOH Concentration on the Production of Alumina Nanowires Using Porous Anodic Alumina Template

NASA Astrophysics Data System (ADS)

Sadeghpour-Motlagh, M.; Mokhtari-Zonouzi, K.; Aghajani, H.; Kakroudi, M. Ghassemi

2014-06-01

In this work, two-step anodizing of commercial aluminum foil in acid oxalic solution was applied for producing alumina film. Then the anodic alumina film was etched in sodium hydroxide (NaOH) solution resulting dense and aligned alumina nanowires. This procedure leads to splitting of alumina nanotubes. Subsequently nanowires are produced. The effects of NaOH solution concentration (0.2-1 mol/L) and etching time (60-300 s) at constant temperature on characteristic of nanotubes and produced nanowires were investigated using scanning electron microscopy. The results show that an increase in NaOH solution concentration increases the rate of nanowires production and in turn the manipulation process will be more specific.

Tunable hole injection of solution-processed polymeric carbon nitride towards efficient organic light-emitting diode

NASA Astrophysics Data System (ADS)

Zhang, Xiaowen; Zheng, Qinghong; Tang, Zhenyu; Li, Wanshu; Zhang, Yan; Xu, Kai; Xue, Xiaogang; Xu, Jiwen; Wang, Hua; Wei, Bin

2018-02-01

Polymeric carbon nitride (CNxHy) has been facilely synthesized from dicyandiamide and functions as a solution-processed hole injection layer in organic light-emitting diodes (OLEDs). The measurements using X-ray diffraction, atomic force microscopy, X-ray photoelectron spectroscopy, ultraviolet photoelectron spectroscopy, and impedance spectroscopy elucidate that CNxHy exhibits superior film morphology and extra electric properties such as tailored work function and tunable hole injection. The luminous efficiency of CNxHy-based OLED is found to improve by 76.6% in comparison to the counterpart using favorite solution-processed poly(ethylene dioxythiophene):poly(styrene sulfonate) as the hole injection layer. Our results also pave a way for broadening carbon nitride applications in organic electronics using the solution process.

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

Popa, C. L.; Ciobanu, C. S.; Predoi, D., E-mail: dpredoi@gmail.com

The aim of this study was to synthetize new nanoparticles based on methyltrimethoxysilane coated hydroxyapatite (MTHAp) for lead removal in aqueous solutions. The morphological and compositional analysis of MTHAp was investigated by scanning electron microscopy (SEM) equipped with an energy dispersive X-ray spectrometer (EDS). Removal experiments of Pb{sup 2+} ions were carried out in aqueous solutions with controlled concentration of Pb{sup 2+} and at fixed pH of 5. After the removal experiment of Pb{sup 2+} ions from solutions, porous hydroxyapatite nanoparticles were transformed into PbMTHAp-5 via the adsorption of Pb{sup 2+} ions followed by a cation exchange reaction. Our resultsmore » demonstrate that the porous hydroxyapatite nanoparticles can be used as an adsorbent for removing Pb{sup 2+} ions from aqueous solution.« less

Effect of Heat Treatment on Electrochemical Properties of Mg-9 wt.%Al-2.5 wt.%Pb Alloy in Sodium Chloride Solution

NASA Astrophysics Data System (ADS)

Wang, Linqian; Wang, Richu; Feng, Yan; Deng, Min; Wang, Naiguang

2017-12-01

Mg-Al-Pb alloy can serve as a good candidate for the anode material in seawater-activated batteries. The effect of solution and aging treatment on electrochemical properties of Mg-9 wt.%Al-2.5 wt.%Pb alloy in 3.5 wt.% NaCl solution was investigated through scanning electron microscopy and electrochemical tests. The results indicate that the discharge activity of Mg-9 wt.%Al-2.5 wt.%Pb alloy decreases after solution treatment, although its anodic efficiency increases slightly. In contrast, its discharge performance and anodic efficiency, which are crucial for the application of batteries, are both enhanced after aging at 200°C for 12 h.

Preparation and characterization of a novel highly hydrophilic and antifouling polysulfone/nanoporous TiO2 nanocomposite membrane.

PubMed

Bidsorkhi, H Cheraghi; Riazi, H; Emadzadeh, D; Ghanbari, M; Matsuura, T; Lau, W J; Ismail, A F

2016-10-14

In this research, novel ultrafiltration nanocomposite membranes were prepared by incorporating self-synthesized nanoporous titanium dioxide (NTiO2) nanoparticles into polysulfone. The surface of the nanoparticle was treated with a silane-based modifier to improve its distribution in the host polymer. Atomic-force microscopy, scanning electron microscopy, Fourier transform infrared spectroscopy, Brunauer-Emmett-Teller, transmission electron microscopy, energy-dispersive x-ray spectroscopy, porosity and contact angle tests were conducted to characterize the properties of the particles as well as the fabricated nanocomposite membranes. The effects of the nanoparticle incorporation were evaluated by conducting ultrafiltration experiments. It was reported that the membrane pure water flux was increased with increasing NTiO2 loading owing to the high porosity of the nanoparticles embedded and/or formation of enlarged pores upon addition of them. The antifouling capacity of the membranes was also tested by ultrafiltration of bovine serum albumin fouling solution. It was found that both water flux and antifouling capacity tended to reach desired level if the NTiO2 added was at optimized loading.

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

NASA Astrophysics Data System (ADS)

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

2018-04-01

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

DIRECT COUNTING AND SIZING OF MITOCHONDRIA IN SOLUTION

PubMed Central

Gear, Adrian R. L.; Bednarek, Jana M.

1972-01-01

Resistive particle counting has been developed for the accurate sizing and counting of mitochondria in solution. The normal detection limit with a 30 µ aperture is 0.48 µ diameter, or 0.056 µ3 particle volume The mean volume of rat liver mitochondria was 0.42 µ3 or 0.93 µ in diameter. The average value for numbers of particles per milligram of mitochondrial protein was 4.3 x 103, and per gram of rat liver was about 11 x 1010. These values compare satisfactorily with those derived by light microscopy and electron microscopy. The mean volume for mitochondria from rat heart was 0 60 µ3 and from rat kidney cortex, 0.23 µ3. These values agree within 15% of those determined by electron microscopy of whole tissue. Mitochondrial fragility and contaminating subcellular organelles were shown to have little influence on the experimentally determined size distributions The technique may be applied to rapid swelling studies, as well as to estimations of the number and size of mitochondria from animals under different conditions such as liver regeneration and hormonal, pathological, or drug-induced states Mitochondrial DNA, RNA, cytochrome c-oxidase, cytochrome (a ÷ a 3), and iron were nearly constant per particle over large differences in particle size. Such data may be particularly valuable for biogenesis studies and support the hypothesis that the net amount per particle of certain mitochondrial constituents remains constant during mitochondrial growth and enlargement PMID:4339279

Coacervation and aggregate transitions of a cationic ammonium gemini surfactant with sodium benzoate in aqueous solution.

PubMed

Wang, Ruijuan; Tian, Maozhang; Wang, Yilin

2014-03-21

Coacervation in an aqueous solution of cationic ammonium gemini surfactant hexamethylene-1,6-bis(dodecyldimethylammonium bromide) (C12C6C12Br2) with sodium benzoate (NaBz) has been investigated at 25 °C by turbidity titration, light microscopy, dynamic light scattering, cryogenic temperature transmission electron microscopy (Cryo-TEM), scanning electron microscopy (SEM), isothermal titration calorimetry, ζ potential and (1)H NMR measurements. There is a critical NaBz concentration of 0.10 M, only above which coacervation can take place. However, if the NaBz concentration is too large, coacervation also becomes difficult. Coacervation takes place at a very low concentration of C12C6C12Br2 and exists in a very wide concentration region of C12C6C12Br2. The phase behavior in the NaBz concentration from 0.15 to 0.50 M includes spherical micelles, threadlike micelles, coacervation, and precipitation. With increasing NaBz concentration, the phase boundaries of coacervation shift to higher C12C6C12Br2 concentration. Moreover, the C12C6C12Br2-NaBz aggregates in the coacervate are found to be close to charge neutralized. The Cryo-TEM and SEM images of the coacervate shows a layer-layer stacking structure consisting of a three-dimensional network formed by the assembly of threadlike micelles. Long, dense and almost uncharged threadlike micelles are the precursors of coacervation in the system.

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.

Ab initio structure determination of nanocrystals of organic pharmaceutical compounds by electron diffraction at room temperature using a Timepix quantum area direct electron detector.

PubMed

van Genderen, E; Clabbers, M T B; Das, P P; Stewart, A; Nederlof, I; Barentsen, K C; Portillo, Q; Pannu, N S; Nicolopoulos, S; Gruene, T; Abrahams, J P

2016-03-01

Until recently, structure determination by transmission electron microscopy of beam-sensitive three-dimensional nanocrystals required electron diffraction tomography data collection at liquid-nitrogen temperature, in order to reduce radiation damage. Here it is shown that the novel Timepix detector combines a high dynamic range with a very high signal-to-noise ratio and single-electron sensitivity, enabling ab initio phasing of beam-sensitive organic compounds. Low-dose electron diffraction data (∼ 0.013 e(-) Å(-2) s(-1)) were collected at room temperature with the rotation method. It was ascertained that the data were of sufficient quality for structure solution using direct methods using software developed for X-ray crystallography (XDS, SHELX) and for electron crystallography (ADT3D/PETS, SIR2014).

Development and characterization of Mn2+-doped MgO nanoparticles by solution combustion synthesis

NASA Astrophysics Data System (ADS)

Basha, Md. Hussain; Gopal, N. O.; Rao, J. L.; Nagabhushana, H.; Nagabhushana, B. M.; Chakradhar, R. P. S.

2015-06-01

Mn doped MgO Nanoparticles have been prepared by Solution Combustion Synthesis. The synthesized sample is characterized by X-ray diffraction (XRD), Scanning Electron Microscopy (SEM) and Electron Paramagnetic Resonance (EPR). The prepared MgO:Mn (1 mol%) nano crystals appear to be of simple cubic crystalline phase with lattice parameters a = 4.218(2) Å and cell volume = 74.98 (7) Å3. SEM micrograph of powders show highly porous, many agglomerates with irregular morphology, large voids, cracks and pores. EPR spectrum of the sample at room temperature exhibit an isotropic sextet hyperfine pattern, centered at g=1.99, characteristic if Mn2+ ions with S=I=5/2.The observed g value and the hyperfine value reveal the ionic bonding between Mn2+ and its surroundings.

Morphological and phase evolution of TiO 2 nanocrystals prepared from peroxotitanate complex aqueous solution: Influence of acetic acid

NASA Astrophysics Data System (ADS)

Chang, Jeong Ah; Vithal, Muga; Baek, In Chan; Seok, Sang Il

2009-04-01

Nanosized anatase and rutile TiO 2 having different shape, phase and size have been prepared from aqueous solutions of peroxo titanium complex starting from titanium(IV) isopropoxide (TTIP), acetic acid and hydrogen peroxide (H 2O 2) in water/isopropanol media by a facile sol-gel process. The TiO 2 nanocrystals are characterized by powder X-ray diffraction (XRD), Raman spectroscopy, FT-IR spectroscopy, TEM, high resolution transmission electron microscopy (HRTEM) and selected area electron diffraction (SAED) techniques. The influence of pH and the sequence of addition of reaction contents on the phase and morphology of TiO 2 are studied. The reasons for the observation of only anatase and/or mixture of anatase and rutile are given.

Engineering Non-Wetting Antimicrobial Fabrics

NASA Astrophysics Data System (ADS)

van den Berg, Desmond

This research presents novel techniques and a review of commercially available fabrics for their antimicrobial potential. Based on previous research into the advantages of superhydrophobic self-cleaning surfaces against bacterial contamination, insights into what can make a superhydrophobic fabric inherently antimicrobial were analyzed. Through comparing the characterization results of scanning electron microscopy (SEM) and optical profilometry to microbiology experiments, hypotheses into the relationship between the contact area of a bacterial solution and the extent of contamination is developed. Contact scenario experiments, involving the use of fluorescence microscopy and calculating colony forming units, proved that the contamination potential of any fabric is due to the wetting state exhibited by the fabric, as well as the extent of surface texturing. Transmission experiments, utilizing a novel technique of stamping a contaminated fabric, outlined the importance of retention of solutions or bacteria during interactions within the hospital environment on the extent of contamination.

Removal of xenotropic murine leukemia virus by nanocellulose based filter paper.

PubMed

Asper, M; Hanrieder, T; Quellmalz, A; Mihranyan, A

2015-11-01

The removal of xenotrpic murine leukemia virus (xMuLV) by size-exclusion filter paper composed of 100% naturally derived cellulose was validated. The filter paper was produced using cellulose nanofibers derived from Cladophora sp. algae. The filter paper was characterized using atomic force microscopy, scanning electron microscopy, helium pycnometry, and model tracer (100 nm latex beads and 50 nm gold nanoparticles) retention tests. Following the filtration of xMuLV spiked solutions, LRV ≥5.25 log10 TCID50 was observed, as limited by the virus titre in the feed solution and sensitivity of the tissue infectivity test. The results of the validation study suggest that the nanocellulose filter paper is useful for removal of endogenous rodent retroviruses and retrovirus-like particles during the production of recombinant proteins. Copyright © 2015 The International Alliance for Biological Standardization. Published by Elsevier Ltd. All rights reserved.

New developments in electron microscopy for serial image acquisition of neuronal profiles.

PubMed

Kubota, Yoshiyuki

2015-02-01

Recent developments in electron microscopy largely automate the continuous acquisition of serial electron micrographs (EMGs), previously achieved by laborious manual serial ultrathin sectioning using an ultramicrotome and ultrastructural image capture process with transmission electron microscopy. The new systems cut thin sections and capture serial EMGs automatically, allowing for acquisition of large data sets in a reasonably short time. The new methods are focused ion beam/scanning electron microscopy, ultramicrotome/serial block-face scanning electron microscopy, automated tape-collection ultramicrotome/scanning electron microscopy and transmission electron microscope camera array. In this review, their positive and negative aspects are discussed. © The Author 2015. Published by Oxford University Press on behalf of The Japanese Society of Microscopy. All rights reserved. For permissions, please e-mail: journals.permissions@oup.com.

Patterned self-assembled monolayers of alkanethiols on copper nanomembranes by submerged laser ablation

NASA Astrophysics Data System (ADS)

Rhinow, Daniel; Hampp, Norbert A.

2012-06-01

Self-assembled monolayers (SAMs) of alkanethiols are major building blocks for nanotechnology. SAMs provide a functional interface between electrodes and biomolecules, which makes them attractive for biochip fabrication. Although gold has emerged as a standard, copper has several advantages, such as compatibility with semiconductors. However, as copper is easily oxidized in air, patterning SAMs on copper is a challenging task. In this work we demonstrate that submerged laser ablation (SLAB) is well-suited for this purpose, as thiols are exchanged in-situ, avoiding air exposition. Using different types of ω-substituted alkanethiols we show that alkanethiol SAMs on copper surfaces can be patterned using SLAB. The resulting patterns were analyzed by atomic force microscopy (AFM) and scanning electron microscopy (SEM). Both methods indicate that the intense laser beam promotes the exchange of thiols at the copper surface. Furthermore, we present a procedure for the production of free-standing copper nanomembranes, oxidation-protected by alkanethiol SAMs. Incubation of copper-coated mica in alkanethiol solutions leads to SAM formation on both surfaces of the copper film due to intercalation of the organic molecules. Corrosion-protected copper nanomembranes were floated onto water, transferred to electron microscopy grids, and subsequently analyzed by electron energy loss spectroscopy (EELS).

Identification of Metal Oxide Nanoparticles in Histological Samples by Enhanced Darkfield Microscopy and Hyperspectral Mapping.

PubMed

Roth, Gary A; Sosa Peña, Maria del Pilar; Neu-Baker, Nicole M; Tahiliani, Sahil; Brenner, Sara A

2015-12-08

Nanomaterials are increasingly prevalent throughout industry, manufacturing, and biomedical research. The need for tools and techniques that aid in the identification, localization, and characterization of nanoscale materials in biological samples is on the rise. Currently available methods, such as electron microscopy, tend to be resource-intensive, making their use prohibitive for much of the research community. Enhanced darkfield microscopy complemented with a hyperspectral imaging system may provide a solution to this bottleneck by enabling rapid and less expensive characterization of nanoparticles in histological samples. This method allows for high-contrast nanoscale imaging as well as nanomaterial identification. For this technique, histological tissue samples are prepared as they would be for light-based microscopy. First, positive control samples are analyzed to generate the reference spectra that will enable the detection of a material of interest in the sample. Negative controls without the material of interest are also analyzed in order to improve specificity (reduce false positives). Samples can then be imaged and analyzed using methods and software for hyperspectral microscopy or matched against these reference spectra in order to provide maps of the location of materials of interest in a sample. The technique is particularly well-suited for materials with highly unique reflectance spectra, such as noble metals, but is also applicable to other materials, such as semi-metallic oxides. This technique provides information that is difficult to acquire from histological samples without the use of electron microscopy techniques, which may provide higher sensitivity and resolution, but are vastly more resource-intensive and time-consuming than light microscopy.

Effect of Cu content on exfoliation corrosion and electrochemical corrosion of A7N01 aluminum alloy in EXCO solution

NASA Astrophysics Data System (ADS)

He, Yaling; Wang, Xiaomin; Hu, Jie; Zhou, Qiang; Chen, Hui

2017-07-01

The exfoliation corrosion (EXCO) sensitivities and electrochemical corrosions of A7N01 aluminum (Al) alloys with 0.074% and 0.136% Cu contents were investigated in EXCO solution. The exfoliation corrosion developed more rapidly for the alloy with 0.136% Cu by expressing higher exfoliation rate and deeper corrosion pits as observed by SEM and laser confocal scanning microscopy (LCSM). In EXCO solution, the alloy with 0.136% Cu content showed lower open-circuit potential (OCP) than the alloy with 0.074% Cu content. The alloy with 0.136% Cu content had bigger “hysteresis loop” in cyclic polarization curve which meant lower self-passivation ability. In electrochemical impedance spectroscopy plot, its curvature radius and capacitance index were lower. The electrochemical test results revealed that the alloy with 0.136% Cu content showed more severe electrochemical corrosion than the alloy with 0.074% Cu content, consistent with the exfoliation corrosion results. The microstructures of two alloys were observed through optical microscopy (OM) and transmission electron microscopy (TEM). The continuous distribution of the equilibrium precipitate η-MgZn2 on grain boundaries, the decreasing of the width of precipitate-free zone (PFZ) and the coarse Cu-Fe-Si-rich phase were responsible for the higher corrosion sensitivity of the Al alloy with 0.136% Cu than that of Al alloy with 0.074% Cu content in EXCO solution.

Effect of Solution Treatment on Microstructure and Properties of Gd - AZ91 Magnesium Alloy

NASA Astrophysics Data System (ADS)

Li, Yao; Wang, Huiling

2018-01-01

In this paper, the Gd-AZ91 alloy was manufactured by adding rare earth element Gd in AZ91 magnesium alloy. The effects of solution treatment on the microstructures of rare earth elements Gd were investigated by means of optical microscopy, scanning electron microscopy, X-ray diffraction analysis and equipment for testing mechanical properties. The experimental results show that the addition of rare earth element Gd in AZ91 magnesium alloy can refine the alloy grain, turn β-Mg17Al12 phase into a discontinuous network or point structure, and produce granular compound Al2Gd in the alloy; when solution temperature is about 380 °C, the alloy structure is the best, the tensile strength of the alloy is the largest with the value larger than 250Mpa; when the solution temperature exceeds 380 °C, the alloy structure is coarsened and the mechanical properties of the alloy are reduced. With the increase of rare earth element Gd content, the tensile strength of the alloy shows a tendency to increase gradually, which Indicates that the addition of a certain amount of rare earth elements Gd can improve the plasticity of the alloy.

Photocatalytic properties of h-WO3 nanoparticles obtained by annealing and h-WO3 nanorods prepared by hydrothermal method

NASA Astrophysics Data System (ADS)

Boyadjiev, Stefan I.; Nagy-Kovács, Teodóra; Lukács, István; Szilágyi, Imre M.

2016-03-01

In the present study, two different methods for preparing hexagonal WO3 (h-WO3) photocatalysts were used - controlled thermal decomposition and hydrothermal synthesis. WO3 nanoparticles with hexagonal structure were obtained by annealing (NH4)xWO3-y at 500 °C in air. WO3 nanorods were prepared by a hydrothermal method using sodium tungstate Na2WO4, HCl, (COOH)2 and NaSO4 precursors at 200 °C. The formation, morphology, structure and composition of the as-prepared nanoparticles and nanorods were studied by powder X-ray diffraction (XRD), transmission electron microscopy (TEM), and scanning electron microscopy combined with energy-dispersive X-ray spectroscopy (SEM-EDX). The photocatalytic activity of the h-WO3 nanoparticles and nanorods was studied by decomposing methyl orange in aqueous solution under UV light irradiation.

Synthesis of nano-crystalline hydroxyapatite and ammonium sulfate from phosphogypsum waste

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

Mousa, Sahar, E-mail: dollyriri@yahoo.com; King Abdulaziz University, Science and Art College, Chemistry Department, Rabigh Campus, P.O. Box:344, Postal code: 21911 Rabigh; Hanna, Adly

2013-02-15

Graphical abstract: TEM micrograph of dried HAP at 800 °C. -- Abstract: Phosphogypsum (PG) waste which is derived from phosphoric acid manufacture by using wet method was converted into hydroxyapatite (HAP) and ammonium sulfate. Very simple method was applied by reacting PG with phosphoric acid in alkaline medium with adjusting pH using ammonia solution. The obtained nano-HAP was dried at 80 °C and calcined at 600 °C and 900 °C for 2 h. Both of HAP and ammonium sulfate were characterized by X-ray diffraction (XRD) and infrared spectroscopy (IR) to study the structural evolution. The thermal behavior of nano-HAP wasmore » studied; the particle size and morphology were estimated by using transmission electron microscopy (TEM) and scanning electron microscopy (SEM). All the results showed that HAP nano-crystalline and ammonium sulfate can successfully be produced from phosphogypsum waste.« less

Preparation of α-Fe2O3 nanotubes via electrospinning and research on their catalytic properties

NASA Astrophysics Data System (ADS)

Shao, Hao; Zhang, Xuebin; Chen, Fanyan; Liu, Shasha; Ji, Yi; Zhu, Yajun; Feng, Yi

2012-09-01

In this paper, smooth α-Fe2O3 nanotubes have been successfully synthesized by electrospinning of ferric nitrate-polyvinyl alcohol solution followed by calcination in air. The morphologies and structures of the samples were characterized by transmission electron microscopy, scanning electron microscopy and X-ray diffraction. The catalytic properties were studied by differential thermal analysis and thermogravimetric analysis. The results indicated that the as-prepared α-Fe2O3 nanotubes showed a continuous morphology and an extremely high degree of crystallization. The average inner and outer diameters of the obtained α-Fe2O3 nanotubes were about 60 nm and 100 nm, respectively. The obtained α-Fe2O3 nanotubes were able to lower the temperature of the high-temperature thermal decomposition of ammonium perchlorate, while they had little effect on the crystallographic phase transformation and the low-temperature thermal decomposition.

Phase development in a U-7 wt.% Mo vs. Al-7 wt.% Ge diffusion couple

NASA Astrophysics Data System (ADS)

Perez, E.; Keiser, D. D.; Sohn, Y. H.

2013-10-01

Fuel development for the Reduced Enrichment for Research and Test Reactors (RERTR) program has demonstrated that U-Mo alloys in contact with Al develop interaction regions with phases that have poor irradiation behavior. The addition of Si to the Al has been considered with positive results. In this study, compositional modification is considered by replacing Si with Ge to determine the effect on the phase development in the system. The microstructural and phase development of a diffusion couple of U-7 wt.% Mo in contact with Al-7 wt.% Ge was examined by transmission electron microscopy, scanning electron microscopy and energy dispersive spectroscopy. The interdiffusion zone developed a microstructure that included the cubic-UGe3 phase and amorphous phases. The UGe3 phase was observed with and without Mo and Al solid solution developing a (U,Mo)(Al,Ge)3 phase.

CTAB assisted synthesis of tungsten oxide nanoplates as an efficient low temperature NOX sensor

NASA Astrophysics Data System (ADS)

Mehta, Swati S.; Tamboli, Mohaseen S.; Mulla, Imtiaz S.; Suryavanshi, Sharad S.

2018-02-01

Tungsten oxide nanoplates with porous morphology were effectively prepared by acidification using CTAB (HexadeCetyltrimethyl ammonium bromide) as a surfactant. For characterization, the synthesized materials were subjected to X-Ray powder diffraction (XRD), scanning electron microscopy (SEM), high resolution transmission electron microscopy (HRTEM), UV-Visible spectroscopy (UV-Vis) and surface area (BET) measurements. The morphology and size of the particles were controlled by solution acidity. The BET results confirmed that the materials are well crystallized and mesoporous in nature. The nanocrystalline powder was used to prepare thick films by screen printing on alumina substrate for the investigation of gas sensing properties. The gas response measurements revealed that the samples acidified using 10 M H2SO4 exhibits highest response of 91% towards NOX at optimum temperature of 200 °C for 100 ppm, and it also exhibits 35% response at room temperature.

Green synthesis of silver nanoparticles using Alternanthera dentata leaf extract at room temperature and their antimicrobial activity.

PubMed

Kumar, Deenadayalan Ashok; Palanichamy, V; Roopan, Selvaraj Mohana

2014-06-05

A green rapid biogenic synthesis of silver nanoparticles AgNPs using Alternanthera dentata (A. dentata) aqueous extract was demonstrated in this present study. The formation of silver nanoparticles was confirmed by Surface Plasmon Resonance (SPR) at 430nm using UV-visible spectrophotometer. The reduction of silver ions to silver nanoparticles by A. dentata extract was completed within 10min. Synthesized nanoparticles were characterized using UV-visible spectroscopy; Fourier transformed infrared spectroscopy (FT-IR), X-ray diffraction (XRD), scanning electron microscopy and transmission electron microscopy (TEM). The extracellular silver nanoparticles synthesis by aqueous leaf extract demonstrates rapid, simple and inexpensive method comparable to chemical and microbial methods. The colloidal solution of silver nanoparticles were found to exhibit antibacterial activity against Escherichia coli, Pseudomonas aeruginosa, Klebsiella pneumonia and, Enterococcus faecalis. Copyright © 2014 Elsevier B.V. All rights reserved.

Synthesis procedure optimization and characterization of europium (III) tungstate nanoparticles

NASA Astrophysics Data System (ADS)

Rahimi-Nasrabadi, Mehdi; Pourmortazavi, Seied Mahdi; Ganjali, Mohammad Reza; Reza Banan, Ali; Ahmadi, Farhad

2014-09-01

Taguchi robust design as a statistical method was applied for the optimization of process parameters in order to tunable, facile and fast synthesis of europium (III) tungstate nanoparticles. Europium (III) tungstate nanoparticles were synthesized by a chemical precipitation reaction involving direct addition of europium ion aqueous solution to the tungstate reagent solved in an aqueous medium. Effects of some synthesis procedure variables on the particle size of europium (III) tungstate nanoparticles were studied. Analysis of variance showed the importance of controlling tungstate concentration, cation feeding flow rate and temperature during preparation of europium (III) tungstate nanoparticles by the proposed chemical precipitation reaction. Finally, europium (III) tungstate nanoparticles were synthesized at the optimum conditions of the proposed method. The morphology and chemical composition of the prepared nano-material were characterized by means of X-ray diffraction, scanning electron microscopy, transmission electron microscopy, FT-IR spectroscopy and fluorescence.

An in vitro study of the microstructure, composition and nanoindentation mechanical properties of remineralizing human dental enamel

NASA Astrophysics Data System (ADS)

Arsecularatne, J. A.; Hoffman, M.

2014-08-01

This paper describes the results of an in vitro investigation on the interrelations among microstructure, composition and mechanical properties of remineralizing human dental enamel. Polished enamel samples have been demineralized for 10 min in an acetic acid solution (at pH 3) followed by remineralization in human saliva for 30 and 120 min. Microstructure variations of sound, demineralized and remineralized enamel samples have been analysed using focused ion beam, scanning electron microscopy and transmission electron microscopy, while their compositions have been analysed using energy dispersive x-ray. Variations in the mechanical properties of enamel samples have been assessed using nanoindentation. The results reveal that, under the selected conditions, only partial remineralization of the softened enamel surface layer occurs where some pores remain unrepaired. As a result, while the nanoindentation elastic modulus shows an improvement following remineralization, hardness does not.

Functional Carbon Nanofibers with Semi-Embedded Titanium Oxide Particles via Electrospinning.

PubMed

Chang, Guoqing; Ullah, Wajid; Hu, Yunfeng; Lin, Liwei; Wang, Xu; Li, Chang-Zhi

2018-05-22

The formulation of optoelectronic components into 1D nanostructures allows the promotion of new materials with multifunctionalities. In this work, it is demonstrated that new synthesis of photocatalytic carbon nanofiber decorated with semi-embedded titanium oxide (TiO 2 ), namely, TiO 2 @carbon fiber, is conveniently accessed through the electrospinning of polyacrylonitrile polymer and TiO 2 particle comixture, and then followed by photon-activated self-erosion to expose the embedded TiO 2 and carbonization. The hybrid nanofibers are characterized by field emission scanning electron microscopy, transmission electron microscopy, and X-ray diffraction analysis. Furthermore, the photocatalytic activities of the resultant fibers are tested with photodegradation of Rhodamine B in aqueous solution, which reveals that the carbon nanofiber with semi-embedded TiO 2 drastically improved catalytic efficiency and recyclability, comparing to those fibers without or with embedded TiO 2 . © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

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

NASA Astrophysics Data System (ADS)

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

2010-10-01

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

Photocatalytic degradation of organic dyes using composite nanofibers under UV irradiation

NASA Astrophysics Data System (ADS)

Salama, Ahmed; Mohamed, Alaa; Aboamera, Nada M.; Osman, T. A.; Khattab, A.

2018-02-01

In this work, photocatalytic degradation of organic dyes such as methylene blue (MB) and indigo carmine (IC) have been studied by composite nanofibers systems containing cellulose acetate (CA), multiwall carbon nanotubes (CNT) and TiO2 nanoparticles under UV light. The amino factionalized TiO2-NH2 NPs cross-linked to the CA/CNT composite nanofibers works as a semiconductor catalyst. The morphology and crystallinity were characterized by scanning electron microscopy, transmission electron microscopy (TEM), X-ray diffraction, and Fourier transform infrared spectroscopy. It was also seen that many factors affected the photodegradation rate, mainly the pH of the solution and the dye concentration, temperature, etc. The study demonstrated that IC degrades at a higher rate than MB. The maximum photodegradation rate of both organic dyes was achieved at a pH 2. In comparison to other studies, this work achieved high photodegradation rate in lower time and using less power intensity.

STUDY ON SYNTHESIS AND EVOLUTION OF NANOCRYSTALLINE Mg4Ta2O9 BY AQUEOUS SOL-GEL PROCESS

NASA Astrophysics Data System (ADS)

Wu, H. T.; Yang, C. H.; Wu, W. B.; Yue, Y. L.

2012-06-01

Nanosized and highly reactive Mg4Ta2O9 were successfully synthesized by aqueous sol-gel method compared with conventional solid-state method. Ta-Mg-citric acid solution was first formed and then evaporated resulting in a dry gel for calcination in the temperature ranging from 600°C to 800°C for crystallization in oxygen atmosphere. The crystallization process from the gel to crystalline Mg4Ta2O9 was identified by thermal analysis and phase evolution of powders was studied using X-ray diffraction (XRD) technique during calcinations. Particle size and morphology were examined by transmission electron microscopy (TEM) and high resolution scanning electron microscopy (HR-SEM). The results revealed that sol-gel process showed great advantages over conventional solid-state method and Mg4Ta2O9 nanopowders with the size of 20-30 nm were obtained at 800°C.

Solution and electron microscopy characterization of lactococcal phage baseplates expressed in Escherichia coli.

PubMed

Campanacci, Valérie; Veesler, David; Lichière, Julie; Blangy, Stéphanie; Sciara, Giuliano; Moineau, Sylvain; van Sinderen, Douwe; Bron, Patrick; Cambillau, Christian

2010-10-01

We report here the characterization of several large structural protein complexes forming the baseplates (or part of them) of Siphoviridae phages infecting Lactococcus lactis: TP901-1, Tuc2009 and p2. We revisited a "block cloning" expression strategy and extended this approach to genomic fragments encoding proteins whose interacting partners have not yet been clearly identified. Biophysical characterization of some of these complexes using circular dichroism and size exclusion chromatography, coupled with on-line light scattering and refractometry, demonstrated that the over-produced recombinant proteins interact with each other to form large (up to 1.9MDa) and stable baseplate assemblies. Some of these complexes were characterized by electron microscopy confirming their structural homogeneity as well as providing a picture of their overall molecular shapes and symmetry. Finally, using these results, we were able to highlight similarities and differences with the well characterized much larger baseplate of the myophage T4.

Removal combined with reduction of hexavalent chromium from aqueous solution by Fe-ethylene glycol complex microspheres

NASA Astrophysics Data System (ADS)

Zhang, Yong-Xing; Jia, Yong

2016-12-01

Three-dimensional Fe-ethylene glycol (Fe-EG) complex microspheres were synthesized by a facile hydrothermal method, and were characterized by field emission scanning electron microscopy and transmission electron microscopy. The adsorption as well as reduction properties of the obtained Fe-EG complex microspheres towards Cr(VI) ions were studied. The experiment data of adsorption kinetic and isotherm were fitted by nonlinear regression approach. In neutral condition, the maximum adsorption capacity was 49.78 mg g-1 at room temperature, and was increased with the increasing of temperature. Thermodynamic parameters including the Gibbs free energy, standard enthalpy and standard entropy revealed that adsorption of Cr(VI) was a feasible, spontaneous and endothermic process. Spectroscopic analysis revealed the adsorption of Cr(VI) was a physical adsorption process. The adsorbed CrO42- ions were partly reduced to Cr(OH)3 by Fe(II) ions and the organic groups in the Fe-EG complex.

The MOF+ Technique: A Significant Synergic Effect Enables High Performance Chromate Removal.

PubMed

Luo, Ming Biao; Xiong, Yang Yang; Wu, Hui Qiong; Feng, Xue Feng; Li, Jian Qiang; Luo, Feng

2017-12-18

A significant synergic effect between a metal-organic framework (MOF) and Fe 2 SO 4 , the so-called MOF + technique, is exploited for the first time to remove toxic chromate from aqueous solutions. The results show that relative to the pristine MOF samples (no detectable chromate removal), the MOF + method enables super performance, giving a 796 Cr mg g -1 adsorption capacity. The value is almost eight-fold higher than the best value of established MOF adsorbents, and the highest value of all reported porous adsorbents for such use. The adsorption mechanism, unlike the anion-exchange process that dominates chromate removal in all other MOF adsorbents, as unveiled by X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM), and transmission electron microscopy (TEM), is due to the surface formation of Fe 0.75 Cr 0.25 (OH) 3 nanospheres on the MOF samples. © 2017 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

Flexible free-standing TiO2/graphene/PVdF films as anode materials for lithium-ion batteries

NASA Astrophysics Data System (ADS)

Ren, H. M.; Ding, Y. H.; Chang, F. H.; He, X.; Feng, J. Q.; Wang, C. F.; Jiang, Y.; Zhang, P.

2012-12-01

Graphene composites were prepared by hydrothermal method using titanium dioxide (TiO2) adsorbed graphene oxide (GO) sheets as precursors. Free-standing hybrid films for lithium-ion batteries were prepared by adding TiO2/graphene composites to the polyvinylidene fluoride (PVdF)/N-methyl-2-pyrrolidone (NMP) solution, followed by a solvent evaporation technique. These films were characterized by atomic force microscopy (AFM), X-ray diffraction (XRD), scanning electron microscopy (SEM) and various electrochemical techniques. Flexible films show an excellent cycling performance, which was attributed to the interconnected graphene conducting network, which depressed the increasing of electric resistance during the cycling.

Development of a magnetic system for the treatment of Helicobacter pylori infections

NASA Astrophysics Data System (ADS)

Silva, Érica L.; Carvalho, Juliana F.; Pontes, Thales R. F.; Oliveira, Elquio E.; Francelino, Bárbara L.; Medeiros, Aldo C.; do Egito, E. Sócrates T.; Araujo, José H.; Carriço, Artur S.

2009-05-01

We report a study to develop a magnetic system for local delivery of amoxicillin. Magnetite microparticles produced by coprecipitation were coated with a solution of amoxicillin and Eudragit ®S100 by spray drying. Scanning electron microscopy, optical microscopy, X-ray powder diffraction and vibrating sample magnetometry revealed that the particles were superparamagnetic, with an average diameter of 17.2 μm, and an initial susceptibility controllable by the magnetite content in the suspension feeding the sprayer. Our results suggest a possible way to treat Helicobacter pylori infections, using an oral drug delivery system, and open prospects to coat magnetic microparticles by spray drying for biomedical applications.

Highly patterned growth of SnO2 nanowires using a sub-atmospheric vapor-liquid-solid deposition

NASA Astrophysics Data System (ADS)

Akbari, M.; Mohajerzadeh, S.

2017-08-01

We report the realization of tin-oxide nanowires on patterned structures using a vapor-liquid-solid (VLS) process. While gold acts as the catalyst for the growth of wires, a tin-oxide containing sol-gel solution is spin coated on silicon substrate to act as the source for SnO vapor. The growth of tin-oxide nano-structures occurs mostly at the vicinity of the pre-deposited solution. By patterning the gold as the catalyst material, one is able to observe the growth at desired places. The growth of nanowires is highly dense within 100 µm away from such in situ source and their length is of the order of 5 µm. By further distancing from the source, the growth becomes more limited and nanowires become shorter and more sparsely distributed. The growth of nanowires has been studied using scanning and transmission electron microscopy tools while their composition has been investigated using XRD and EDS analyses. As a novel application, we have employed the grown nanowires as electron detection elements to measure the emitted electrons from electron sources. This configuration can be further used as electron detectors for scanning electron microscopes.

Precipitation in Ni-Si during electron and ion irradiation

NASA Astrophysics Data System (ADS)

Lucas, G. E.; Zama, T.; Ishino, S.

1986-11-01

This study was undertaken to further investigate how the nature of the irradiation condition affects precipitation in a dilute Ni-Si system. Transmission electron microscopy (TEM) discs of a solution annealed Ni alloy containing 5 at% Si were irradiated with 400 keV Ar + ions, 200 keV He + ions and 1 MeV electrons at average displacement rates in the range 2 × 10 -5dpa/s to 2 × 10 -3dpa/s at temperatures in the range 25°C to 450°C. Samples irradiated with electrons were observed in situ in an HVEM, while ion irradiated specimens were examined in a TEM after irradiation. Precipitation of Ni 3Si was detected by the appearance of superlattice spots in the electron diffraction patterns. It was found that as the mass of the irradiating species increased, the lower bound temperature at which Ni 3Si precipitation was first observed increased. For electron irradiation, the lower bound temperature at 2 × 10 -3dpa/s was ˜125°C, whereas for 400 keV Ar + irradiation at a similar average displacement rate the lower boundary was approximately 325°C. This suggests that cascade disordering competes with radiation induced solute segregation.

Conductive indium-tin oxidenanowire and nanotube arrays made by electrochemically assisted deposition in template membranes: switching between wire and tube growth modes by surface chemical modification of the template

NASA Astrophysics Data System (ADS)

Kovtyukhova, Nina I.; Mallouk, Thomas E.

2011-04-01

Tin-doped indium hydroxide (InSnOH) nanowires (NWs) and nanotubes (NTs) were grown from acidic aqueous solutions of inorganic precursors in a simple one-step electrochemically assisted deposition (EAD) process inside Au-plugged anodic aluminium oxide and polycarbonatemembranes. When the membranes were used without any pre-treatment, InSnOH crystals nucleated on the both the Au-cathode and pore wall surfaces. By adjusting the surface chemistry of Au or the pore walls, it was possible to switch between NW and NT growth modes. InSnOH was converted into indiumtin oxide (ITO) by annealing the InSnOH-filled membranes at 300 °C. The resulting wires and tubes were characterized by field emission scanning electron microscopy, transmission electron microscopy, X-ray and electron diffraction, Auger electron spectroscopy and electrical conductivity measurements. InSnOH and ITO NWs and NTs consisted of ~25-50 nm in size crystalline grains with the cubic crystal structures of In(OH)3 and In2O3, respectively, and showed essentially the same morphological features as planar ITO films made by the same method. Separate tin oxide/hydroxide phases were not observed by any of the characterization methods. After heating in air at 600 °C, the ITO NWs had resistivity on the order of 10°Ω cm. EAD is an inexpensive and scalable solution-based technique, and allows one to grow dense arrays of vertically aligned, crystalline and conductive ITO NWs and NTs.

Electron microscopy of whole cells in liquid with nanometer resolution

PubMed Central

de Jonge, N.; Peckys, D. B.; Kremers, G. J.; Piston, D. W.

2009-01-01

Single gold-tagged epidermal growth factor (EGF) molecules bound to cellular EGF receptors of fixed fibroblast cells were imaged in liquid with a scanning transmission electron microscope (STEM). The cells were placed in buffer solution in a microfluidic device with electron transparent windows inside the vacuum of the electron microscope. A spatial resolution of 4 nm and a pixel dwell time of 20 μs were obtained. The liquid layer was sufficiently thick to contain the cells with a thickness of 7 ± 1 μm. The experimental findings are consistent with a theoretical calculation. Liquid STEM is a unique approach for imaging single molecules in whole cells with significantly improved resolution and imaging speed over existing methods. PMID:19164524

Multiphase materials with lignin. VI. Effect of cellulose derivative structure on blend morphology with lignin

Treesearch

Timothy G. Rials; Wolfgang G. Glasser

1989-01-01

Polymeric blends of lignin with ethyl cellulose (EC) and cellulose acetate/butyrate (CAB) prepared by solution casting from dioxane. Fracture surface analysis by scanning electron microscopy revealed phase separation when the lignin content exceeded 10% for blends with EC and 5% in the CAB system. While this phase behavior is as predicted for the EC blends, a greater...

Corrosion Behavior of Metal Active Gas Welded Joints of a High-Strength Steel for Automotive Application

NASA Astrophysics Data System (ADS)

Garcia, Mainã Portella; Mantovani, Gerson Luiz; Vasant Kumar, R.; Antunes, Renato Altobelli

2017-10-01

In this work, the corrosion behavior of metal active gas-welded joints of a high-strength steel with tensile yield strength of 900 MPa was investigated. The welded joints were obtained using two different heat inputs. The corrosion behavior has been studied in a 3.5 wt.% NaCl aqueous solution using electrochemical impedance spectroscopy and potentiodynamic polarization tests. Optical microscopy images, scanning electron microscopy and transmission electron microscopy with energy-dispersive x-ray revealed different microstructural features in the heat-affected zone (HAZ) and the weld metal (WM). Before and after the corrosion process, the sample was evaluated by confocal laser scanning microscopy to measure the depth difference between HAZ and WM. The results showed that the heat input did not play an important role on corrosion behavior of HSLA steel. The anodic and cathodic areas of the welded joints could be associated with depth differences. The HAZ was found to be the anodic area, while the WM was cathodic with respect to the HAZ. The corrosion behavior was related to the amount and orientation nature of carbides in the HAZ. The microstructure of the HAZ consisted of martensite and bainite, whereas acicular ferrite was observed in the weld metal.

Synthesis and Photoluminescence Characteristics of Eu(3+)-Doped Molybdates Nanocrystals.

PubMed

Li, Fuhai; Yu, Lixin; Wei, Shuilin; Sun, Jiaju; Chen, Weiqing; Sun, Wei

2015-12-01

In this paper, the Eu(3+)-doped molybdate (CaMoO4, ZnMoO4 and BaMoO4) phosphors have been prepared by a hydrothermal method through modulating the pH value of the precursor solution (pH = 8, 10, and 12, respectively). The crystalline phase, morphology, photoluminescent properties of the prepared samples were systematically characterized by means of X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM) and photoluminescence (PL) spectra. The results indicate that the photoluminescence and morphology can be affected by the precursor solution. And the growth of the ZnMoO4 crystals also can be affected by the pH value of the precursor solution.

Utilization of fish bone as adsorbent of Fe3+ ion by controllable removal of its carbonaceous component

NASA Astrophysics Data System (ADS)

Nurhadi, M.; Kusumawardani, R.; Widiyowati, I. I.; Wirhanuddin; Nur, H.

2018-05-01

The performance of fish bone to adsorb Fe3+ ion in solution was studied. Powdered fish bone and carbonized fish bone were used as adsorbent. All absorbents were characterized by X-ray diffraction (XRD), IR spectroscopy, nitrogen adsorption, scanning electron microscopy (SEM) and TG analysis. Powdered fish bone and carbonized fish bone were effective as adsorbent for removing Fe3+ ion in solution. The metal adsorptions of Fe3+ ion were 94 and 98% for powdered fish bone and fish bone which carbonized at 400 and 500 °C.

Removal of Cu(II) metal ions from aqueous solution by amine functionalized magnetic nanoparticles

NASA Astrophysics Data System (ADS)

Kothavale, V. P.; Karade, V. C.; Waifalkar, P. P.; Sahoo, Subasa C.; Patil, P. S.; Patil, P. B.

2018-04-01

The adsorption behavior of Cu(II) metal cations was investigated on the amine functionalized magnetic nanoparticles (MNPs). TheMNPs were synthesized by thesolvothermal method and functionalized with (3-Aminopropyl)triethoxysilane (APTES). MNPs were characterized by X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM) and vibrating sample magnetometer (VSM). The MNPs have pure magnetite phase with particle size around 10-12 nm. MNPs exhibits superparamagnetic behavior with asaturation magnetization of 68 emu/g. The maximum 38 % removal efficiency was obtained for Cu(II) metal ions from the aqueous solution.

Study of the Formation and Solution Properties of Worm-Like Micelles Formed Using Both N-Hexadecyl-N-Methylpiperidinium Bromide-Based Cationic Surfactant and Anionic Surfactant

PubMed Central

Yan, Zhihu; Dai, Caili; Feng, Haishun; Liu, Yifei; Wang, Shilu

2014-01-01

The viscoelastic properties of worm-like micelles formed by mixing the cationic surfactant N-hexadecyl-N-methylpiperidinium bromide (C16MDB) with the anionic surfactant sodium laurate (SL) in aqueous solutions were investigated using rheological measurements. The effects of sodium laurate and temperature on the worm-like micelles and the mechanism of the observed shear thinning phenomenon and pseudoplastic behavior were systematically investigated. Additionally, cryogenic transmission electron microscopy images further ascertained existence of entangled worm-like micelles. PMID:25296131

Specific physical and chemical properties of two modifications of poly(N-vinylcaprolcatam)

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

Chihacheva, I. P.; Timaeva, O. I.; Kuz’micheva, G. M., E-mail: galina-kuzmicheva@list.ru

2016-05-15

Two modifications of poly(N-vinylcaprolactam)—PVCL25 and PVCL40 (drying of a PVCL solution at 25 and 40°C, respectively)—as powdered films and their solutions were systematically investigated for the first time. Powders were studied by X-ray diffraction, IR spectroscopy, scanning electron microscopy, low-temperature krypton adsorption, and differential scanning calorimetry. Solutions were studied by smallangle X-ray scattering and dynamic light scattering. It was demonstrated that powders of PVCL25 and PVCL40 differ in the characteristics of the sub- and microstructure and in the water content and the solutions differ in the particle size. The relationships between the characteristics of the systems in the solid andmore » liquid state and between the hydrodynamic diameter of PVCL particles in solution and their coagulation time were found.« less

Electrochemical characteristics of bioresorbable binary MgCa alloys in Ringer's solution: Revealing the impact of local pH distributions during in-vitro dissolution.

PubMed

Mareci, D; Bolat, G; Izquierdo, J; Crimu, C; Munteanu, C; Antoniac, I; Souto, R M

2016-03-01

Biodegradable magnesium-calcium (MgCa) alloy is a very attractive biomaterial. Two MgCa alloys below the solid solubility of Ca were considered, as to solely investigate the effect of Ca content on the behavior of magnesium and the pH changes associated to metal dissolution. X-ray diffraction analysis and optical microscopy showed that both Mg-0.63Ca and Mg-0.89Ca alloys were solely composed of α(Mg) phase. Degradation characteristics and electrochemical characterization of MgCa alloys were investigated during exposure to Ringer's solution at 37 °C by electrochemical impedance spectroscopy and scanning electrochemical microscopy. The impedance behavior showed both capacitive and inductive features that are related to the alloy charge transfer reaction and the relaxation of the absorbed corrosion compounds, and can be described in terms of an equivalent circuit. Scanning electron microscopy (SEM) was employed to view the surface morphology of the MgCa samples after 1 week immersion in Ringer's solution showing extensive precipitation of corrosion products, whereas the substrate shows evidence of a non-uniform corrosion process. Energy dispersive analysis showed that the precipitates contained oxygen, calcium, magnesium and chlorine, and the Mg:Ca ratios were smaller than in the alloys. Scanning electrochemical microscopy (SECM) was used to visualize local pH changes associated to these physicochemical processes with high spatial resolution. The occurrence of pH variations in excess of 3 units between anodic and cathodic half-cell reactions was monitored in situ. Copyright © 2015 Elsevier B.V. All rights reserved.

Ab initio structure determination of nanocrystals of organic pharmaceutical compounds by electron diffraction at room temperature using a Timepix quantum area direct electron detector

PubMed Central

van Genderen, E.; Clabbers, M. T. B.; Das, P. P.; Stewart, A.; Nederlof, I.; Barentsen, K. C.; Portillo, Q.; Pannu, N. S.; Nicolopoulos, S.; Gruene, T.; Abrahams, J. P.

2016-01-01

Until recently, structure determination by transmission electron microscopy of beam-sensitive three-dimensional nanocrystals required electron diffraction tomography data collection at liquid-nitrogen temperature, in order to reduce radiation damage. Here it is shown that the novel Timepix detector combines a high dynamic range with a very high signal-to-noise ratio and single-electron sensitivity, enabling ab initio phasing of beam-sensitive organic compounds. Low-dose electron diffraction data (∼0.013 e− Å−2 s−1) were collected at room temperature with the rotation method. It was ascertained that the data were of sufficient quality for structure solution using direct methods using software developed for X-ray crystallography (XDS, SHELX) and for electron crystallography (ADT3D/PETS, SIR2014). PMID:26919375

Enhanced corrosion resistance of strontium hydroxyapatite coating on electron beam treated surgical grade stainless steel

NASA Astrophysics Data System (ADS)

Gopi, D.; Rajeswari, D.; Ramya, S.; Sekar, M.; R, Pramod; Dwivedi, Jishnu; Kavitha, L.; Ramaseshan, R.

2013-12-01

The surface of 316L stainless steel (316L SS) is irradiated by high energy low current DC electron beam (HELCDEB) with energy of 500 keV and beam current of 1.5 mA followed by the electrodeposition of strontium hydroxyapatite (Sr-HAp) to enhance its corrosion resistance in physiological fluid. The coatings were characterised by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR) and High resolution scanning electron microscopy (HRSEM). The Sr-HAp coating on HELCDEB treated 316L SS exhibits micro-flower structure. Electrochemical results show that the Sr-HAp coating on HELCDEB treated 316L SS possesses maximum corrosion resistance in Ringer's solution.

Conducting Polymeric Hydrogel Electrolyte Based on Carboxymethylcellulose and Polyacrylamide/Polyaniline for Supercapacitor Applications

NASA Astrophysics Data System (ADS)

Suganya, N.; Jaisankar, V.; Sivakumar, E. K. T.

Conducting polymer hydrogels represent a unique class of materials that possess enormous application in flexible electronic devices. In the present work, conducting carboxymethylcellulose (CMC)-co-polyacrylamide (PAAm)/polyaniline was synthesized by a two-step interpenetrating network solution polymerization technique. The synthesized CMC-co-PAAm/polyaniline with interpenetrating network structure was prepared by in situ polymerization of aniline to enhance conductivity. The molecular structure and morphology of the copolymer hydrogels were characterized by Fourier transform infrared spectroscopy and scanning electron microscopy. The novel conducting polymer hydrogels show good electrical and electrochemical behavior, which makes them potentially useful in electronic devices such as supercapacitors, biosensors, bioelectronics, solar cells and memory devices.

One-dimensional self-confinement promotes polymorph selection in large-area organic semiconductor thin films.

PubMed

Giri, Gaurav; Li, Ruipeng; Smilgies, Detlef-M; Li, Er Qiang; Diao, Ying; Lenn, Kristina M; Chiu, Melanie; Lin, Debora W; Allen, Ranulfo; Reinspach, Julia; Mannsfeld, Stefan C B; Thoroddsen, Sigurdur T; Clancy, Paulette; Bao, Zhenan; Amassian, Aram

2014-04-16

A crystal's structure has significant impact on its resulting biological, physical, optical and electronic properties. In organic electronics, 6,13(bis-triisopropylsilylethynyl)pentacene (TIPS-pentacene), a small-molecule organic semiconductor, adopts metastable polymorphs possessing significantly faster charge transport than the equilibrium crystal when deposited using the solution-shearing method. Here, we use a combination of high-speed polarized optical microscopy, in situ microbeam grazing incidence wide-angle X-ray-scattering and molecular simulations to understand the mechanism behind formation of metastable TIPS-pentacene polymorphs. We observe that thin-film crystallization occurs first at the air-solution interface, and nanoscale vertical spatial confinement of the solution results in formation of metastable polymorphs, a one-dimensional and large-area analogy to crystallization of polymorphs in nanoporous matrices. We demonstrate that metastable polymorphism can be tuned with unprecedented control and produced over large areas by either varying physical confinement conditions or by tuning energetic conditions during crystallization through use of solvent molecules of various sizes.

Dissolution and Characterization of Boron Nitride Nanotubes in Superacid.

PubMed

Kleinerman, Olga; Adnan, Mohammed; Marincel, Daniel M; Ma, Anson W K; Bengio, E Amram; Park, Cheol; Chu, Sang-Hyon; Pasquali, Matteo; Talmon, Yeshayahu

2017-12-19

Boron nitride nanotubes (BNNTs) are of interest for their unique combination of high tensile strength, high electrical resistivity, high neutron cross section, and low reactivity. The fastest route to employing these properties in composites and macroscopic articles is through solution processing. However, dispersing BNNTs without functionalization or use of a surfactant is challenging. We show here by cryogenic transmission electron microscopy that BNNTs spontaneously dissolve in chlorosulfonic acid as disentangled individual molecules. Electron energy loss spectroscopy of BNNTs dried from the solution confirms preservation of the sp 2 hybridization for boron and nitrogen, eliminating the possibility of BNNT functionalization or damage. The length and diameter of the BNNTs was statistically calculated to be ∼4.5 μm and ∼4 nm, respectively. Interestingly, bent or otherwise damaged BNNTs are filled by chlorosulfonic acid. Additionally, nanometer-sized synthesis byproducts, including boron nitride clusters, isolated single and multilayer hexagonal boron nitride, and boron particles, were identified. Dissolution in superacid provides a route for solution processing BNNTs without altering their chemical structure.

Influence of Solution Treatment Duration on Microstructural Features of an Industrial Forged UNS S32750/1.4410/F53 Super Duplex Stainless Steel (SDSS) Alloy

NASA Astrophysics Data System (ADS)

Cojocaru, Vasile Dănuţ; Răducanu, Doina; Angelescu, Mariana Lucia; Vintilă, Adrian Nicolae; Şerban, Nicolae; Dan, Ioan; Cojocaru, Elisabeta Mirela; Cinca, Ion

2017-08-01

The microstructural changes induced by solution treatment of an industrial forged F53 Super Duplex Stainless Steel alloy were studied, in order to emphasize how component phases are influenced by heat treatment temperature and duration. The solution treatment was done at a temperature of 1100°C, with variable holding times: 0.6 ks (10 min), 3.6 ks (60 min) and 10.8 ks (180 min). Scanning electron microscopy-electron backscattered diffraction was used as main characterization technique, to obtain and analyse data referring to microstructural features, such as: nature and morphology of constituent phases, average grain-size and grain misorientation. It was shown that in all studied cases the microstructure consisted of a mixture of about 45% δ-Fe (ferrite) and 55% γ-Fe (austenite). Besides δ-Fe and γ-Fe phases, other phases were also identified, such as τ-phase (chromium-iron carbide), σ-phase (chromium-iron) and δ-(Cr-Fe) (ferrite).

Microstructural, phase evolution and corrosion properties of silicon carbide reinforced pulse electrodeposited nickel-tungsten composite coatings

NASA Astrophysics Data System (ADS)

Singh, Swarnima; Sribalaji, M.; Wasekar, Nitin P.; Joshi, Srikant; Sundararajan, G.; Singh, Raghuvir; Keshri, Anup Kumar

2016-02-01

Silicon carbide (SiC) reinforced nickel-tungsten (Ni-W) coatings were successfully fabricated on steel substrate by pulse electrodeposition method (PED) and the amount of SiC was varied as 0 g/l, 2 g/l, and 5 g/l in Ni-W coating. Effect of subsequent addition of SiC on microstructures, phases and on corrosion property of the coating was investigated. Field emission scanning electron microscopy (FE-SEM) image of the surface morphology of the coating showed the transformation from the dome like structure to turtle shell like structure. X-ray diffraction (XRD) of Ni-W-5 g/l SiC showed the disappearance of (220) plane of Ni(W), peak splitting in major peak of Ni(W) and formation of distinct peak of W(Ni) solid solution. Absence of (220) plane, peak splitting and presence of W(Ni) solid solution was explained by the high resolution transmission electron microscopy (HR-TEM) images. Tafel polarization plot was used to study the corrosion property of the coatings in 0.5 M NaCl solution. Ni-W-5 g/l SiC coating was showed higher corrosion resistance (i.e. ∼21% increase in corrosion potential, Ecorr) compared to Ni-W coating. Two simultaneous phenomena have been identified for the enhanced corrosion resistance of Ni-W-5 g/l SiC coating. (a) Presence of crystallographic texture (b) formation of continuous double barrier layer of NiWO4 and SiO2.

TiO2 Nanorods Preparation from Titanyl Sulphate Produced by Dissolution of Ilmenite

NASA Astrophysics Data System (ADS)

Wahyuningsih, S.; Rinawati, L.; Munifa, R. M. I.; Ramelan, A. H.; Sulistyono, Eko

2017-02-01

One-dimensional titanium oxides (TiO2) nanorods have substantial applications in photocatalytic, nanoelectronic, and photoelectrochemical solar cells. These applications require large quantities of materials and a production technique suitable for future industry fabrication. We demonstrate here a new method of TiO2 nanorods production from ilmenite sands (FeTiO3). In this process, the roasted ilmenite sand was separated from the iron content and dissolved in the sulphuric acid solution. Separation process of TiO2 from ilmenite has been carried out by roasting, leaching and precipitation processes. The roasting process was conducted by the addition of Na2S at a temperature of 800°C that had been deomposed ilmenite into hematite (Fe2O3), anatase TiO2, rutile TiO2, Na2SO4, NaFeS2 and NaFeO2. Separation TiO2 from titanyl sulfate (TiOSO4) after leaching in H2SO4 solution was conducted by hydrolysis-condensation step and complexation step of Fe2+ content. KCNS solution was used as a complexing agent. The xerogel synthesized TiO2 then was prepared to 1-D nanostructure of TiO2 nanorods by hydrothermal process under alkaline condition. By the two-step method, we finally gain the 1D nanorods TiO2 extracted from ilmenite sand. The characterization using the Scanning Electron Microscopy (SEM) and Transmission Electron Microscopy (TEM) obtained the nanorod morphology at a diameter about 9.6 nm.

Nano-TiO2, ultrasound and sequential nano-TiO2/ultrasonic degradation of N-acetyl-para-aminophenol from aqueous solution.

PubMed

Ayanda, Olushola S; Nelana, Simphiwe M; Petrik, Leslie F; Naidoo, Eliazer B

2017-10-01

The application of nano-TiO 2 as adsorbent combined with ultrasound for the degradation of N-acetyl-para-aminophenol (AAP) from aqueous solution was investigated. The nano-TiO 2 was characterized by means of powder X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), energy dispersive spectroscopy (EDS), and attenuated total reflection-Fourier transform infrared spectroscopy (ATR-FTIR). Experimental results revealed that the adsorption of AAP by nano-TiO 2 fitted the pseudo-second-order kinetic model, the equilibrium could be explained by the Freundlich isotherm and the treatment process is exothermic. The optimum removal efficiency of AAP (128.89 mg/g (77.33%)) was achieved at pH 4 when 0.03 g of nano-TiO 2 was mixed with 50 mL of 100 mg/L AAP aqueous solution at ambient temperature, 60 min contact time, and a stirring speed of 120 rpm. Ultrasound at 20 kHz and pH 3 was favorable and it resulted in 52.61% and 57.43% removal efficiency with and without the addition of nano-TiO 2 , respectively. The degradation of AAP by ultrasound followed by nano-TiO 2 treatment resulted in approximately 99.50% removal efficiency. This study showed that a sequential ultrasound and nano-TiO 2 treatment process could be employed for the removal of AAP or other emerging water and wastewater contaminants.

Hierarchically assembled Au microspheres and sea urchin-like architectures: formation mechanism and SERS study

NASA Astrophysics Data System (ADS)

Wang, Xiansong; Yang, Da-Peng; Huang, Peng; Li, Min; Li, Chao; Chen, Di; Cui, Daxiang

2012-11-01

The hierarchically assembled Au microspheres/sea urchin-like structures have been synthesized in aqueous solution at room temperature with and without proteins (bovine serum albumin, BSA) as mediators. The average diameter of an individual Au microsphere is 300-600 nm, which is composed of some compact nanoparticles with an average diameter of about 15 nm. Meanwhile, the sea urchin-like Au architecture exhibits an average diameter of 600-800 nm, which is made up of some nanopricks with an average length of 100-200 nm. These products are characterized by means of scanning electron microscopy (SEM), X-ray diffraction (XRD) and transmission electronic microscopy (TEM). It is found that the BSA and ascorbic acid (AA) have great effects on the morphology of the resulting products. Two different growth mechanisms are proposed. The study on surface enhanced Raman scattering (SERS) activities is also carried out between Au microspheres and Au sea urchin-like architectures. It is found that Au urchin-like architectures possess much higher SERS activity than the Au microspheres. Our work may shed light on the design and synthesis of hierarchically self-assembled 3D micro/nano-architectures for SERS, catalysis and biosensors.The hierarchically assembled Au microspheres/sea urchin-like structures have been synthesized in aqueous solution at room temperature with and without proteins (bovine serum albumin, BSA) as mediators. The average diameter of an individual Au microsphere is 300-600 nm, which is composed of some compact nanoparticles with an average diameter of about 15 nm. Meanwhile, the sea urchin-like Au architecture exhibits an average diameter of 600-800 nm, which is made up of some nanopricks with an average length of 100-200 nm. These products are characterized by means of scanning electron microscopy (SEM), X-ray diffraction (XRD) and transmission electronic microscopy (TEM). It is found that the BSA and ascorbic acid (AA) have great effects on the morphology of the resulting products. Two different growth mechanisms are proposed. The study on surface enhanced Raman scattering (SERS) activities is also carried out between Au microspheres and Au sea urchin-like architectures. It is found that Au urchin-like architectures possess much higher SERS activity than the Au microspheres. Our work may shed light on the design and synthesis of hierarchically self-assembled 3D micro/nano-architectures for SERS, catalysis and biosensors. Electronic supplementary information (ESI) available. See DOI: 10.1039/c2nr32405a

Effect of intrinsic electronic defect states on the morphology and optoelectronic properties of Sn-rich SnS particles

NASA Astrophysics Data System (ADS)

Singh, Chetan C.; Panda, Emila

2018-05-01

A small variation in the elemental composition of a chemical compound can cause the formation of additional electronic defect states in the material, thereby altering the overall microstructure and thus induced properties. In this work, we observed chemical constitution-induced modification in the morphology and optoelectronic properties of SnS. To this end, SnS particles were prepared using the solution chemical route and were characterized using a wide range of experimental techniques, such as x-ray diffractometry, field emission scanning electron microscopy, high resolution transmission electron microscopy, energy dispersive spectroscopy (EDS), x-ray photoelectron spectroscopy (XPS), UV-Vis spectrophotometry, and scanning tunneling spectroscopy (STS). All these SnS particles are found to be Sn-rich and p-type. However, distinctly different morphologies (i.e., flower-like and aggregated ones) are observed. These are then correlated with the electronic defect states, which are induced because of the presence of Sn vacancies, Sn antisites, and/or Sn interstitials. A combination of EDS, XPS, and STS data confirmed the presence of a higher concentration of Sn vacancies along with lower quantities of Sn interstitials and/or antisites in the SnS particles with flower-like morphologies giving rise to higher hole concentration, which subsequently leads to reduced transport, optical band gaps, and barrier heights.

Pitting corrosion of titanium. Interim report, June-December 1993

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

Casillas, N.; Charlebois, S.J.; Smyrl, W.H.

1994-01-20

The breakdown of native and anodically-grown oxide films on Ti electrodes is investigated by scanning electrochemical microscopy (SECM), video microscopy, transmission electron microscopy and voltammetry. SECM is used to demonstrate that the oxidation of Br- on Ti occurs at microscopic surface sites (10 - 50 micrometer diameter, 30 sites/sq cm) that are randomly positioned across the oxide surface. After determining the position of the active sites for Br- oxidation, breakdown of the oxide is initiated by increasing the electrode potential to more positive values. Direct correspondence is observed between the location of the electroactive sites and corrosion pits, indicating thatmore » oxide breakdown is associated with a localized site of high electrical conductivity. The potential at which pitting is observed in voltammetric experiments is found to be proportional to the average oxide thickness, for values ranging between 20 and 100 A, indicating that breakdown is determined either by the magnitude of the electric field within the oxide or by the interfacial potential at the oxide/Br- solution interface. Pitting occurs at significantly lower potentials in Br- solutions than in C 1- solutions, suggesting a strong chemical interaction between the TiO2 surface and Br-. A mechanism of oxide breakdown is proposed that is based on the potential-dependent chemical dissolution of the oxide at microscopic surface sites.« less

Fabrication of resistively-coupled single-electron device using an array of gold nanoparticles

NASA Astrophysics Data System (ADS)

Huong, Tran Thi Thu; Matsumoto, Kazuhiko; Moriya, Masataka; Shimada, Hiroshi; Kimura, Yasuo; Hirano-Iwata, Ayumi; Mizugaki, Yoshinao

2017-08-01

We demonstrated one type of single-electron device that exhibited electrical characteristics similar to those of resistively-coupled SE transistor (R-SET) at 77 K and room temperature (287 K). Three Au electrodes on an oxidized Si chip served as drain, source, and gate electrodes were formed using electron-beam lithography and evaporation techniques. A narrow (70-nm-wide) gate electrode was patterned using thermal evaporation, whereas wide (800-nm-wide) drain and source electrodes were made using shadow evaporation. Subsequently, aqueous solution of citric acid and 15-nm-diameter gold nanoparticles (Au NPs) and toluene solution of 3-nm-diameter Au NPs chemisorbed via decanethiol were dropped on the chip to make the connections between the electrodes. Current-voltage characteristics between the drain and source electrodes exhibited Coulomb blockade (CB) at both 77 and 287 K. Dependence of the CB region on the gate voltage was similar to that of an R-SET. Simulation results of the model based on the scanning electron microscopy image of the device could reproduce the characteristics like the R-SET.

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

NASA Astrophysics Data System (ADS)

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

2018-06-01

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

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

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

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

2014-12-01

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

CTAB-assisted hydrothermal synthesis of YVO 4:Eu 3+ powders in a wide pH range

NASA Astrophysics Data System (ADS)

Wang, Juan; Hojamberdiev, Mirabbos; Xu, Yunhua

2012-01-01

Rhombus-, rod-, soya bean- and aggregated soya bean-like YVO 4:Eu 3+ micro- and nanostructures were synthesized by a cetyltrimethylammonium bromide (CTAB)-assisted hydrothermal method at 180 °C for 24 h in a wide pH range. The as-synthesized powders were characterized by X-ray powder diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and photoluminescence spectroscopy (PL). The XRD results confirmed the formation of phase-pure YVO 4:Eu 3+ powders with tetragonal structure under hydrothermal process in a wide pH range. Electron microscopic observations evidenced the morphological transformation of YVO 4:Eu 3+ powders from rhombus-like microstructure to rod-, soya bean, and aggregated soya bean-like nanostructures with an increase in the pH of the synthesis solution. The results from the PL measurements revealed that the intensities of PL emission peaks were significantly affected by the morphologies and crystallinity of samples due to the absence of an inversion symmetry at the Eu 3+ lattice site, and the highest luminescence intensity was observed for rod-like YVO 4:Eu 3+ powders.

Room temperature synthesis of silver nanowires from tabular silver bromide crystals in the presence of gelatin

NASA Astrophysics Data System (ADS)

Liu, Suwen; Wehmschulte, Rudolf J.; Lian, Guoda; Burba, Christopher M.

2006-03-01

Long silver nanowires were synthesized at room temperature by a simple and fast process derived from the development of photographic films. A film consisting of an emulsion of tabular silver bromide grains in gelatin was treated with a photographic developer (4-(methylamino)phenol sulfate (metol), citric acid) in the presence of additional aqueous silver nitrate. The silver nanowires have lengths of more than 50 μm, some even more than 100 μm, and average diameters of about 80 nm. Approximately, 70% of the metallic silver formed in the reduction consists of silver nanowires. Selected area electron diffraction (SAED) results indicate that the silver nanowires grow along the [111] direction. It was found that the presence of gelatin, tabular silver bromide crystals and silver ions in solution are essential for the formation of the silver nanowires. The nanowires appear to originate from the edges of the silver bromide crystals. They were characterized by transmission electron microscopy (TEM), SAED, scanning electron microscopy (SEM), and powder X-ray diffraction (XRD).

Room temperature synthesis of silver nanowires from tabular silver bromide crystals in the presence of gelatin

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

Liu Suwen; Wehmschulte, Rudolf J.; Lian Guoda

2006-03-15

Long silver nanowires were synthesized at room temperature by a simple and fast process derived from the development of photographic films. A film consisting of an emulsion of tabular silver bromide grains in gelatin was treated with a photographic developer (4-(methylamino)phenol sulfate (metol), citric acid) in the presence of additional aqueous silver nitrate. The silver nanowires have lengths of more than 50 {mu}m, some even more than 100 {mu}m, and average diameters of about 80 nm. Approximately, 70% of the metallic silver formed in the reduction consists of silver nanowires. Selected area electron diffraction (SAED) results indicate that the silvermore » nanowires grow along the [111] direction. It was found that the presence of gelatin, tabular silver bromide crystals and silver ions in solution are essential for the formation of the silver nanowires. The nanowires appear to originate from the edges of the silver bromide crystals. They were characterized by transmission electron microscopy (TEM), SAED, scanning electron microscopy (SEM), and powder X-ray diffraction (XRD)« less

Effect of polymer matrix on structure of Se particles formed in aqueous solutions during redox process

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

Suvorova, E. I., E-mail: suvorova@ns.crys.ras.ru; Klechkovskaya, V. V.

2010-12-15

Transmission electron microscopy and X-ray energy dispersive microanalysis study of the structure of particles formed during the reduction of Se(IV) to Se(0) in aqueous solutions in the presence of amphiphilic polymers showed the formation of Se/polymer composite particles. The content of carbon inside the particles can be as large as 80 at %. Polymers deeply influence the structure of particles. Depending on polymers, the composite particles may be unstable with time and they spontaneously evolve from Se/polymer composite particles to crystalline particles of monoclinic Se. For the stable ones, addition of bacterial cellulose Acetobacter xylinum gel-film can induce crystallization inmore » the particles which expel the polymeric material. The Se/polymer composite particles and Se crystalline particles exhibit different sensitivity to electron irradiation and stiffness.« less

Investigating the interaction of x-ray free electron laser radiation with grating structure.

PubMed

Gaudin, Jérôme; Ozkan, Cigdem; Chalupský, Jaromír; Bajt, Saša; Burian, Tomáš; Vyšín, Ludek; Coppola, Nicola; Farahani, Shafagh Dastjani; Chapman, Henry N; Galasso, Germano; Hájková, Vera; Harmand, Marion; Juha, Libor; Jurek, Marek; Loch, Rolf A; Möller, Stefan; Nagasono, Mitsuru; Störmer, Michael; Sinn, Harald; Saksl, Karel; Sobierajski, Ryszard; Schulz, Joachim; Sovak, Pavol; Toleikis, Sven; Tiedtke, Kai; Tschentscher, Thomas; Krzywinski, Jacek

2012-08-01

The interaction of free electron laser pulses with grating structure is investigated using 4.6±0.1 nm radiation at the FLASH facility in Hamburg. For fluences above 63.7±8.7 mJ/cm2, the interaction triggers a damage process starting at the edge of the grating structure as evidenced by optical and atomic force microscopy. Simulations based on solution of the Helmholtz equation demonstrate an enhancement of the electric field intensity distribution at the edge of the grating structure. A procedure is finally deduced to evaluate damage threshold.

A study of fullerene-quantum dot composite structure on substrates with a transparent electrode layer

NASA Astrophysics Data System (ADS)

Pavlov, S. I.; Kirilenko, D. A.; Nashchekin, A. V.; Sokolov, R. V.; Konnikov, S. G.

2015-02-01

We have studied the structure of films consisting of fullerene clusters and a related fullerene-based composite with incorporated quantum dots. The films were obtained by electrophoretic deposition from solution onto glass substrates with a transparent indium-doped tin oxide (ITO) electrode layer. The average cluster size, as measured by electron microscopy, amounts to 300 nm in pure fullerene films and 800 nm in the composite material. Electron diffraction measurements showed that pure fullerene clusters had an fcc lattice, while the introduction of quantum dots rendered the fullerene matrix predominantly amorphous.

Deposition of an Ultraflat Graphene Oxide Nanosheet on Atomically Flat Substrates

NASA Astrophysics Data System (ADS)

Khan, M. Z. H.; Shahed, S. M. F.; Yuta, N.; Komeda, T.

2017-07-01

In this study, graphene oxide (GO) sheets produced in the form of stable aqueous dispersions were deposited on Au (111), freshly cleaved mica, and highly oriented pyrolytic graphite (HOPG) substrates. Atomic force microscopy (AFM) and scanning electron microscopy (SEM) were used to study the presence and distinct contact of GO sheets on the substrates. It was revealed from the topography images that high-quality ultraflat GO monolayer sheets formed on the substrates without distinct cracking/wrinkling or folding. GO sheets with apparent height variation observed by microscopy also indicate ultraflat deposition with clear underlying steps. It was observed that ultrasonication and centrifuge steps prior to deposition were very effective for getting oxidation debris (OD)-free ultraflat single monolayer GO nanosheets onto substrates and that the process depends on the concentration of supplied GO solutions.

Assembled microcapsules by doxorubicin and polysaccharide as high effective anticancer drug carriers.

PubMed

Du, Cuiling; Zhao, Jie; Fei, Jinbo; Cui, Yue; Li, Junbai

2013-09-01

Doxorubicin, together with the modified polysaccharide (alginate dialdehyde), was used as a wall material to fabricate microcapsules through self-cross-linking by a template method. The microcapsules as-prepared are pH-responsive. Relevant scanning electronic microscopy, atom force microscopy and confocal laser scanning microscopy confirm the morphology of the uniform microcapsules. The spectroscopic results show that the microcapsules are assembled through electrostatic interaction and Schiff's base covalent bonding. Doxorubicin can be released sustainably from the capsules in buffer solution at a lower pH value. The cellular uptake of the microcapsules and drug release induced by acidic microenvironment are time-dependent processes. The cell cytotoxicity experiments in vitro demonstrate that the doxorubicin-based microcapsules have high efficiency to kill the cancer cells. Copyright © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Platinum replica electron microscopy: Imaging the cytoskeleton globally and locally.

PubMed

Svitkina, Tatyana M

2017-05-01

Structural studies reveal how smaller components of a system work together as a whole. However, combining high resolution of details with full coverage of the whole is challenging. In cell biology, light microscopy can image many cells in their entirety, but at a lower resolution, whereas electron microscopy affords very high resolution, but usually at the expense of the sample size and coverage. Structural analyses of the cytoskeleton are especially demanding, because cytoskeletal networks are unresolvable by light microscopy due to their density and intricacy, whereas their proper preservation is a challenge for electron microscopy. Platinum replica electron microscopy can uniquely bridge the gap between the "comfort zones" of light and electron microscopy by allowing high resolution imaging of the cytoskeleton throughout the entire cell and in many cells in the population. This review describes the principles and applications of platinum replica electron microscopy for studies of the cytoskeleton. Copyright © 2017 Elsevier Ltd. All rights reserved.

Platinum Replica Electron Microscopy: Imaging the Cytoskeleton Globally and Locally

PubMed Central

SVITKINA, Tatyana M.

2017-01-01

Structural studies reveal how smaller components of a system work together as a whole. However, combining high resolution of details with full coverage of the whole is challenging. In cell biology, light microscopy can image many cells in their entirety, but at a lower resolution, whereas electron microscopy affords very high resolution, but usually at the expense of the sample size and coverage. Structural analyses of the cytoskeleton are especially demanding, because cytoskeletal networks are unresolvable by light microscopy due to their density and intricacy, whereas their proper preservation is a challenge for electron microscopy. Platinum replica electron microscopy can uniquely bridge the gap between the “comfort zones” of light and electron microscopy by allowing high resolution imaging of the cytoskeleton throughout the entire cell and in many cells in the population. This review describes the principles and applications of platinum replica electron microscopy for studies of the cytoskeleton. PMID:28323208

Electrochemically Controlled Ion-exchange Property of Carbon Nanotubes/Polypyrrole Nanocomposite in Various Electrolyte Solutions

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

Choi, Daiwon; Zhu, Chengzhou; Fu, Shaofang

2016-09-15

The electrochemically controlled ion-exchange properties of multi-wall carbon nanotube (MWNT)/electronically conductive polypyrrole (PPy) polymer composite in the various electrolyte solutions have been investigated. The ion-exchange behavior, rate and capacity of the electrochemically deposited polypyrrole with and without carbon nanotube (CNT) were compared and characterized using cyclic voltammetry (CV), chronoamperometry (CA), electrochemical quartz crystal microbalance (EQCM), X-ray photoelectron spectroscopy (XPS) and scanning electron microscopy (SEM). It has been found that the presence of carbon nanotube backbone resulted in improvement in ion-exchange rate, stability of polypyrrole, and higher anion loading capacity per PPy due to higher surface area, electronic conductivity, porous structuremore » of thin film, and thinner film thickness providing shorter diffusion path. Chronoamperometric studies show that electrically switched anion exchange could be completed more than 10 times faster than pure PPy thin film. The anion selectivity of CNT/PPy film is demonstrated using X-ray photoelectron spectroscopy (XPS).« less

Permeability of Dental Adhesives – A SEM Assessment

PubMed Central

Malacarne-Zanon, Juliana; de Andrade e Silva, Safira M.; Wang, Linda; de Goes, Mario F.; Martins, Adriano Luis; Narvaes-Romani, Eliene O.; Anido-Anido, Andrea; Carrilho, Marcela R. O.

2010-01-01

Objectives: To morphologically evaluate the permeability of different commercial dental adhesives using scanning electron microscopy. Methods: Seven adhesive systems were evaluated: one three-step system (Scotchbond Multi-Purpose - MP); one two-step self-etching primer system (Clearfil SE Bond – SE); three two-step etch-and-rinse systems (Single Bond 2 – SB; Excite – EX; One-Step – OS); and two single-step self-etching adhesives (Adper Prompt – AP; One-Up Bond F – OU). The mixture of primer and bond agents of the Clearfil SE Bond system (SE-PB) was also tested. The adhesives were poured into a brass mold (5.8 mm x 0.8 mm) and light-cured for 80 s at 650 mW/cm2. After a 24 h desiccation process, the specimens were immersed in a 50% ammoniac silver nitrate solution for tracer permeation. Afterwards, they were sectioned in ultra-fine slices, carbon-coated, and analyzed under backscattered electrons in a scanning electron microscopy. Results: MP and SE showed slight and superficial tracer permeation. In EX, SB, and OS, permeation extended beyond the inner superficies of the specimens. SE-PB did not mix well, and most of the tracer was precipitated into the primer agent. In AP and OU, “water-trees” were observed all over the specimens. Conclusions: Different materials showed distinct permeability in aqueous solution. The extent of tracer permeation varied according to the composition of each material and it was more evident in the more hydrophilic and solvated ones. PMID:20922163

In vitro feasibility study of the use of a magnetic electrospun chitosan nanofiber composite for hyperthermia treatment of tumor cells.

PubMed

Lin, Ta-Chun; Lin, Feng-Huei; Lin, Jui-Che

2012-07-01

Hyperthermia has been reported to be an effective cancer treatment modality, as tumor cells are more temperature-sensitive than their normal counterparts. Since the ambient temperature can be increased by placing magnetic nanoparticles in an alternating magnetic field it has become of interest to incorporate these magnetic nanoparticles into biodegradable nanofibers for possible endoscopic hyperthermia treatment of malignant tumors. In this preliminary investigation we have explored various characteristics of biodegradable electrospun chitosan nanofibers containing magnetic nanoparticles prepared by different methods. These methods included: (1) E-CHS-Fe(3)O(4), with electrospun chitosan nanofibers directly immersed in a magnetic nanoparticle solution; (2) E-CHS-Fe(2+), with the electrospun chitosan nanofibers initially immersed in Fe(+2)/Fe(+3) solution, followed by chemical co-precipitation of the magnetic nanoparticles. The morphology and crystalline phase of the magnetic electrospun nanofiber matrices were determined by scanning electron microscopy, transmission electron microscopy, selected area electron diffraction, and X-ray diffraction spectroscopy. The magnetic characteristics were measured using a superconducting quantum interference device. The heating properties of these magnetic electrospun nanofiber matrices in an alternating magnetic field were investigated at a frequency of 750 kHz and magnetic intensity of 6.4 kW. In vitro cell incubation experiments indicated that these magnetic electrospun nanofiber matrices are non-cytotoxic and can effectively reduce tumor cell proliferation upon application of a magnetic field. Copyright © 2012 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

Polyethylene nano crystalsomes formed at a curved liquid/liquid interface.

PubMed

Wang, Wenda; Staub, Mark C; Zhou, Tian; Smith, Derrick M; Qi, Hao; Laird, Eric D; Cheng, Shan; Li, Christopher Y

2017-12-21

Crystallization is incommensurate with nanoscale curved space due to the lack of three dimensional translational symmetry of the latter. Herein, we report the formation of single-crystal-like, nanosized polyethylene (PE) capsules using a miniemulsion solution crystallization method. The miniemulsion was formed at elevated temperatures using PE organic solution as the oil phase and sodium dodecyl sulfate as the surfactant. Subsequently, cooling the system stepwisely for controlled crystallization led to the formation of hollow, nanosized PE crystalline capsules, which are named as crystalsomes since they mimic the classical self-assembled structures such as liposome, polymersome and colloidosome. We show that the formation of the nanosized PE crystalsomes is driven by controlled crystallization at the curved liquid/liquid interface of the miniemulson droplet. The morphology, structure and mechanical properties of the PE crystalsomes were characterized using scanning electron microscopy, transmission electron microscopy, X-ray diffraction, and atomic force spectroscopy. Electron diffraction showed the single-crystal-like nature of the crystalsomes. The incommensurateness between the nanocurved interface and the crystalline packing led to reduced crystallinity and crystallite size of the PE crystalsome, as observed from the X-ray diffraction measurements. Moreover, directly quenching the emulsion below the spinodal line led to the formation of hierarchical porous PE crystalsomes due to the coupling of the PE crystallization and liquid/liquid phase separation. We anticipate that this unique crystalsome represents a new type of nanostructure that might be used as nanodrug carriers and ultrasound contrast agents.

Highly active carbon supported ternary PdSnPtx (x=0.1-0.7) catalysts for ethanol electro-oxidation in alkaline and acid media.

PubMed

Wang, Xiaoguang; Zhu, Fuchun; He, Yongwei; Wang, Mei; Zhang, Zhonghua; Ma, Zizai; Li, Ruixue

2016-04-15

A series of trimetallic PdSnPtx (x=0.1-0.7)/C catalysts with varied Pt content have been synthesized by co-reduction method using NaBH4 as a reducing agent. These catalysts were characterized using X-ray diffraction (XRD), transmission electron microscopy (TEM), high resolution transmission electron microscopy (HRTEM), energy dispersive X-ray spectroscopy (EDX), X-ray photoelectron spectroscopy (XPS), cyclic voltammetry (CV) and chronoamperometry (CA). The electrochemical results show that, after adding a minor amount of Pt dopant, the resultant PdSnPtx/C demonstrated more superior catalytic performance toward ethanol oxidation as compared with that of mono-/bi-metallic Pd/C or PdSn/C in alkaline solution and the PdSnPt0.2/C with optimal molar ratio reached the best. In acid solution, the PdSnPt0.2/C also depicted a superior catalytic activity relative to the commercial Pt/C catalyst. The possible enhanced synergistic effect between Pd, Sn/Sn(O) and Pt in an alloyed state should be responsible for the as-revealed superior ethanol electro-oxidation performance based upon the beneficial electronic effect and bi-functional mechanism. It implies the trimetallic PdSnPt0.2/C with a low Pt content has a promising prospect as anodic electrocatalyst in fields of alkali- and acid-type direct ethanol fuel cells. Copyright © 2016 Elsevier Inc. All rights reserved.

Silver stain for electron microscopy

NASA Technical Reports Server (NTRS)

Corbett, R. L.

1972-01-01

Ammoniacal silver stain used for light microscopy was adapted advantageously for use with very thin biological sections required for electron microscopy. Silver stain can be performed in short time, has more contrast, and is especially useful for low power electron microscopy.

Increased resistance of contact lens related bacterial biofilms to antimicrobial activity of soft contact lens care solutions

PubMed Central

Szczotka-Flynn, Loretta B.; Imamura, Yoshifumi; Chandra, Jyotsna; Yu, Changping; Mukherjee, Pranab K.; Pearlman, Eric; Ghannoum, Mahmoud A.

2014-01-01

PURPOSE To determine if clinical and reference strains of Pseudomonas aeruginosa, Serratia marcescens, and Staphylococcus aureus form biofilms on silicone hydrogel contact lenses, and ascertain antimicrobial activities of contact lens care solutions. METHODS Clinical and American Type Culture Collection (ATCC) reference strains of Pseudomonas aeruginosa, Serratia marcescens, and Staphylococcus aureus were incubated with lotrafilcon A lenses under conditions that facilitate biofilm formation. Biofilms were quantified by quantitative culturing (colony forming units, CFUs), and gross morphology and architecture were evaluated using scanning electron microscopy (SEM) and confocal microscopy. Susceptibilities of the planktonic and biofilm growth phases of the bacteria to five common multipurpose contact lens care solutions and one hydrogen peroxide care solution were assessed. RESULTS P. aeruginosa, S. marcescens, and S. aureus reference and clinical strains formed biofilms on lotrafilcon A silicone hydrogel contact lenses, as dense networks of cells arranged in multiple layers with visible extracellular matrix. The biofilms were resistant to commonly used biguanide preserved multipurpose care solutions. P. aeruginosa and S. aureus biofilms were susceptible to a hydrogen peroxide and a polyquaternium preserved care solution, whereas S. marcescens biofilm was resistant to a polyquaternium preserved care solution but susceptible to hydrogen peroxide disinfection. In contrast, the planktonic forms were always susceptible. CONCLUSIONS P. aeruginosa, S. marcescens, and S. aureus form biofilms on lotrafilcon A contact lenses, which in contrast to planktonic cells, are resistant to the antimicrobial activity of several soft contact lens care products. PMID:19654521

Correlated Light and Electron Microscopy/Electron Tomography of Mitochondria In Situ

PubMed Central

Perkins, Guy A.; Sun, Mei G.; Frey, Terrence G.

2009-01-01

Three-dimensional light microscopy and three-dimensional electron microscopy (electron tomography) separately provide very powerful tools to study cellular structure and physiology, including the structure and physiology of mitochondria. Fluorescence microscopy allows one to study processes in live cells with specific labels and stains that follow the movement of labeled proteins and changes within cellular compartments but does not have sufficient resolution to define the ultrastructure of intracellular organelles such as mitochondria. Electron microscopy and electron tomography provide the highest resolution currently available to study mitochondrial ultrastructure but cannot follow processes in living cells. We describe the combination of these two techniques in which fluorescence confocal microscopy is used to study structural and physiologic changes in mitochondria within apoptotic HeLa cells to define the apoptotic timeframe. Cells can then be selected at various stages of the apoptotic timeframe for examination at higher resolution by electron microscopy and electron tomography. This is a form of “virtual” 4-dimensional electron microscopy that has revealed interesting structural changes in the mitochondria of HeLa cells during apoptosis. The same techniques can be applied, with modification, to study other dynamic processes within cells in other experimental contexts. PMID:19348881

ANALYTICAL CHEMISTRY DIVISION ANNUAL PROGRESS REPORT FOR PERIOD ENDING DECEMBER 31, 1961

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

None

1962-02-01

Research and development progress is reported on analytlcal instrumentation, dlssolver-solution analyses, special research problems, reactor projects analyses, x-ray and spectrochemical analyses, mass spectrometry, optical and electron microscopy, radiochemical analyses, nuclear analyses, inorganic preparations, organic preparations, ionic analyses, infrared spectral studies, anodization of sector coils for the Analog II Cyclotron, quality control, process analyses, and the Thermal Breeder Reactor Projects Analytical Chemistry Laboratory. (M.C.G.)

The 2017 Nobel Prize in Chemistry: cryo-EM comes of age.

PubMed

Shen, Peter S

2018-03-01

The 2017 Nobel Prize in Chemistry was awarded to Jacques Dubochet, Joachim Frank, and Richard Henderson for "developing cryo-electron microscopy (cryo-EM) for the high-resolution structure determination of biomolecules in solution." This feature article summarizes some of the major achievements leading to the development of cryo-EM and recent technological breakthroughs that have transformed the method into a mainstream tool for structure determination.

Cellulose Perversions

PubMed Central

Canejo, João P.; Godinho, Maria H.

2013-01-01

Cellulose micro/nano-fibers can be produced by electrospinning from liquid crystalline solutions. Scanning electron microscopy (SEM), as well as atomic force microscopy (AFM) and polarizing optical microscopy (POM) measurements showed that cellulose-based electrospun fibers can curl and twist, due to the presence of an off-core line defect disclination, which was present when the fibers were prepared. This permits the mimicking of the shapes found in many systems in the living world, e.g., the tendrils of climbing plants, three to four orders of magnitude larger. In this work, we address the mechanism that is behind the spirals’ and helices’ appearance by recording the trajectories of the fibers toward diverse electrospinning targets. The intrinsic curvature of the system occurs via asymmetric contraction of an internal disclination line, which generates different shrinkages of the material along the fiber. The completely different instabilities observed for isotropic and anisotropic electrospun solutions at the exit of the needle seem to corroborate the hypothesis that the intrinsic curvature of the material is acquired during liquid crystalline sample processing inside the needle. The existence of perversions, which joins left and right helices, is also investigated by using suspended, as well as flat, targets. Possible routes of application inspired from the living world are addressed. PMID:28809215

Precursor-controlled synthesis of hierarchical ZnO nanostructures, using oligoaniline-coated Au nanoparticle seeds

NASA Astrophysics Data System (ADS)

Krishnan, Deepti; Pradeep, T.

2009-07-01

Shape-selected synthesis of a large number of zinc oxide (ZnO) nano- and microstructures was achieved by the seed-mediated growth of oligoaniline-coated gold nanoparticle precursors. Distinctive ZnO structures such as nanoplates, nanospheres, microstars, microflowers, microthorns and micromultipods were synthesized by this method. Slightly different shapes were obtained in the absence of the seed solution. This is a fast, low temperature (60 °C) and biomimetic route to make a wide variety of structures. The structure and morphology of the nanostructures were studied by transmission electron microscopy (TEM) and scanning electron microscopy (SEM), respectively. Raman spectroscopy, Fourier-transform infrared (FTIR) spectroscopy and X-ray diffraction (XRD) were utilized for the characterization of the nanostructures. A growth mechanism for these nanostructures was proposed based on these results. The concentrations of the reacting species were the main parameter causing the changes in the morphologies. The variation in morphologies of these structures is believed to be due to the ability of the seed solution as well as polyvinylpyrrolidone (PVP) to selectively suppress/depress the growth of certain planes, allowing growth to occur only in certain specific directions. Changes in the amount of growth nuclei with varying sodium hydroxide (NaOH) concentration is also seen to affect the morphology of these structures.

Synthesis of length-controlled aerosol carbon nanotubes and their dispersion stability in aqueous solution.

PubMed

Moon, Young Kyun; Lee, Jaebeom; Lee, Jae Keun; Kim, Tae Kyu; Kim, Soo H

2009-02-03

A one-step method combining spray pyrolysis and thermal chemical vapor deposition (CVD) processes was developed to grow hybrid carbon nanotube (CNT)-bimetallic composite particles. Nickel, aluminum, and acetylene were used as the catalytic site, noncatalytic matrix, and hydrocarbon source, respectively. The bimetallic particles (i.e., Al-Ni) were spray pyrolized and subsequently passed through thermal CVD. During the thermal CVD, the catalytic decomposition of acetylene occurred on the free-floating bimetallic particles so that sea urchin-like CNTs were radially grown. Scanning electron microscopy (SEM) and transmission electron microscopy (TEM) analyses revealed the CNTs to have a uniform diameter of approximately 10 +/- 2 nm. The length of the CNTs was controlled by varying the residence time of the bimetallic nanoparticles with a length of 200-1000 nm. After nitric acid treatment, the CNTs were released by melting the bimetallic particles. The resulting CNTs were then dispersed in an aqueous solution to examine the effect of the length of CNTs on their dispersion stability, which is a critical issue for the stability and repeatability of the heat transfer performance in nanofluids. Ultraviolet-visible (UV-vis) spectrometer analysis showed that shorter CNTs were less stable than the longer CNTs due to the higher mobility-induced agglomeration of the shorter CNTs.

Magnetic cobalt ferrite composite as an efficient catalyst for photocatalytic oxidation of carbamazepine.

PubMed

He, Yongzhen; Dai, Chaomeng; Zhou, Xuefei

2017-01-01

A magnetic spinel cobalt ferrite nanoparticle composite (CFO) was prepared via an ultrasonication-assisted co-precipitation method. The morphological structure and surface composition of CFO before and after reaction were investigated by using X-ray diffraction, scanning electron microscopy, transmission electron microscopy, energy dispersive X-ray, and Fourier transform infrared spectroscopy, indicating the consumption of iron oxide during photodegradation. X-ray photoelectron spectroscopy and vibrating sample magnetometry confirm the preparation of the ferrite nanoparticle composite and its magnetic properties. The prepared CFO was then used for the photocatalytic degradation of carbamazepine (CBZ) as an example of pharmaceuticals and personal care products (PPCPs) from aqueous solution. The effects of the nanocomposite dosage, contact time, and solution pH on the photodegradation process were investigated. More than 96% of the CBZ was degraded within 100 min at 0.2 g·L -1 CFO in the presence of UV light. The reactive species for CBZ degradation in the CFO/UV system was identified as hydroxyl radicals by the methanol scavenging method. Combined with the detection of leached iron ions during the process, the CBZ degradation mechanism can be presumed to be heterogeneous and homogeneous photocatalytic degradation in the CFO/UV system. Furthermore, iminostilbene and acridine were detected as intermediate products by GC-MS.

Polymer mediated layer-by-layer assembly of different shaped gold nanoparticles.

PubMed

Budy, Stephen M; Hamilton, Desmond J; Cai, Yuheng; Knowles, Michelle K; Reed, Scott M

2017-02-01

Gold nanoparticles (GNPs) have a wide range of properties with potential applications in electronics, optics, catalysis, and sensing. In order to demonstrate that dense, stable, and portable samples could be created for these applications, multiple layers of GNPs were assembled via drop casting on glass substrates by layer-by-layer (LBL) techniques. Two cationic polyelectrolytes, poly(diallyldimethylammonium chloride) and polyethyleneimine, one anionic polyelectrolyte, poly(sodium 4-styrene sulfonate), and one neutral polymer, polyvinylpyrrolidone, were combined with four different shapes of GNPs (spherical, rod, triangular prismatic, and octahedral) to prepare thin films. A subset of these polymer nanoparticle combinations were assembled into thin films. Synthesized GNPs were characterized via dynamic light scattering, UV-vis spectroscopy, and transmission electron microscopy and the LBL thin films were characterized using UV-vis spectroscopy and atomic force microscopy. Sensing applications of the nanoparticles in solution and thin films were tested by monitoring the localized surface plasmon resonance of the GNPs. LBL thin films were prepared ranging from 25 to 100 layers with optical densities at plasmon from 0.5 to 3.0. Sensitivity in solutions ranged from 14 to 1002nm/refractive index units (RIU) and films ranged from 18.8 to 135.1nm/RIU suggesting reduced access to the GNPs within the films. Copyright © 2016 Elsevier Inc. All rights reserved.

Glutaraldehyde-induced remineralization improves the mechanical properties and biostability of dentin collagen.

PubMed

Chen, Chaoqun; Mao, Caiyun; Sun, Jian; Chen, Yi; Wang, Wei; Pan, Haihua; Tang, Ruikang; Gu, Xinhua

2016-10-01

The purpose of this study was to induce a biomimetic remineralization process by using glutaraldehyde (GA) to reconstruct the mechanical properties and biostability of demineralized collagen. Demineralized dentin disks (35% phosphoric acid, 10s) were pretreated with a 5% GA solution for 3min and then cultivated in a calcium phosphate remineralization solution. The remineralization kinetics and superstructure of the remineralization layer were evaluated by Raman spectroscopy, transmission electron microscopy, scanning electron microscopy and nanoindentation tests. The biostability was examined by enzymatic degradation experiments. A significant difference was found in dentin remineralization process between dentin with and without GA pretreating. GA showed a specific affinity to dentin collagen resulting in the formation of a cross-linking superstructure. GA pretreating could remarkably shorten remineralization time from 7days to 2days. The GA-induced remineralized collagen fibrils were well encapsulated by newly formed hydroxyapatite mineral nanocrystals. With the nano-hydroxyapatite coating, both the mechanical properties (elastic modulus and hardness) and the biostability against enzymatic degradation of the collagen were significantly enhanced, matching those of natural dentin. The results indicated that GA cross-linking of dentin collagen could promote dentin biomimetic remineralization, resulting in an improved mechanical properties and biostability. It may provide a promising tissue-engineering technology for dentin repair. Copyright © 2016 Elsevier B.V. All rights reserved.

Thermo-reversible supramolecular hydrogels of trehalose-type diblock methylcellulose analogues.

PubMed

Yamagami, Mao; Kamitakahara, Hiroshi; Yoshinaga, Arata; Takano, Toshiyuki

2018-03-01

This paper describes the design and synthesis of new trehalose-type diblock methylcellulose analogues with nonionic, cationic, and anionic cellobiosyl segments, namely 1-(tri-O-methyl-cellulosyl)-4-[β-d-glucopyranosyl-(1→4)-β-d-glucopyranosyloxymethyl]-1H-1,2,3-triazole (1), 1-(tri-O-methyl-cellulosyl)-4-[(6-amino-6-deoxy-β-d-glucopyranosyl)-(1→4)- 6-amino-6-deoxy-β-d-glucopyranosyloxymethyl]-1H-1,2,3-triazole (2), and 4-(tri-O-methyl-cellulosyloxymethyl)-1-[β-d-glucopyranuronosyl-(1→4)-β-d-glucopyranuronosyl]-1H-1,2,3-triazole (3), respectively. Aqueous solutions of all of the 1,2,3-triazole-linked diblock methylcellulose analogues possessed higher surface activities than that of industrially produced methylcellulose and exhibited lower critical solution temperatures, that allowed the formation of thermoresponsive supramolecular hydrogels at close to human body temperature. Supramolecular structures of thermo-reversible hydrogels based on compounds 1, 2, and 3 were investigated by means of scanning electron microscopy (SEM) and transmission electron microscopy (TEM). Detailed structure-property-function relationships of compounds 1, 2, and 3 were discussed. Not only nonionic hydrophilic segment but also ionic hydrophilic segments of diblock methylcellulose analogues were valid for the formation of thermo-reversible supramolecular hydrogels based on end-functionalized methylcellulose. Copyright © 2017 Elsevier Ltd. All rights reserved.

Novel synthesis of ZnO/PMMA nanocomposites for photocatalytic applications

PubMed Central

Di Mauro, Alessandro; Cantarella, Maria; Nicotra, Giuseppe; Pellegrino, Giovanna; Gulino, Antonino; Brundo, Maria Violetta; Privitera, Vittorio; Impellizzeri, Giuliana

2017-01-01

The incorporation of nanostructured photocatalysts in polymers is a strategic way to obtain novel water purification systems. This approach takes the advantages of: (1) the presence of nanostructured photocatalyst; (2) the flexibility of polymer; (3) the immobilization of photocatalyst, that avoids the recovery of the nanoparticles after the water treatment. Here we present ZnO-polymer nanocomposites with high photocatalytic performance and stability. Poly (methyl methacrylate) (PMMA) powders were coated with a thin layer of ZnO (80 nm thick) by atomic layer deposition at low temperature (80 °C). Then the method of sonication and solution casting was performed so to obtain the ZnO/PMMA nanocomposites. A complete morphological, structural, and chemical characterization was made by scanning electron microscopy (SEM), transmission electron microscopy (TEM), energy-dispersive X-ray spectroscopy (EDS), X-ray diffraction (XRD), and X-ray photoelectron spectroscopy (XPS) analyses. The remarkable photocatalytic efficiency of the nanocomposites was demonstrated by the degradation of methylene blue (MB) dye and phenol in aqueous solution under UV light irradiation. The composites also resulted reusable and stable, since they maintained an unmodified photo-activity after several MB discoloration runs. Thus, these results demonstrate that the proposed ZnO/PMMA nanocomposite is a promising candidate for photocatalytic applications and, in particular, for novel water treatment. PMID:28098229

Detection of abnormal extracellular matrix in the interstitium of regenerating renal tubules.

PubMed

Minuth, Will W; Denk, Lucia

2014-12-15

Stem/progenitor cells are promising candidates for the regeneration of parenchyma in acute and chronic renal failure. However, recent data exhibit that survival of stem/progenitor cells after implantation in diseased renal parenchyma is restricted. To elaborate basic parameters improving survival, cell seeding was simulated under advanced in vitro conditions. After isolation, renal stem/progenitor cells were mounted in a polyester interstitium for perfusion culture. During generation of tubules, chemically defined CO2 Independent Medium or Leibovitz's L-15 Medium was applied. Specimens were then fixed for transmission electron microscopy to analyze morphological features in generated tubules. Fixation in conventional glutaraldehyde (GA) solution shows development of tubules each exhibiting a polarized epithelium, an intact basal lamina and an inconspicuous interstitium. In contrast, special fixation of specimens in GA solution containing cupromeronic blue, ruthenium red or tannic acid unveils previously not visible extracellular matrix. Control experiments elucidate that a comparable extracellular matrix is not present in the interstitium of the matured kidney. Thus, generation of renal tubules in combination with advanced fixation of specimens for electron microscopy demonstrates that development of abnormal features in the newly developed interstitium has to be considered, when repair of renal parenchyma is performed by implantation of stem/progenitor cells.

Modeling and prediction of copper removal from aqueous solutions by nZVI/rGO magnetic nanocomposites using ANN-GA and ANN-PSO.

PubMed

Fan, Mingyi; Hu, Jiwei; Cao, Rensheng; Xiong, Kangning; Wei, Xionghui

2017-12-21

Reduced graphene oxide-supported nanoscale zero-valent iron (nZVI/rGO) magnetic nanocomposites were prepared and then applied in the Cu(II) removal from aqueous solutions. Scanning electron microscopy, transmission electron microscopy, X-ray photoelectron spectroscopy and superconduction quantum interference device magnetometer were performed to characterize the nZVI/rGO nanocomposites. In order to reduce the number of experiments and the economic cost, response surface methodology (RSM) combined with artificial intelligence (AI) techniques, such as artificial neural network (ANN), genetic algorithm (GA) and particle swarm optimization (PSO), has been utilized as a major tool that can model and optimize the removal processes, because a tremendous advance has recently been made on AI that may result in extensive applications. Based on RSM, ANN-GA and ANN-PSO were employed to model the Cu(II) removal process and optimize the operating parameters, e.g., operating temperature, initial pH, initial concentration and contact time. The ANN-PSO model was proven to be an effective tool for modeling and optimizing the Cu(II) removal with a low absolute error and a high removal efficiency. Furthermore, the isotherm, kinetic, thermodynamic studies and the XPS analysis were performed to explore the mechanisms of Cu(II) removal process.

Microhardness variation and related microstructure in Al-Cu alloys prepared by HF induction melting and RF sputtering

NASA Astrophysics Data System (ADS)

Boukhris, N.; Lallouche, S.; Debili, M. Y.; Draissia, M.

2009-03-01

The materials under consideration are binary aluminium-copper alloys (10 at% to 90.3 at%Cu) produced by HF melting and RF magnetron sputtering. The resulting micro structures have been observed by standard metallographic techniques, X-ray powder diffraction, scanning electron microscopy and transmission electron microscopy. Vickers microhardness of bulk Al-Cu alloys reaches a maximum of 1800 MPa at 70.16 at%Cu. An unexpected metastable θ ' phase has been observed within aluminium grain in Al-37 at%Cu. The mechanical properties of a family of homogeneous Al{1-x}Cu{x} (0 < x < 0.92) thin films made by radiofrequency (13.56 MHz) cathodic magnetron sputtering from composite Al-Cu targets have been investigated. The as-deposited microstructures for all film compositions consisted of a mixture of the two expected face-centred-cubic (fcc) Al solid solution and tetragonal θ (Al{2}Cu) phases. The microhardness regularly increases and the grain size decreases both with copper concentration. This phenomenon of significant mechanical strengthening of aluminium by means of copper is essentially due to a combination between solid solution effects and grain size refinement. This paper reports some structural features of different Al-Cu alloys prepared by HF melting and RF magnetron on glass substrate sputtering.

Preparation and Characterization of Polyhydroxybutyrate/Polycaprolactone Nanocomposites

PubMed Central

Liau, Cha Ping; Bin Ahmad, Mansor; Shameli, Kamyar; Yunus, Wan Md Zin Wan

2014-01-01

Polyhydroxybutyrate (PHB)/polycaprolactone (PCL)/stearate Mg-Al layered double hydroxide (LDH) nanocomposites were prepared via solution casting intercalation method. Coprecipitation method was used to prepare the anionic clay Mg-Al LDH from nitrate salt solution. Modification of nitrate anions by stearate anions between the LDH layers via ion exchange reaction. FTIR spectra showed the presence of carboxylic acid (COOH) group which indicates that stearate anions were successfully intercalated into the Mg-Al LDH. The formation of nanocomposites only involves physical interaction as there are no new functional groups or new bonding formed. X-ray diffraction (XRD) and transmission electron microscopy (TEM) indicated that the mixtures of nanocomposites are intercalated and exfoliated types. XRD results showed increasing of basal spacing from 8.66 to 32.97 Å in modified stearate Mg-Al LDH, and TEM results revealed that the stearate Mg-Al LDH layers are homogeneously distributed in the PHB/PCL polymer blends matrix. Enhancement in 300% elongation at break and 66% tensile strength in the presence of 1.0 wt % of the stearate Mg-Al LDH as compare with PHB/PCL blends. Scanning electron microscopy (SEM) proved that clay improves compatibility between polymer matrix and the best ratio 80PHB/20PCL/1stearate Mg-Al LDH surface is well dispersed and stretched before it breaks. PMID:24600329

Preservation of human ovarian follicles within tissue frozen by vitrification in a xeno-free closed system using only ethylene glycol as a permeating cryoprotectant.

PubMed

Sheikhi, Mona; Hultenby, Kjell; Niklasson, Boel; Lundqvist, Monalill; Hovatta, Outi

2013-07-01

To study the preservation of follicles within ovarian tissue vitrified using only one or a combination of three permeating cryoprotectants. Experimental study. University hospital. Ovarian tissue was donated by consenting women undergoing elective cesarean section. Ovarian tissue was vitrified in closed sealed vials using either a combination of dimethyl sulfoxide, 1,2-propanediol, and ethylene glycol (EG), or only EG as permeating cryoprotectants. Ovarian tissue was vitrified with the use of two vitrification methods. Tissue from the same donor was used for comparison of two different solutions. The morphology of the follicles was evaluated after vitrification, warming, and culture by light microscopy and transmission electron microscopy. Apoptosis was assessed by immunohistochemistry for active caspase-3 in fresh and vitrified tissue. Light and electron microscopic analysis showed equally well preserved morphology of oocytes, granulosa cells, and ovarian stroma when either of the vitrification solutions was used. No apoptosis was observed in primordial and primary follicles. Using only EG as a permeating cryoprotectant in a closed tube gives as good ultrastructural preservation of ovarian follicles as a more complicated system using several cryoprotectants. Copyright © 2013 American Society for Reproductive Medicine. Published by Elsevier Inc. All rights reserved.

Ultra-fine grained microstructure of metastable beta Ti-15Mo alloy and its effects on the phase transformations

NASA Astrophysics Data System (ADS)

Václavová, K.; Stráský, J.; Zháňal, P.; Veselý, J.; Polyakova, V.; Semenova, I.; Janeček, M.

2017-05-01

Processing of metastable titanium alloys by severe plastic deformation provides an opportunity to achieve exceptional grain refinement, to enhance the strength and to affect phase transformations occurring during thermal treatment. The main aim of this study is to investigate the microstructure of ultra-fine grained (UFG) material and effect of microstructural changes on phase transformations in metastable β-Ti alloy Ti-15Mo. Metastable β-Ti alloys are currently the most studied Ti-based materials with prospective use in medicine. Ti-15Mo alloy after solution treatment contains metastable β-phase. Metastable ω-phase and stable α-phase particles are formed upon annealing,. Solution treated Ti-15Mo alloy was deformed by high pressure torsion (HPT) at room temperature. Severely deformed structure after HPT with grain size of ~200 nm was studied by transmission electron microscopy. In-situ electrical resistance measurements showed significant changes in undergoing phase transformations when compared to coarse-grained (CG) material. Scanning electron microscopy revealed heterogeneous precipitation of α-particles at grain boundaries (GB). Due to the high density of GBs in UFG structure, these precipitates are very fine and equiaxed. The study demonstrates that SPD is capable of enhancing mechanical properties due to grain refinement and via affecting precipitation processes in metastable β-Ti alloys.

Dual function of EDTA with silver nanoparticles for root canal treatment-A novel modification.

PubMed

Martinez-Andrade, Juan M; Avalos-Borja, Miguel; Vilchis-Nestor, Alfredo R; Sanchez-Vargas, Luis O; Castro-Longoria, Ernestina

2018-01-01

The chelating and antimicrobial capacity of a novel modification of 17% EDTA with silver nanoparticles (AgNPs) (EDTA-AgNPs) was evaluated in-vitro for root canal treatment (RCT). The EDTA-AgNPs solution was characterized by UV-Vis spectroscopy, ζ-potential and high-resolution transmission electron microscopy (HRTEM). Antimicrobial capacity was evaluated against Candida albicans and Staphylococcus aureus in planktonic and biofilm cells by broth macrodilution (24 h) and XTT assays, (1, 10 and 30 min) respectively. The chelating capacity of EDTA-AgNPs was assessed indirectly (smear layer removal) and directly (demineralizing effect) in bovine dentin at two silver concentrations, 16 and 512 μg/ml at 1 and 10 minutes of exposure time. Smear layer removal was evaluated by atomic force microscopy (AFM) and scanning electron microscopy (SEM). The demineralizing effect was determined by atomic absorption spectroscopy (AAS), microhardness test (MH) and X-ray diffractometer (XRD). Synthesized AgNPs were quasi-spherical in shape with an average size of 13.09 ± 8.05 nm. 17% EDTA-AgNPs was effective to inhibit C. albicans and S. aureus in planktonic and biofilm cultures. The smear layer removal and demineralizing effect were similar between 17% EDTA-AgNPs and 17% EDTA treatments. The 17% EDTA-AgNPs solution proved to be an effective antimicrobial agent, and has a similar chelating capacity to 17% EDTA alone. These in-vitro studies strongly suggest that EDTA-AgNPs could be used for effective smear layer removal, having an antimicrobial effect at the same time during RCT.

Dual function of EDTA with silver nanoparticles for root canal treatment–A novel modification

PubMed Central

Martinez-Andrade, Juan M.; Avalos-Borja, Miguel; Vilchis-Nestor, Alfredo R.; Sanchez-Vargas, Luis O.

2018-01-01

The chelating and antimicrobial capacity of a novel modification of 17% EDTA with silver nanoparticles (AgNPs) (EDTA-AgNPs) was evaluated in-vitro for root canal treatment (RCT). The EDTA-AgNPs solution was characterized by UV-Vis spectroscopy, ζ-potential and high-resolution transmission electron microscopy (HRTEM). Antimicrobial capacity was evaluated against Candida albicans and Staphylococcus aureus in planktonic and biofilm cells by broth macrodilution (24 h) and XTT assays, (1, 10 and 30 min) respectively. The chelating capacity of EDTA-AgNPs was assessed indirectly (smear layer removal) and directly (demineralizing effect) in bovine dentin at two silver concentrations, 16 and 512 μg/ml at 1 and 10 minutes of exposure time. Smear layer removal was evaluated by atomic force microscopy (AFM) and scanning electron microscopy (SEM). The demineralizing effect was determined by atomic absorption spectroscopy (AAS), microhardness test (MH) and X-ray diffractometer (XRD). Synthesized AgNPs were quasi-spherical in shape with an average size of 13.09 ± 8.05 nm. 17% EDTA-AgNPs was effective to inhibit C. albicans and S. aureus in planktonic and biofilm cultures. The smear layer removal and demineralizing effect were similar between 17% EDTA-AgNPs and 17% EDTA treatments. The 17% EDTA-AgNPs solution proved to be an effective antimicrobial agent, and has a similar chelating capacity to 17% EDTA alone. These in-vitro studies strongly suggest that EDTA-AgNPs could be used for effective smear layer removal, having an antimicrobial effect at the same time during RCT. PMID:29346398

A new solution chemical method to make low dimensional thermoelectric materials

NASA Astrophysics Data System (ADS)

Ding, Zhongfen

2001-11-01

Bismuth telluride and its alloys are currently the best thermoelectric materials known at room temperature and are therefore used for portable solid-state refrigeration. If the thermal electric figure of merit ZT could be improved by a factor of about 3, quiet and rugged solid-state devices could eventually replace conventional compressor based cooling systems. In order to test a theory that improved one-dimensional or two-dimensional materials could enhance ZT due to lower thermal conductivity, we are developing solution processing methods to make low dimensional materials. Bismuth telluride and its p-type and n-type alloys have layered structures consisting of 5 atom thick Te-Bi-Te-Bi-Te sheets, each sheet about 10 A thick. Lithium ions are intercalated into the layered materials using liquid ammonia. The lithium-intercalated materials are then exfoliated in water to form colloidal suspensions with narrow particle size distributions and are stable for more than 24 hours. The layers are then deposited on substrates, which after annealing at low temperatures, form highly c-axis oriented thin films. The exfoliated layers can potentially be restacked with other ions or layered materials in between the sheets to form novel structures. The restacked layers when treated with nitric acid and sonication form high yield nanorod structured materials. This new intercalation and exfoliation followed by sonication method could potentially be used for many other layered materials to make nanorod structured materials. The low dimensional materials are characterized by powder X-ray diffraction, atomic force microscopy (AFM), transmission electron microscopy (TEM), scanning electron microscopy (SEM), inductively coupled plasma (ICP) and dynamic light scattering.

Graphene-enabled electron microscopy and correlated super-resolution microscopy of wet cells.

PubMed

Wojcik, Michal; Hauser, Margaret; Li, Wan; Moon, Seonah; Xu, Ke

2015-06-11

The application of electron microscopy to hydrated biological samples has been limited by high-vacuum operating conditions. Traditional methods utilize harsh and laborious sample dehydration procedures, often leading to structural artefacts and creating difficulties for correlating results with high-resolution fluorescence microscopy. Here, we utilize graphene, a single-atom-thick carbon meshwork, as the thinnest possible impermeable and conductive membrane to protect animal cells from vacuum, thus enabling high-resolution electron microscopy of wet and untreated whole cells with exceptional ease. Our approach further allows for facile correlative super-resolution and electron microscopy of wet cells directly on the culturing substrate. In particular, individual cytoskeletal actin filaments are resolved in hydrated samples through electron microscopy and well correlated with super-resolution results.

Effect of SiO2, PVA and glycerol concentrations on chemical and mechanical properties of alginate-based films.

PubMed

Yang, Manli; Shi, Jinsheng; Xia, Yanzhi

2018-02-01

Sodium alginate (SA)/polyvinyl alcohol (PVA)/SiO 2 nanocomposite films were prepared by in situ polymerization through solution casting and solvent evaporation. The effect of different SA/PVA ratios, SiO 2 , and glycerol content on the mechanical properties, water content, water solubility, and water vapor permeability were studied. The nanocomposite films were characterized by Fourier transform infrared, X-ray diffraction, scanning electron microscopy, transmission electron microscopy, and thermal stability (thermogravimetric analysis/differential thermogravimetry) analyses. The nanocomposites showed the highest values of mechanical properties, such as SA/PVA ratio, SiO 2 , and glycerol content was 7:3, 6wt.%, and 0.25g/g SA, respectively. The tensile strength and elongation at break (E%) of the nanocomposites increased by 525.7% and 90.7%, respectively, compared with those of the pure alginate film. The Fourier transform infrared spectra showed a new SiOC band formed in the SA/PVA/SiO 2 nanocomposite film. The scanning electron microscopy image revealed good adhesion between SiO 2 and SA/PVA matrix. After the incorporation of PVA and SiO 2 , the water resistance of the SA/PVA/SiO 2 nanocomposite film was markedly improved. Transparency decreased with increasing PVA content but was enhanced by adding SiO 2 . Copyright © 2017. Published by Elsevier B.V.

Surface modification of cellulose acetate membrane using thermal annealing to enhance produced water treatment

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

Kusworo, T. D., E-mail: tdkusworo@che.undip.ac.id; Aryanti, N., E-mail: nita.aryanti@gmail.com; Firdaus, M. M. H.

2015-12-29

This study is performed primarily to investigate the effect of surface modification of cellulose acetate using thermal annealing on the enhancement of membrane performance for produced water treatment. In this study, Cellulose Acetate membranes were casted using dry/wet phase inversion technique. The effect of additive and post-treatment using thermal annealing on the membrane surface were examined for produced water treatment. Therma annealing was subjected to membrane surface at 60 and 70 °C for 5, 10 and 15 second, respectively. Membrane characterizations were done using membrane flux and rejection with produced water as a feed, Scanning Electron Microscopy (SEM) and Fouriermore » Transform Infra Red (FTIR) analysis. Experimental results showed that asymmetric cellulose acetate membrane can be made by dry/wet phase inversion technique. The results from the Scanning Electron Microscopy (FESEM) analysis was also confirmed that polyethylene glycol as additivie in dope solution and thermal annealing was affected the morphology and membrane performance for produced water treatment, respectively. Scanning electron microscopy micrographs showed that the selective layer and the substructure of membrane became denser and more compact after the thermal annealing processes. Therefore, membrane rejection was significantly increased while the flux was slighty decreased, respectively. The best membrane performance is obtained on the composition of 18 wt % cellulose acetate, poly ethylene glycol 5 wt% with thermal annealing at 70° C for 15 second.« less

Organic-inorganic random copolymers from methacrylate-terminated poly(ethylene oxide) with 3-methacryloxypropylheptaphenyl polyhedral oligomeric silsesquioxane: synthesis via RAFT polymerization and self-assembly behavior.

PubMed

Wei, Kun; Li, Lei; Zheng, Sixun; Wang, Ge; Liang, Qi

2014-01-14

In this contribution, we report the synthesis of organic-inorganic random polymers from methacrylate-terminated poly(ethylene oxide) (MAPEO) (Mn = 950) and 3-methacryloxypropylheptaphenyl polyhedral oligomeric silsesquioxane (MAPOSS) macromers via reversible addition-fragmentation chain transfer (RAFT) polymerization with 4-cyano-4-(thiobenzoylthio) valeric acid (CTBTVA) as the chain transfer agent. The organic-inorganic random copolymers were characterized by means of (1)H NMR spectroscopy, gel permeation chromatography (GPC) and differential scanning calorimetry (DSC). The results of GPC indicate that the polymerizations were carried out in a controlled fashion. Transmission electron microscopy (TEM) showed that the organic-inorganic random copolymers in bulk were microphase-separated and the POSS microdomains were formed via POSS-POSS interactions. In aqueous solutions the organic-inorganic random copolymers were capable of self-assembling into spherical nanoobjects as evidenced by transmission electron microscopy (TEM) and dynamic laser scattering (DLS). The self-assembly behavior of the organic-inorganic random copolymers was also found to occur in the mixtures with the precursors of epoxy. The nanostructures were further fixed via subsequent curing reaction and thus the organic-inorganic nanocomposites were obtained. The formation of nanophases in epoxy thermosets was confirmed by transmission electron microscopy (TEM) and dynamic mechanical thermal analysis (DMTA). The organic-inorganic nanocomposites displayed the enhanced surface hydrophobicity as evidenced by surface contact angle measurements.

Combined frequency modulated atomic force microscopy and scanning tunneling microscopy detection for multi-tip scanning probe microscopy applications

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

Morawski, Ireneusz; Institute of Experimental Physics, University of Wrocław, pl. M. Borna 9, 50-204 Wrocław; Spiegelberg, Richard

A method which allows scanning tunneling microscopy (STM) tip biasing independent of the sample bias during frequency modulated atomic force microscopy (AFM) operation is presented. The AFM sensor is supplied by an electronic circuit combining both a frequency shift signal and a tunneling current signal by means of an inductive coupling. This solution enables a control of the tip potential independent of the sample potential. Individual tip biasing is specifically important in order to implement multi-tip STM/AFM applications. An extensional quartz sensor (needle sensor) with a conductive tip is applied to record simultaneously topography and conductivity of the sample. Themore » high resonance frequency of the needle sensor (1 MHz) allows scanning of a large area of the surface being investigated in a reasonably short time. A recipe for the amplitude calibration which is based only on the frequency shift signal and does not require the tip being in contact is presented. Additionally, we show spectral measurements of the mechanical vibration noise of the scanning system used in the investigations.« less

Scanning electron microscopic and X-ray micro analysis on tooth enamel exposed to alkaline agents.

PubMed

Taubee, Fabian; Steiniger, Frank; Nietzsche, Sandor; Norén, Jörgen G

2010-01-01

The background of this study comprises two clinical cases, where patients exposed to aerosols of an alkaline and surface active cleaning agent developed loss of enamel substance on their teeth, further resulting in loss of teeth and partially destroyed soft tissues. The alkaline cleaning agent consisted of potassium hydroxide and various surfactants. The purpose of this study was to investigate possible changes in morphology and composition in human teeth enamel exposed to alkaline solutions, by means of X-ray micro analysis (XRMA), FTIR-spectroscopic analyses and scanning electron microscopy (SEM). Extracted premolars, exposed to potassium hydroxide solutions and alkaline cleaning solution,were analyzed by means of XRMA and SEM. Enamel powder, exposed to cleaning solution, was analyzed by means of FTIR. The SEM analysis revealed an increased porosity of the enamel surface and partially loss of enamel substance after exposure to alkaline solutions. The XRMA analyses revealed a decrease in carbon concentration while phosphorous and calcium showed no marked changes. The FTIR analyses showed no significant changes in peak heights or peak positions for phosphate, carbonate or hydroxide. It was concluded that human teeth enamel exposed to alkaline solutions showed loss of organic substance, marked pores in enamel surface and loss of substance in the enamel surface.

Morphology and structure of polymer layers protecting dental enamel against erosion.

PubMed

Beyer, Markus; Reichert, Jörg; Sigusch, Bernd W; Watts, David C; Jandt, Klaus D

2012-10-01

Human dental erosion caused by acids is a major factor for tooth decay. Adding polymers to acidic soft drinks is one important approach to reduce human dental erosion caused by acids. The aim of this study was to investigate the thickness and the structure of polymer layers adsorbed in vitro on human dental enamel from polymer modified citric acid solutions. The polymers propylene glycol alginate (PGA), highly esterified pectin (HP) and gum arabic (GA) were used to prepare polymer modified citric acids solutions (PMCAS, pH 3.3). With these PMCAS, enamel samples were treated for 30, 60 and 120s respectively to deposit polymer layers on the enamel surface. Profilometer scratches on the enamel surface were used to estimate the thickness of the polymer layers via atomic force microscopy (AFM). The composition of the deposited polymer layers was investigated with X-ray photoelectron spectroscopy (XPS). In addition the polymer-enamel interaction was investigated with zeta-potential measurements and scanning electron microscopy (SEM). It has been shown that the profilometer scratch depth on the enamel with deposited polymers was in the range of 10nm (30s treatment time) up to 25nm (120s treatment time). Compared to this, the unmodified CAS-treated surface showed a greater scratch depth: from nearly 30nm (30s treatment time) up to 60nm (120s treatment time). Based on XPS measurements, scanning electron microscopy (SEM) and zeta-potential measurements, a model was hypothesized which describes the layer deposited on the enamel surface as consisting of two opposing gradients of polymer molecules and hydroxyapatite (HA) particles. In this study, the structure and composition of polymer layers deposited on in vitro dental enamel during treatment with polymer modified citric acid solutions were investigated. Observations are consistent with a layer consisting of two opposing gradients of hydroxyapatite particles and polymer molecules. This leads to reduced erosive effects of citric acid solutions on dental enamel surfaces. Copyright © 2012 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Size and surface effects on the magnetism of magnetite and maghemite nanoparticles

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

Nikiforov, V. N., E-mail: pppnvn@yandex.ru; Ignatenko, A. N.; Irkhin, V. Yu.

2017-02-15

The size effects of magnetite and maghemite nanoparticles on their magnetic properties (magnetic moment, Curie temperature, blocking temperature, etc.) have been investigated. Magnetic separation and centrifugation of an aqueous solution of nanoparticles were used for their separation into fractions; their sizes were measured by atomic force microscopy, dynamic light scattering, and electron microscopy. A change in the size leads to a change in the Curie temperature and magnetic moment per formula unit. Both native nanoparticles and those covered with a bioresorbable layer have been considered. The magnetic properties have been calculated by the Monte Carlo method for the classical Heisenbergmore » model with various bulk and surface magnetic moments.« less

Interaction of Water-Soluble CdTe Quantum Dots with Bovine Serum Albumin

PubMed Central

2011-01-01

Semiconductor nanoparticles (quantum dots) are promising fluorescent markers, but it is very little known about interaction of quantum dots with biological molecules. In this study, interaction of CdTe quantum dots coated with thioglycolic acid (TGA) with bovine serum albumin was investigated. Steady state spectroscopy, atomic force microscopy, electron microscopy and dynamic light scattering methods were used. It was explored how bovine serum albumin affects stability and spectral properties of quantum dots in aqueous media. CdTe–TGA quantum dots in aqueous solution appeared to be not stable and precipitated. Interaction with bovine serum albumin significantly enhanced stability and photoluminescence quantum yield of quantum dots and prevented quantum dots from aggregating. PMID:27502633

Fabrication of composite films containing zirconia and cationic polyelectrolytes.

PubMed

Pang, Xin; Zhitomirsky, Igor

2004-03-30

Composite films were prepared by electrophoretic deposition of poly(ethylenimine) or poly(allylamine hydrochloride) combined with cathodic precipitation of zirconia. Films of up to several micrometers thick were obtained on Ni, Pt, stainless-steel, graphite, and carbon-felt substrates. When the concentration of polyelectrolytes in solutions and the deposition time were varied, the amount of the deposited material and its composition can be varied. The electrochemical intercalation of yttria-stabilized zirconia particles into the composite films has been demonstrated. Obtained results pave the way for the electrodeposition of other polymer-ceramic composites. The deposits were studied by thermogravimetric analysis, X-ray diffraction analysis, scanning electron microscopy, and atomic force microscopy. The mechanisms of deposition are discussed.

Recent advances in plant-mediated engineered gold nanoparticles and their application in biological system.

PubMed

Siddiqi, Khwaja Salahuddin; Husen, Azamal

2017-03-01

For biosynthesis of gold nanoparticles different parts of a plant are used as they contain metabolites such as alkaloids, flavonoids, phenols, terpenoids, alcohols, sugars and proteins which act as reducing agents to produce nanoparticles. They also act as capping agent and stabilizer for them. They are used in medicine, agriculture and many other technologies. The attention is therefore focussed on all plant species which have either aroma or colour in their leaves, flowers or roots for the synthesis of nanoparticles because they all contain such chemicals which reduce the metal ions to metal nanoparticles. The size and morphology of gold nanoparticles is dependent on the biogenic-synthetic route, incubation time, temperature, concentration and pH of the solution. In this review, we have discussed the latest developments for the fabrication of gold nanoparticles from herbal extract, their characterization by UV-vis., Fourier transform infrared spectroscopy, transmission electron microscopy, scanning electron microscopy, X-ray diffraction, atomic force microscopy, energy-dispersive X-ray spectroscopy, dynamic light scattering and Zeta Potential techniques. Their application in drug delivery, cancer treatment, catalysis and as antimicrobial agent has also been discussed. Copyright © 2016 Elsevier GmbH. All rights reserved.

Impact of high hydrostatic pressure and pasteurization on the structure and the extractability of bioactive compounds of persimmon “Rojo Brillante”.

PubMed

Hernández-Carrión, M; Vázquez-Gutiérrez, J L; Hernando, I; Quiles, A

2014-01-01

Rojo Brillante is an astringent oriental persimmon variety with high levels of bioactive compounds such as soluble tannins, carotenoids, phenolic acids, and dietary fiber. The purpose of this study was to investigate the effects of high hydrostatic pressure (HHP) and pasteurization on the structure of the fruit and on the extractability of certain bioactive compounds. The microstructure was studied using light microscopy, transmission electron microscopy, and low temperature scanning electron microscopy, and certain physicochemical properties (carotenoid and total soluble tannin content, antioxidant activity, fiber content, color, and texture properties) were measured. The structural changes induced by HHP caused a rise in solute circulation in the tissues that could be responsible for the increased carotenoid level and the unchanged antioxidant activity in comparison with the untreated persimmon. In contrast, the changes that took place during pasteurization lowered the tannin content and antioxidant activity. Consequently, HHP treatment could improve the extraction of potentially bioactive compoundsxsts from persimmons. A high nutritional value ingredient to be used when formulating new functional foods could be obtained using HHP. © 2013 Institute of Food Technologists®

Potentiality of uranium biosorption from nitric acid solutions using shrimp shells.

PubMed

Ahmed, S H; El Sheikh, E M; Morsy, A M A

2014-08-01

Biosorption has gained important credibility during recent years because of its good performance and low cost. This work is concerned with studying the potentiality of the chitin component of the shrimp shells for uranium biosorption from nitric acid liquid solutions. The structural characteristics of the working chitin have been determined via Fourier Transform Infrared Spectroscopy (FTIR). The surface morphology was examined using Scanning Electron Microscopy (SEM). The adsorption capacity of biomass was investigated experimentally. The influence of contact time, pH, metal ion concentration, solution volume to mass ratio and temperature were evaluated and the results were fitted using adsorption isotherm models. The kinetic of uranium biosorption was also investigated as well as biosorption thermodynamic. Copyright © 2014 Elsevier Ltd. All rights reserved.

Plasma induced grafting carboxymethyl cellulose on multiwalled carbon nanotubes for the removal of UO(2)(2+) from aqueous solution.

PubMed

Shao, Dadong; Jiang, Zhongqing; Wang, Xiangke; Li, Jiaxing; Meng, Yuedong

2009-01-29

Carboxymethyl cellulose (CMC) is grafted on multiwalled carbon nanotubes (MWCNT) by using plasma techniques. The CMC grafted MWCNT (MWCNT-g-CMC) is characterized by using Fourier transform infrared spectra (FT-IR), Raman spectra, powder X-ray diffraction (XRD), thermogravimetric analysis (TGA)-differential thermal analysis (DTA), scanning electron microscopy (SEM), and N(2)-BET methods in detail. The application of MWCNT-g-CMC in the removal of UO(2)(2+) from aqueous solution is investigated. MWCNT-g-CMC has much higher sorption ability in the removal of UO(2)(2+) than raw MWCNT. The MWCNT-g-CMC is a suitable material in the preconcentration and solidification of heavy metal ions from large volume of aqueous solutions.

Scanning ultrafast electron microscopy.

PubMed

Yang, Ding-Shyue; Mohammed, Omar F; Zewail, Ahmed H

2010-08-24

Progress has been made in the development of four-dimensional ultrafast electron microscopy, which enables space-time imaging of structural dynamics in the condensed phase. In ultrafast electron microscopy, the electrons are accelerated, typically to 200 keV, and the microscope operates in the transmission mode. Here, we report the development of scanning ultrafast electron microscopy using a field-emission-source configuration. Scanning of pulses is made in the single-electron mode, for which the pulse contains at most one or a few electrons, thus achieving imaging without the space-charge effect between electrons, and still in ten(s) of seconds. For imaging, the secondary electrons from surface structures are detected, as demonstrated here for material surfaces and biological specimens. By recording backscattered electrons, diffraction patterns from single crystals were also obtained. Scanning pulsed-electron microscopy with the acquired spatiotemporal resolutions, and its efficient heat-dissipation feature, is now poised to provide in situ 4D imaging and with environmental capability.

Freeze-Fracture Ultrastructure of Thylakoid Membranes in Chloroplasts from Manganese-Deficient Plants

PubMed Central

Simpson, David J.; Robinson, Simon P.

1984-01-01

Leaves from spinach (Spinacia oleracea L. cv Hybrid 102) plants grown in Mn-deficient nutrient solution were characterized by chlorosis, lowered chlorophyll a/b ratio and reduced electron transport. There were characteristic changes in room temperature fluorescence induction kinetics with increased initial yield (Fo) and decreased variable fluorescence (Fv). The fluorescence yield after the maximum fell rapidly to a level below Fo. The shape of the rise from Fo to the maximum was altered and the size of photosystem II units increased, as measured by half-rise time of Fv in the presence of 3-(3,4-dichlorophenyl)-1,1-dimethylurea. The Mn-deficient leaves were harvested before necrosis, when thin section electron microscopy revealed no disorganization of the thylakoid system. Thylakoid membranes were examined by freeze-fracture electron microscopy. The effect of Mn-deficiency was the specific loss of three-quarters of the particles from the endoplasmic fracture face of appressed thylakoids (EFs). Mn-deficient leaves were restored to near normal 2 days after application of exogenous Mn to the nutrient solution. It is concluded that the loss of most, but not all, functional photosystem II reaction centers from grana, with no alteration in light-harvesting complex or photosystem I, is responsible for the fluorescence and functional properties observed. The response of thylakoids to Mn deficiency shows that there is a fundamental difference in composition and function of stacked and unstacked endoplasmic fracture particles. The stacked endoplasmic fracture particle probably contains, in close association, the photosystem II reaction center and also the Mn-containing polypeptide, the 3-(3,4-dichlorophenyl)-1,1-dimethylurea-binding protein, and all electron transport components in between. Images Fig. 3 Fig. 4 Fig. 5 PMID:16663491

High-Resolution of Electron Microscopy of Montmorillonite and Montmorillonite/Epoxy Nanocomposites

DTIC Science & Technology

2005-01-01

AFRL-ML-WP-TP-2006-464 HIGH-RESOLUTION OF ELECTRON MICROSCOPY OF MONTMORILLONITE AND MONTMORILLONITE /EPOXY NANOCOMPOSITES Lawrence F...HIGH-RESOLUTION OF ELECTRON MICROSCOPY OF MONTMORILLONITE AND MONTMORILLONITE /EPOXY NANOCOMPOSITES 5c. PROGRAM ELEMENT NUMBER 62102F 5d...transmission electron microscopy the structure and morphology of montmorillonite (MMT), a material of current interest for use in polymer nanocomposites, was

Recovery of metals from simulant spent lithium-ion battery as organophosphonate coordination polymers in aqueous media.

PubMed

Perez, Emilie; Andre, Marie-Laure; Navarro Amador, Ricardo; Hyvrard, François; Borrini, Julien; Carboni, Michaël; Meyer, Daniel

2016-11-05

An innovative approach is proposed for the recycling of metals from a simulant lithium-ion battery (LIBs) waste aqueous solution. Phosphonate organic linkers are introduced as precipitating agents to selectively react with the metals to form coordination polymers from an aqueous solution containing Ni, Mn and Co in a hydrothermal process. The supernatant is analyzed by ICP-AES to quantify the efficiency and the selectivity of the precipitation and the materials are characterized by Scanning Electron Microscopy (SEM), Powder X-Ray Diffraction (PXRD), Thermogravimetric Analyses (TGA) and nitrogen gas sorption (BET). Conditions have been achieved to selectively precipitate Manganese or Manganese/Cobalt from this solution with a high efficiency. This work describes a novel method to obtain potentially valuable coordination polymers from a waste metal solution that can be generalized on any waste solution. Copyright © 2016 Elsevier B.V. All rights reserved.

Spatially and temporally controlled biomineralization is facilitated by interaction between self-assembled dentin matrix protein 1 and calcium phosphate nuclei in solution.

PubMed

He, Gen; Gajjeraman, Sivakumar; Schultz, David; Cookson, David; Qin, Chunlin; Butler, William T; Hao, Jianjun; George, Anne

2005-12-13

Bone and dentin biomineralization are well-regulated processes mediated by extracellular matrix proteins. It is widely believed that specific matrix proteins in these tissues modulate nucleation of apatite nanoparticles and their growth into micrometer-sized crystals via molecular recognition at the protein-mineral interface. However, this assumption has been supported only circumstantially, and the exact mechanism remains unknown. Dentin matrix protein 1 (DMP1) is an acidic matrix protein, present in the mineralized matrix of bone and dentin. In this study, we have demonstrated using synchrotron small-angle X-ray scattering that DMP1 in solution can undergo oligomerization and temporarily stabilize the newly formed calcium phosphate nanoparticle precursors by sequestering them and preventing their further aggregation and precipitation. The solution structure represents the first low-resolution structural information for DMP1. Atomic force microscopy and transmission electron microscopy studies further confirmed that the nascent calcium phosphate nuclei formed in solution were assembled into ordered protein-mineral complexes with the aid of oligomerized DMP1, recombinant and native. This study reveals a novel mechanism by which DMP1 might facilitate initiation of mineral nucleation at specific sites during bone and dentin mineralization and prevent spontaneous calcium phosphate precipitation in areas in which mineralization is not desirable.

Structure and properties of novel fibers spun from cellulose in NaOH/thiourea aqueous solution.

PubMed

Ruan, Dong; Zhang, Lina; Zhou, Jinping; Jin, Huiming; Chen, Hui

2004-12-15

Cellulose was dissolved rapidly in a NaOH/thiourea aqueous solution (9.5:4.5 in wt.-%) to prepare a transparent cellulose solution, which was employed, for the first time, to spin a new class of regenerated cellulose fibers by wet spinning. The structure and mechanical properties of the resulting cellulose fibers were characterized, and compared with those of commercially available viscose rayon, cuprammonium rayon and Lyocell fibers. The results from wide angle X-ray diffraction and CP/MAS 13C NMR indicated that the novel cellulose fibers have a structure typical for a family II cellulose and possessed relatively high degrees of crystallinity. Scanning electron microscopy (SEM) and optical microscopy images revealed that the cross-section of the fibers is circular, similar to natural silk. The new fibers have higher molecular weights and better mechanical properties than those of viscose rayon. This low-cost technology is simple, different from the polluting viscose process. The dissolution and regeneration of the cellulose in the NaOH/thiourea aqueous solutions were a physical process and a sol-gel transition rather than a chemical reaction, leading to the smoothness and luster of the fibers. This work provides a potential application in the field of functional fiber manufacturing.

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

PubMed

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

2010-07-27

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

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

PubMed Central

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

2010-01-01

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

Elastomeric photo-actuators and their investigation by confocal laser scanning microscopy

NASA Astrophysics Data System (ADS)

Czaniková, Klaudia; Ilčíková, Markéta; Krupa, Igor; Mičušík, Matej; Kasák, Peter; Pavlova, Ewa; Mosnáček, Jaroslav; Chorvát, Dušan, Jr.; Omastová, Mária

2013-10-01

The photo-actuation behavior of nanocomposites based on ethylene-vinylacetate copolymer (EVA) and styrene-isoprene-styrene (SIS) block copolymer filled with well-dispersed and modified multiwalled carbon nanotubes (MWCNTs) is discussed in this paper. The nanocomposites were prepared by casting from solution. To improve the dispersion of the MWCNTs in EVA, the MWCNT surface was modified with a non-covalent surfactant, cholesteryl 1-pyrenecarboxylate (PyChol). To prepare SIS nanocomposites, the MWCNT surface was covalently modified with polystyrene chains. The good dispersion of the filler was confirmed by transmission electron microscopy (TEM). Special, custom-made punch/die molds were used to create a Braille element (BE)-like shape, which under shear forces induces a uniaxial orientation of the MWCNTs within the matrix. The uniaxial orientation of MWCNTs is an essential precondition to ensure the photo-actuating behavior of MWCNTs in polymeric matrices. The orientation of the MWCNTs within the matrices was examined by scanning electron microscopy (SEM). Nanocomposite BEs were illuminated from the bottom by a red light-emitting diode (LED), and the photo-actuation was investigated by confocal laser scanning microscopy (CLSM). When the BEs were exposed to light, a temporary increase in the height of the element was detected. This process was observed to be reversible: after switching off the light, the BEs returned to their original shape and height.

Microstructures and microhardness evolutions of melt-spun Al-8Ni-5Nd-4Si alloy

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

Karakoese, Ercan, E-mail: ekarakose@karatekin.edu.tr; Keskin, Mustafa

2012-03-15

Al-Ni-Nd-Si alloy with nominal composition of Al-8 wt.%Ni-5 wt.%Nd-4 wt.%Si was rapidly solidified by using melt-spinning technique to examine the influence of the cooling rate/conditions on microstructure and mechanical properties. The resulting conventional cast (ingot) and melt-spun ribbons were characterized by X-ray diffraction, optical microscopy, scanning electron microscopy together with energy dispersive spectroscopy, differential scanning calorimetry, differential thermal analysis and Vickers microhardness tester. The ingot alloys consists of four phases namely {alpha}-Al, intermetallic Al{sub 3}Ni, Al{sub 11}Nd{sub 3} and fcc Si. Melt-spun ribbons are completely composed of {alpha}-Al phase. The optical microscopy and scanning electron microscopy results show that themore » microstructures of rapidly solidified ribbons are clearly different from their ingot alloy. The change in microhardness is discussed based on the microstructural observations. - Highlights: Black-Right-Pointing-Pointer Rapid solidification allows a reduction in grain size, extended solid solution ranges. Black-Right-Pointing-Pointer We observed the matrix lattice parameter increases with increasing wheel speed. Black-Right-Pointing-Pointer Melt-spun ribbons consist of partly amorphous phases embedded in crystalline phases. Black-Right-Pointing-Pointer The solidification rate is high enough to retain most of alloying elements in the Al matrix. Black-Right-Pointing-Pointer The rapid solidification has effect on the phase constitution.« less

Exploring Charge Transport in Guest Molecule Infiltrated Cu 3(BTC) 2 Metal Organic Framework

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

Leonard, Francois Leonard; Stavila, Vitalie; Allendorf, Mark D.

2014-09-01

The goal of this Exploratory Express project was to expand the understanding of the physical properties of our recently discovered class of materials consisting of metal-organic frameworks with electroactive ‘guest’ molecules that together form an electrically conducting charge-transfer complex (molecule@MOF). Thin films of Cu 3(BTC) 2 were grown on fused silica using solution step-by-step growth and were infiltrated with the molecule tetracyanoquinodimethane (TCNQ). The infiltrated MOF films were extensively characterized using optical microscopy, scanning electron microscopy, Raman spectroscopy, electrical conductivity, and thermoelectric properties. Thermopower measurements on TCNQ@Cu 3(BTC) 2 revealed a positive Seebeck coefficient of ~400 μV/k, indicating that holesmore » are the primary carriers in this material. The high value of the Seebeck coefficient and the expected low thermal conductivity suggest that molecule@MOF materials may be attractive for thermoelectric power conversion applications requiring low cost, solution-processable, and non-toxic active materials.« less

A novel method for the fabrication of microfluidic devices by photopolymerization of polymethylmethacrylate

NASA Astrophysics Data System (ADS)

Forstater, Jacob; Augustine, Brian; Hughes, Chris

2006-11-01

We have developed a new technique for the rapid fabrication of structures useful for microfluidic devices called micromolding by photopolymerization in capillaries (μ-PIC). The technique involves the replication of features from a silicon master in which features on the order of tens to hundreds of microns have been formed by crystallographic etching. The negative of the features is then transferred to a sheet of polymethylmethacrylate (PMMA) by placing the PMMA sheet over the silicon master and injecting a solution of methylmethacrylate monomer with a benzoin methyl ether photoinitiator. This solution is drawn between the PMMA and the silicon by capillary action forming a liquid layer that is no more than a few hundred microns thick. This liquid is then polymerized by exposure to ultraviolet light for less than a half hour. The features transferred in this manner have nearly identical surface structure and roughness. Analysis of these surfaces and structures by atomic force microscopy and scanning electron microscopy will be presented.

Investigation of Mechanical Properties and Fracture Simulation of Solution-Treated AA 5754

NASA Astrophysics Data System (ADS)

Kumar, Pankaj; Singh, Akhilendra

2017-10-01

In this work, mechanical properties and fracture toughness of as-received and solution-treated aluminum alloy 5754 (AA 5754) are experimentally evaluated. Solution heat treatment of the alloy is performed at 530 °C for 2 h, and then, quenching is done in water. Yield strength, ultimate tensile strength, impact toughness, hardness, fatigue life, brittle fracture toughness (K_{Ic} ) and ductile fracture toughness (J_{Ic} ) are evaluated for as-received and solution-treated alloy. Extended finite element method has been used for the simulation of tensile and fracture behavior of material. Heaviside function and asymptotic crack tip enrichment functions are used for modelling of the crack in the geometry. Ramberg-Osgood material model coupled with fracture energy is used to simulate the crack propagation. Fracture surfaces obtained from various mechanical tests are characterized by scanning electron microscopy.

SnS2 Thin Film Deposition by Spray Pyrolysis

NASA Astrophysics Data System (ADS)

Jaber, Abdallah Yahia; Alamri, Saleh Noaiman; Aida, Mohammed Salah

2012-06-01

Tin disulfide (SnS2) thin films have been synthesized using a simplified spray pyrolysis technique using a perfume atomizer. The films were deposited using two different solutions prepared by the dilution of SnCl2 and thiourea in distilled water and in methanol. The obtained films have a microcrystalline structure. The film deposited using methanol as the solvent is nearly stochiometric SnS2 with a spinel phase having a (001) preferential orientation. The film prepared with an aqueous solution is Sn-rich. Scanning electronic microscopy (SEM) images reveal that the film deposited with the aqueous solution is rough and is formed with large wires. However, the film deposited with methanol is dense and smooth. Conductivity measurements indicate that the aqueous solution leads to an n-type semiconductor, while methanol leads to a p-type semiconductor.

Mesoporous aluminium organophosphonates: a reusable chemsensor for the detection of explosives

NASA Astrophysics Data System (ADS)

Li, Dongdong; Yu, Xiang

2016-07-01

Rapid and sensitive detection of explosives is in high demand for homeland security and public safety. In this work, electron-rich of anthracene functionalized mesoporous aluminium organophosphonates (En-AlPs) were synthesized by a one-pot condensation process. The mesoporous structure and strong blue emission of En-AlPs were confirmed by the N2 adsorption-desorption isotherms, transmission electron microscopy images and fluorescence spectra. The materials En-AlPs can serve as sensitive chemosensors for various electron deficient nitroderivatives, with the quenching constant and the detection limit up to 1.5×106 M-1 and 0.3 ppm in water solution. More importantly, the materials can be recycled for many times by simply washed with ethanol, showing potential applications in explosives detection.

Attaching quantum dots to HER2 specific phage antibodies

NASA Astrophysics Data System (ADS)

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

2010-06-01

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

Evaluation of preparation methods for suspended nano-objects on substrates for dimensional measurements by atomic force microscopy

PubMed Central

Göhler, Daniel; Wessely, Benno; Stintz, Michael; Lazzerini, Giovanni Mattia; Yacoot, Andrew

2017-01-01

Dimensional measurements on nano-objects by atomic force microscopy (AFM) require samples of safely fixed and well individualized particles with a suitable surface-specific particle number on flat and clean substrates. Several known and proven particle preparation methods, i.e., membrane filtration, drying, rinsing, dip coating as well as electrostatic and thermal precipitation, were performed by means of scanning electron microscopy to examine their suitability for preparing samples for dimensional AFM measurements. Different suspensions of nano-objects (with varying material, size and shape) stabilized in aqueous solutions were prepared therefore on different flat substrates. The drop-drying method was found to be the most suitable one for the analysed suspensions, because it does not require expensive dedicated equipment and led to a uniform local distribution of individualized nano-objects. Traceable AFM measurements based on Si and SiO2 coated substrates confirmed the suitability of this technique. PMID:28904839

Evaluation of preparation methods for suspended nano-objects on substrates for dimensional measurements by atomic force microscopy.

PubMed

Fiala, Petra; Göhler, Daniel; Wessely, Benno; Stintz, Michael; Lazzerini, Giovanni Mattia; Yacoot, Andrew

2017-01-01

Dimensional measurements on nano-objects by atomic force microscopy (AFM) require samples of safely fixed and well individualized particles with a suitable surface-specific particle number on flat and clean substrates. Several known and proven particle preparation methods, i.e., membrane filtration, drying, rinsing, dip coating as well as electrostatic and thermal precipitation, were performed by means of scanning electron microscopy to examine their suitability for preparing samples for dimensional AFM measurements. Different suspensions of nano-objects (with varying material, size and shape) stabilized in aqueous solutions were prepared therefore on different flat substrates. The drop-drying method was found to be the most suitable one for the analysed suspensions, because it does not require expensive dedicated equipment and led to a uniform local distribution of individualized nano-objects. Traceable AFM measurements based on Si and SiO 2 coated substrates confirmed the suitability of this technique.

Phase relations in the system CuMoS

USGS Publications Warehouse

Dawei, H.; Chang, L.L.Y.; Knowles, C.R.

1990-01-01

Phase relations in the system CuMoS were studied in the temperature range 500-1000 ??C by using the conventional sealed, evacuated glass capsule technique. Reflected-light microscopy, X-ray powder diffraction and electron microprobe analysis were used for phase characterization. The chevrel-type phase, CuxMo3S4, is stable above 600??C, and forms equilibrium assemblages with the cubic Cu2S solid solution, copper, molybdenum, Mo2S3 and MoS2. Its solid solution ranges from Cu1.50-2.00Mo3S4 at 700??C to Cu1.22-2.00Mo3S4 at 1000 ??C. ?? 1990.

Determination of dextrose in peritoneal dialysis solution by localized surface plasmon resonance technique based on silver nanoparticles formation

NASA Astrophysics Data System (ADS)

Masrournia, Mahboube; Montazarolmahdi, Maliheh; Sani, Faramarz Aliasghari

2017-07-01

Determination of dextrose in peritoneal dialysis with a method based on silver nanoparticles (AgNPs) formation was investigated. In a green chemistry method, silver nanoparticles (AgNPs) were synthesized in the natural polymeric matrix of gelatin. The nanoparticles were characterized with UV-Vis spectroscopy and transmission electron microscopy (TEM). Absorbance signal of AgNPs could be applied to determine the various concentrations of dextrose solutions. Drop wise and ultrasonic methods were used and compared with each other. The dynamic range of methods with limit of detection and relative standard deviations were obtained. Results for real sample (peritoneal dialysis) were satisfied.

Influence of sodium bis(2-ethylhexyl) sulfosuccinate (AOT) on zinc electrodeposition

NASA Astrophysics Data System (ADS)

Lehr, I. L.; Saidman, S. B.

2012-03-01

This work is a study of the electrodeposition of zinc onto SAE 4140 steel electrodes using solutions containing zinc sulfate and bis(2-ethylhexyl) sodium sulfosuccinate (AOT). The influence of different parameters such as electrolyte concentration, electrodeposition time and temperature on the morphology of the electrodeposits was analyzed. The deposits were characterized by scanning electron microscopy (SEM), energy dispersive X-ray (EDX) and X-ray diffraction. The variation of open circuit potential over time in chloride solutions was also evaluated. The nucleation-growth process and consequently the morphology of the electrodeposits are modified in the presence of AOT. The surfactant induces the formation of a porous deposit.

Effect of Phosphine-Free Selenium Precursor Reactivity on The Optical and Vibrational properties of Colloidal CdSe Nanocrystals

NASA Astrophysics Data System (ADS)

Thi, L. A.; Lieu, N. T. T.; Hoa, N. M.; Tran, N.; Binh, N. T.; Quang, V. X.; Nghia, N. X.

2018-03-01

Phosphine-free selenium precursor solutions have been prepared by heating at temperatures ranging from 160 °C to 240 °C and studied by means of infrared absorption spectroscopy. The colloidal CdSe nanocrystals (NCs) synthesized from all those solutions by the wet chemical method. The influence of heating temperature on the chemical reactivity of selenium precursor and its role on the optical and vibrational properties of CdSe NCs are discussed in details. Their morphology, particle size, structural, optical and vibrational properties were investigated using transmission electron microscopy, X-ray diffraction, UV-Vis, fluorescence and Raman spectroscopy, respectively.

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

Yulaev, Alexander; Guo, Hongxuan; Strelcov, Evgheni

Atomic-scale thickness, molecular impermeability, low atomic number, and mechanical strength make graphene an ideal electron-transparent membrane for material characterization in liquids and gases with scanning electron microscopy and spectroscopy. Here in this paper, we present a novel sample platform made of an array of thousands of identical isolated graphene-capped microchannels with high aspect ratio. A combination of a global wide field of view with high resolution local imaging of the array allows for high throughput in situ studies as well as for combinatorial screening of solutions, liquid interfaces, and immersed samples. We demonstrate the capabilities of this platform by studyingmore » a pure water sample in comparison with alkali halide solutions, a model electrochemical plating process, and beam-induced crystal growth in liquid electrolyte. Spectroscopic characterization of liquid interfaces and immersed objects with Auger and X-ray fluorescence analysis through the graphene membrane are also demonstrated.« less

Composite Ni-Co-fly ash coatings on 5083 aluminium alloy

NASA Astrophysics Data System (ADS)

Panagopoulos, C. N.; Georgiou, E. P.; Tsopani, A.; Piperi, L.

2011-03-01

Ni-Co-fly ash coatings were deposited on zincate treated 5083 wrought aluminium alloy substrates with the aid of the electrodeposition technique. Structural and chemical characterization of the produced composite coatings was performed with the aid of X-ray diffraction (XRD), scanning electron microscopy (SEM) and electron dispersive X-ray analysis (EDS) techniques. The Ni-Co-fly ash coatings were found to consist of a crystalline Ni-Co solid solution with dispersed fly ash particles. In addition, chemical analysis of the Ni-Co matrix showed that it consisted of 80 wt.% Ni and 20 wt.% Co. The co-deposition of fly ash particles leads to a significant increase of the microhardness of the coating. The corrosion behaviour of the Ni-Co-fly ash/zincate coated aluminium alloy, in a 0.3 M NaCl solution (pH = 3.5), was studied by means of potentiodynamic corrosion experiments.

Development and characterization of Mn{sup 2+}-doped MgO nanoparticles by solution combustion synthesis

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

Basha, Md. Hussain; Gopal, N. O., E-mail: nogopal@yahoo.com; Rao, J. L.

2015-06-24

Mn doped MgO Nanoparticles have been prepared by Solution Combustion Synthesis. The synthesized sample is characterized by X-ray diffraction (XRD), Scanning Electron Microscopy (SEM) and Electron Paramagnetic Resonance (EPR). The prepared MgO:Mn (1 mol%) nano crystals appear to be of simple cubic crystalline phase with lattice parameters a = 4.218(2) Å and cell volume = 74.98 (7) Å{sup 3}. SEM micrograph of powders show highly porous, many agglomerates with irregular morphology, large voids, cracks and pores. EPR spectrum of the sample at room temperature exhibit an isotropic sextet hyperfine pattern, centered at g=1.99, characteristic if Mn{sup 2+} ions with S=I=5/2.The observedmore » g value and the hyperfine value reveal the ionic bonding between Mn{sup 2+} and its surroundings.« less

Cytological evaluation of the effect of azoxystrobin and alternative oxidase inhibitors in Botrytis cinerea.

PubMed

Inoue, Kanako; Tsurumi, Tomohiro; Ishii, Hideo; Park, Pyoyun; Ikeda, Kenichi

2012-01-01

Azoxystrobin (AZ), a strobilurin-derived fungicide, is known to inhibit mitochondrial respiration in fungi by blocking the electron transport chain in the inner mitochondrial membrane. Germination was strongly inhibited when Botrytis cinerea spore suspension was treated with AZ and the alternative oxidase (AOX) inhibitors, salicylhydroxamic acid (SHAM) and n-propyl gallate. However, chemical death indicators trypan blue and propidium iodide showed that those spores were still alive. When the spore suspension in the AZ and SHAM solution was replaced with distilled water, the germination rate almost recovered, at least during the first 2 days of incubation with AZ and SHAM solution. No morphological alteration was detected in the cells treated with AZ and SHAM, especially in mitochondria, using transmission electron microscopy. Therefore, simultaneous application of AZ and AOX inhibitors has a fungistatic, rather than a fungicidal, action. © 2011 Federation of European Microbiological Societies. Published by Blackwell Publishing Ltd. All rights reserved.

In Vitro Toxicity of Silver Nanoparticles in Human Lung Epithelial Cells

DTIC Science & Technology

2009-03-01

software from the particle distributions measured and the polydispersity index (PdI) given is a measure of the size ranges present in the solution...Transmission Electron Microscopy Figure 22 shows the TEM primary particles size and distribution determined from measurement of over 100 particles from...nm uncoated. (B) Ag 80 nm uncoated. (C) Ag 10 nm coated. (D) Ag 80 nm coated Table 4 shows the TEM primary particles size and distribution

Electron Microscopy of Staphylococcus aureus Cell Wall Lysis

PubMed Central

Virgilio, R.; González, C.; Muñoz, Nubia; Mendoza, Silvia

1966-01-01

Virgilio, Rafael (Escuela de Química y Farmacia, Universidad de Chile, Santiago, Chile), C. González, Nubia Muñoz, and Silvia Mendoza. Electron microscopy of Staphylococcus aureus cell wall lysis. J. Bacteriol. 91:2018–2024. 1966.—A crude suspension of Staphylococcus aureus cell walls (strain Cowan III) in buffer solution was shown by electron microscopy to lyse slightly after 16 hr, probably owing to the action of autolysin. The lysis was considerably faster and more intense after the addition of lysozyme. A remarkable reduction in thickness and rigidity of the cell walls, together with the appearance of many irregular protrusions in their outlines, was observed after 2 hr; after 16 hr, there remained only a few recognizable cell wall fragments but many residual particulate remnants. When autolysin was previously inactivated by trypsin, there was a complete inhibition of the lytic action of lysozyme; on the other hand, when autolysin was inactivated by heat and lysozyme was added, a distinct decrease in the thickness of the cell walls was observed, but there was no destruction of the walls. The lytic action of lysozyme, after treatment with hot 5% trichloroacetic acid, gave rise to a marked dissolution of the structure of the cell walls, which became lost against the background, without, however, showing ostensible alteration of wall outlines. From a morphological point of view, the lytic action of autolysin plus lysozyme was quite different from that of trichloroacetic acid plus lysozyme, as shown by electron micrographs, but in both cases it was very intense. This would suggest different mechanisms of action for these agents. Images PMID:5939482

Electron microscopy of Staphylococcus aureus cell wall lysis.

PubMed

Virgilio, R; González, C; Muñoz, N; Mendoza, S

1966-05-01

Virgilio, Rafael (Escuela de Química y Farmacia, Universidad de Chile, Santiago, Chile), C. González, Nubia Muñoz, and Silvia Mendoza. Electron microscopy of Staphylococcus aureus cell wall lysis. J. Bacteriol. 91:2018-2024. 1966.-A crude suspension of Staphylococcus aureus cell walls (strain Cowan III) in buffer solution was shown by electron microscopy to lyse slightly after 16 hr, probably owing to the action of autolysin. The lysis was considerably faster and more intense after the addition of lysozyme. A remarkable reduction in thickness and rigidity of the cell walls, together with the appearance of many irregular protrusions in their outlines, was observed after 2 hr; after 16 hr, there remained only a few recognizable cell wall fragments but many residual particulate remnants. When autolysin was previously inactivated by trypsin, there was a complete inhibition of the lytic action of lysozyme; on the other hand, when autolysin was inactivated by heat and lysozyme was added, a distinct decrease in the thickness of the cell walls was observed, but there was no destruction of the walls. The lytic action of lysozyme, after treatment with hot 5% trichloroacetic acid, gave rise to a marked dissolution of the structure of the cell walls, which became lost against the background, without, however, showing ostensible alteration of wall outlines. From a morphological point of view, the lytic action of autolysin plus lysozyme was quite different from that of trichloroacetic acid plus lysozyme, as shown by electron micrographs, but in both cases it was very intense. This would suggest different mechanisms of action for these agents.

Electron Microscopy.

ERIC Educational Resources Information Center

Beer, Michael

1980-01-01

Reviews technical aspects of structure determination in biological electron microscopy (EM). Discusses low dose EM, low temperature microscopy, electron energy loss spectra, determination of mass or molecular weight, and EM of labeled systems. Cites 34 references. (CS)

Imaging of endodontic biofilms by combined microscopy (FISH/cLSM - SEM).

PubMed

Schaudinn, C; Carr, G; Gorur, A; Jaramillo, D; Costerton, J W; Webster, P

2009-08-01

Scanning electron microscopy is a useful imaging approach for the visualization of bacterial biofilms in their natural environments including their medical and dental habitats, because it allows for the exploration of large surfaces with excellent resolution of topographic features. Most biofilms in nature, however, are embedded in a thick layer of extracellular matrix that prevents a clear identification of individual bacteria by scanning electron microscopy. The use of confocal laser scanning microscopy on the other hand in combination with fluorescence in situ hybridization enables the visualization of matrix embedded bacteria in multi-layered biofilms. In our study, fluorescence in situ hybridization/confocal laser scanning microscopy and scanning electron microscopy were applied to visualize bacterial biofilm in endodontic root canals. The resulting fluorescence in situ hybridization /confocal laser scanning microscopy and scanning electron microscopy and pictures were subsequently combined into one single image to provide high-resolution information on the location of hidden bacteria. The combined use of scanning electron microscopy and fluorescence in situ hybridization / confocal laser scanning microscopy has the potential to overcome the limits of each single technique.

Silver/polysaccharide-based nanofibrous materials synthesized from green chemistry approach.

PubMed

Martínez-Rodríguez, M A; Garza-Navarro, M A; Moreno-Cortez, I E; Lucio-Porto, R; González-González, V A

2016-01-20

In this contribution a novel green chemistry approach for the synthesis of nanofibrous materials based on blends of carboxymethyl-cellulose (CMC)-silver nanoparticles (AgNPs) composite and polyvinyl-alcohol (PVA) is proposed. These nanofibrous materials were obtained from the electrospinning of blends of aqueous solutions of CMC-AgNPs composite and PVA, which were prepared at different CMC/PVA weight ratios in order to electrospin nanofibers applying a constant tension of 15kV. The synthesized materials were characterized by means of transmission electron microscopy, scanning electron microscopy; as well as Fourier-transform infrared, ultraviolet and Raman spectroscopic techniques. Experimental evidence suggests that the diameter of the nanofibers is thinner than any other reported in the literature regarding the electrospinning of CMC. This feature is related to the interactions of AgNPs with carboxyl functional groups of the CMC, which diminish those between the later and acetyl groups of PVA. Copyright © 2015 Elsevier Ltd. All rights reserved.

Effect of intermetallic phases on the anodic oxidation and corrosion of 5A06 aluminum alloy

NASA Astrophysics Data System (ADS)

Li, Song-mei; Li, Ying-dong; Zhang, You; Liu, Jian-hua; Yu, Mei

2015-02-01

Intermetallic phases were found to influence the anodic oxidation and corrosion behavior of 5A06 aluminum alloy. Scattered intermetallic particles were examined by scanning electron microscopy (SEM) and energy dispersive spectroscopy (EDS) after pretreatment. The anodic film was investigated by transmission electron microscopy (TEM), and its corrosion resistance was analyzed by electrochemical impedance spectroscopy (EIS) and Tafel polarization in NaCl solution. The results show that the size of Al-Fe-Mg-Mn particles gradually decreases with the iron content. During anodizing, these intermetallic particles are gradually dissolved, leading to the complex porosity in the anodic film beneath the particles. After anodizing, the residual particles are mainly silicon-containing phases, which are embedded in the anodic film. Electrochemical measurements indicate that the porous anodic film layer is easily penetrated, and the barrier plays a dominant role in the overall protection. Meanwhile, self-healing behavior is observed during the long immersion time.

Hierarchically Self-Assembled Star-Shaped ZnO Microparticles for Electrochemical Sensing of Amines.

PubMed

Du, Jianping; Huang, Xiaoxi; Zhao, Ruihua; Li, Jinping; Asefa, Tewodros

2016-06-06

Novel, hierarchically nanostructured, star-shaped ZnO (SSZ) microparticles are synthesized by a hydrothermal synthetic route. The SSZ microparticles serve as effective platforms for electrochemical detection of amines in solution. The morphology and structure of the materials are characterized by X-ray diffraction, scanning electron microscopy, transmission electron microscopy, Raman spectroscopy, and UV/Vis spectroscopy. The as-synthesized SSZ microparticles comprise self-assembled hexagonal prisms that possess nanometer and micrometer pores in their structure and on their surfaces-structural features that are conducive to sensing applications. An electrode fabricated by using the hierarchically nanostructured SSZ materials serve as a sensitive electrochemical sensor for detection of low concentrations of ethylenediamine, with a sensitivity of 2.98×10(-2)  mA cm(-2)  mm(-1) , a detection limit of 2.36×10(-2)  mm, and a short response time of 8 s. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Nitridation of porous GaAs by an ECR ammonia plasma

NASA Astrophysics Data System (ADS)

Naddaf, M.; Hullavarad, S. S.; Ganesan, V.; Bhoraskar, S. V.

2006-02-01

The effect of surface porosity of GaAs on the nature of growth of GaN, by use of plasma nitridation of GaAs, has been investigated. Porous GaAs samples were prepared by anodic etching of n-type (110) GaAs wafers in HCl solution. Nitridation of porous GaAs samples were carried out by using an electron-cyclotron resonance-induced ammonia plasma. The formation of mixed phases of GaN was investigated using the grazing angle x-ray diffraction method. A remarkable improvement in the intensity of photoluminescence (PL) compared with that of GaN synthesized by direct nitriding of GaAs surface has been observed. The PL intensity of nitrided porous GaAs at the temperature of 380 °C was found to be about two orders of magnitude higher as compared with the directly nitrided GaAs at the temperature of 500 °C. The changes in the morphology of nitrided porous GaAs have been investigated using both scanning electron microscopy and atomic force microscopy.

The facile synthesis of hierarchical NiCoO2 nanotubes comprised ultrathin nanosheets for supercapacitors

NASA Astrophysics Data System (ADS)

Xu, Xin; Zhou, Han; Ding, Shujiang; Li, Jun; Li, Beibei; Yu, Demei

2014-12-01

Hierarchical NiCoO2 nanosheets nanotubes are successfully prepared by a mild solution method based on the template of polymeric nanotubes (PNT) followed by a thermal annealing treatment. The microstructure and chemical composition of NiCoO2 nanosheets nanotubes are characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), Brunauer-Emmett-Teller (BET) analyzer, X-ray diffraction (XRD) and Thermogravimetric analysis (TGA). When evaluated as an electrode material for supercapacitors, the results of electrochemical test show that the unique NiCoO2 nanosheets nanotubes exhibit relatively high specific capacitance of 1468, 1352, 1233, 1178, 1020 and 672 F g-1 at the discharge current densities of 2, 4, 8, 10, 20 and 40 A g-1, respectively. They also reveal an excellent cycling stability of 99.2% retention after 3000 cycles at 10 A g-1. The smart nanostructures of the NiCoO2 nanosheets nanotubes make a prominent contribution to the excellent electrochemical performance.

Biosynthesis of amorphous mesoporous aluminophosphates using yeast cells as templates

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

Sifontes, Ángela B., E-mail: asifonte@ivic.gob.ve; González, Gema; Tovar, Leidy M.

2013-02-15

Graphical abstract: Display Omitted Highlights: ► Amorphous aluminophosphates can take place using yeast as template. ► A mesoporous material was obtained. ► The specific surface area after calcinations ranged between 176 and 214 m{sup 2} g{sup −1}. -- Abstract: In this study aluminophosphates have been synthesized from aluminum isopropoxide and phosphoric acid solutions using yeast cells as template. The physicochemical characterization was carried out by thermogravimetric analysis; X-ray diffraction; Fourier transform infrared; N{sub 2} adsorption–desorption isotherms; scanning electron microscopy; transmission electron microscopy and potentiometric titration with N-butylamine for determination of: thermal stability; crystalline structure; textural properties; morphology and surface acidity,more » respectively. The calcined powders consisted of an intimate mixture of amorphous and crystallized AlPO particles with sizes between 23 and 30 nm. The average pore size observed is 13–16 nm and the specific surface area after calcinations (at 650 °C) ranged between 176 and 214 m{sup 2} g{sup −1}.« less

MnO2 nanotubes assembled on conductive graphene/polyester composite fabric as a three-dimensional porous textile electrode for flexible electrochemical capacitors.

PubMed

Jin, Chun; Jin, Li-Na; Guo, Mei-Xia; Liu, Ping; Zhang, Jia-Nan; Bian, Shao-Wei

2017-12-15

A three-dimensional (3D) electrode material was successfully synthesized through a facile ZnO-assisted hydrothermal process in which vertical MnO 2 nanotube arrays were in situ grown on the conductive graphene/polyester composite fabric. The morphology and structure of MnO 2 nanotubes/graphene/polyester textile electrode were characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS). The 3D electrode structure facilitates to achieve the maximum number of active sites for the pesudocapacitance redox reaction, fast electrolyte ion transportation and short ion diffusion path. The electrochemical measurements showed that the electrode possesses good capacitance capacity which reached 498F/g at a scan rate of 2mV/s in Na 2 SO 4 electrolyte solution. The electrode also showed stable electrochemical performances under the conditions of long-term cycling, and mechanical bending and twisting. Copyright © 2017 Elsevier Inc. All rights reserved.

Efficient estimation of three-dimensional covariance and its application in the analysis of heterogeneous samples in cryo-electron microscopy

PubMed Central

Liao, Hstau Y.; Hashem, Yaser; Frank, Joachim

2015-01-01

Summary Single-particle cryogenic electron microscopy (cryo-EM) is a powerful tool for the study of macromolecular structures at high resolution. Classification allows multiple structural states to be extracted and reconstructed from the same sample. One classification approach is via the covariance matrix, which captures the correlation between every pair of voxels. Earlier approaches employ computing-intensive resampling and estimate only the eigenvectors of the matrix, which are then used in a separate fast classification step. We propose an iterative scheme to explicitly estimate the covariance matrix in its entirety. In our approach, the flexibility in choosing the solution domain allows us to examine a part of the molecule in greater detail. 3D covariance maps obtained in this way from experimental data (cryo-EM images of the eukaryotic pre-initiation complex) prove to be in excellent agreement with conclusions derived by using traditional approaches, revealing in addition the interdependencies of ligand bindings and structural changes. PMID:25982529

Efficient estimation of three-dimensional covariance and its application in the analysis of heterogeneous samples in cryo-electron microscopy.

PubMed

Liao, Hstau Y; Hashem, Yaser; Frank, Joachim

2015-06-02

Single-particle cryogenic electron microscopy (cryo-EM) is a powerful tool for the study of macromolecular structures at high resolution. Classification allows multiple structural states to be extracted and reconstructed from the same sample. One classification approach is via the covariance matrix, which captures the correlation between every pair of voxels. Earlier approaches employ computing-intensive resampling and estimate only the eigenvectors of the matrix, which are then used in a separate fast classification step. We propose an iterative scheme to explicitly estimate the covariance matrix in its entirety. In our approach, the flexibility in choosing the solution domain allows us to examine a part of the molecule in greater detail. Three-dimensional covariance maps obtained in this way from experimental data (cryo-EM images of the eukaryotic pre-initiation complex) prove to be in excellent agreement with conclusions derived by using traditional approaches, revealing in addition the interdependencies of ligand bindings and structural changes. Copyright © 2015 Elsevier Ltd. All rights reserved.

Dead biomass of Amazon yeast: A new insight into bioremediation and recovery of silver by intracellular synthesis of nanoparticles.

PubMed

Salvadori, Marcia R; Ando, Rômulo A; Nascimento, Cláudio A Oller; Corrêa, Benedito

2017-09-19

This investigation was undertaken to describe a natural process for the removal of silver and the simultaneous recovery of Ag/Ag 2 O nanoparticles by dead biomass of the yeast Rhodotorula mucilaginosa. The removal of silver ions from aqueous solution and the synthesis of Ag/Ag 2 O nanoparticles were analyzed based on physicochemical factors and equilibrium concentration, combined with transmission electron microscopy (TEM), scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDS), X-ray photoelectron spectroscopy (XPS), and infrared spectroscopy (FTIR). A successful process for the synthesis of Ag/Ag 2 O nanoparticles was obtained, following the Langmuir isotherm model, showing a high biosorption capacity of silver (49.0 mg g -1 ). The nanoparticles were spherical, had an average size of 11.0 nm, were synthesized intracellularly and capped by yeast proteins. This sustainable protocol is an attractive platform for the industrial-scale production of silver nanoparticles and of a silver nanobiosorbent.

Fabrication of Metal and Metal Oxide Nanoparticles by Algae and their Toxic Effects

NASA Astrophysics Data System (ADS)

Siddiqi, Khwaja Salahuddin; Husen, Azamal

2016-08-01

Of all the aquatic organisms, algae are a good source of biomolecules. Since algae contain pigments, proteins, carbohydrates, fats, nucleic acids and secondary metabolites such as alkaloids, some aromatic compounds, macrolides, peptides and terpenes, they act as reducing agents to produce nanoparticles from metal salts without producing any toxic by-product. Once the algal biomolecules are identified, the nanoparticles of desired shape or size may be fabricated. The metal and metal oxide nanoparticles thus synthesized have been investigated for their antimicrobial activity against several gram-positive and gram-negative bacterial strains and fungi. Their dimension is controlled by temperature, incubation time, pH and concentration of the solution. In this review, we have attempted to update the procedure of nanoparticle synthesis from algae, their characterization by UV-vis, Fourier transform infrared spectroscopy, transmission electron microscopy, scanning electron microscopy, x-ray diffraction, energy-dispersive x-ray spectroscopy, dynamic light scattering and application in cutting-edge areas.

Trimethylamine Sensors Based on Au-Modified Hierarchical Porous Single-Crystalline ZnO Nanosheets.

PubMed

Meng, Fanli; Zheng, Hanxiong; Sun, Yufeng; Li, Minqiang; Liu, Jinhuai

2017-06-22

It is of great significance for dynamic monitoring of foods in storage or during the transportation process through on-line detecting trimethylamine (TMA). Here, TMA were sensitively detected by Au-modified hierarchical porous single-crystalline ZnO nanosheets (HPSCZNs)-based sensors. The HPSCZNs were synthesized through a one-pot wet-chemical method followed by an annealing treatment. Polyethyleneimine (PEI) was used to modify the surface of the HPSCZNs, and then the PEI-modified samples were mixed with Au nanoparticles (NPs) sol solution. Electrostatic interactions drive Au nanoparticles loading onto the surface of the HPSCZNs. The Au-modified HPSCZNs were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and energy dispersive spectrum (EDS), respectively. The results show that Au-modified HPSCZNs-based sensors exhibit a high response to TMA. The linear range is from 10 to 300 ppb; while the detection limit is 10 ppb, which is the lowest value to our knowledge.

Eco-friendly preparation of large-sized graphene via short-circuit discharge of lithium primary battery.

PubMed

Kang, Shaohong; Yu, Tao; Liu, Tingting; Guan, Shiyou

2018-02-15

We proposed a large-sized graphene preparation method by short-circuit discharge of the lithium-graphite primary battery for the first time. LiC x is obtained through lithium ions intercalation into graphite cathode in the above primary battery. Graphene was acquired by chemical reaction between LiC x and stripper agents with dispersion under sonication conditions. The gained graphene is characterized by Raman spectrum, X-ray diffraction (XRD), transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS), Atomic force microscope (AFM) and Scanning electron microscopy (SEM). The results indicate that the as-prepared graphene has a large size and few defects, and it is monolayer or less than three layers. The quality of graphene is significant improved compared to the reported electrochemical methods. The yield of graphene can reach 8.76% when the ratio of the H 2 O and NMP is 3:7. This method provides a potential solution for the recycling of waste lithium ion batteries. Copyright © 2017 Elsevier Inc. All rights reserved.

Colorimeter and scanning electron microscopy analysis of teeth submitted to internal bleaching.

PubMed

Martin-Biedma, Benjamin; Gonzalez-Gonzalez, Teresa; Lopes, Manuela; Lopes, Luis; Vilar, Rui; Bahillo, José; Varela-Patiño, Purificación

2010-02-01

This in vitro study compared the tooth color and the ultrastructure of internal dental tissues before and after internal bleaching. Sodium perborate was placed in the pulp chamber of endodontically treated molars and sealed with intermediate restorative material. The test samples were stored in a physiologic solution, and the bleaching agent was replaced every 7 days. A control group was used. After 1 month, the colors of the test and control samples were measured with a colorimeter, and the internal surfaces were observed under field emission scanning electron microscopy (FESEM). Statistically significant differences were found between the test and control sample colors. The FESEM ultrastructure analysis of the internal enamel and dentin surfaces did not show any changes after the internal bleaching. The results of the present study show that sodium perborate is effective in bleaching nonvital teeth and does not produce ultrastructural changes in the dental tissues. Copyright 2010 American Association of Endodontists. Published by Elsevier Inc. All rights reserved.

Quantification of metallic nanoparticle morphology with tilt series imaging by transmission electron microscopy

NASA Astrophysics Data System (ADS)

Dutta, Aniruddha; Yuan, Biao; Clukay, Christopher J.; Grabill, Christopher N.; Heinrich, Helge; Bhattacharya, Aniket; Kuebler, Stephen M.

2012-02-01

We report on the quantitative analysis of electrolessly deposited Au and Ag nanoparticles (NPs) on SU8 polymer with the help of High-Angle Annular Dark-Field Scanning Transmission Electron Microscopy (HAADF-STEM) in tilt series. Au NPs act as nucleating agents for the electroless deposition of silver. Au NPs were prepared by attachingAu^3+cations to amine functionalized SU8 polymeric surfaces and then reducing it with aqueous NaBH4. The nanoscale morphology of the deposited NPs on the surface of polymer has been studied from the dark field TEM cross sectional images. Ag NPs were deposited on the cross-linked polymeric surface from a silver citrate solution reduced by hydroquinone. HAADF-STEM enables us to determine the distances between the NPs and their exact locations at and near the surface. The particle distribution, sizes and densities provide us with the data necessary to control the parameters for the development of the electroless deposition technique for emerging nanoscale technologies.

Electrodeposition of Rhodium Nanowires Arrays and Their Morphology-Dependent Hydrogen Evolution Activity

PubMed Central

Zhang, Liqiu; Liu, Lichun; Wang, Hongdan; Shen, Hongxia; Cheng, Qiong; Yan, Chao; Park, Sungho

2017-01-01

This work reports on the electrodeposition of rhodium (Rh) nanowires with a controlled surface morphology synthesized using an anodic aluminum oxide (AAO) template. Vertically aligned Rh nanowires with a smooth and coarse morphology were successfully deposited by adjusting the electrode potential and the concentration of precursor ions and by involving a complexing reagent in the electrolyte solution. Scanning electron microscopy (SEM) and transmission electron microscopy (TEM) analyses were used to follow the morphological evolution of Rh nanowires. As a heterogeneous electrocatalyst for hydrogen evolution reactions (HER), the coarse Rh nanowire array exhibited an enhanced catalytic performance respect to smooth ones due to the larger surface area to mass ratio and the higher density of catalytically active defects, as evidenced by voltammetric measurements and TEM. Results suggest that the morphology of metallic nanomaterials could be readily engineered by electrodeposition. The controlled electrodeposition offers great potential for the development of an effective synthesis tool for heterogeneous catalysts with a superior performance for wide applications. PMID:28467375

In situ electron microscopy of Braille microsystems: photo-actuation of ethylene vinyl acetate/carbon nanotube composites

NASA Astrophysics Data System (ADS)

Czaniková, Klaudia; Krupa, Igor; Račko, Dušan; Šmatko, Vasilij; Campo, Eva M.; Pavlova, Ewa; Omastová, Mária

2015-02-01

The development of new types of tactile displays based on the actuation of composite materials can aid the visually impaired. Micro/nano systems based on ethylene vinyl acetate (EVA) polymeric matrices enriched with multiwalled carbon nanotubes (MWCNT) can produce ensembles capable of light-induced actuation. In this report, we investigate two types of commercial EVA copolymers matrices containing 28 and 50 wt% vinyl-acetate (VA). Non-covalent modification of carbon nanotubes was achieved through a compatibilization technique that appends the pyrenenyl and cholesteryl groups on the carbon nanotubes (CNTs) surface. EVA/MWCNT nanocomposites were prepared by casting from a solution. These composites were shaped into Braille elements using molds. The deformation of the Braille element (BE) under light-emitting diode (LED) illumination was observed for the first time by in situ scanning electron microscopy (SEM). The superior actuation performance promoted by the EVA/MWCNT nanocomposites indicates that these materials will be useful in the future as light-driven micro/nano system actuators.

Biocompatible epoxy modified bio-based polyurethane nanocomposites: mechanical property, cytotoxicity and biodegradation.

PubMed

Dutta, Suvangshu; Karak, Niranjan; Saikia, Jyoti Prasad; Konwar, Bolin Kumar

2009-12-01

Epoxy modified Mesua ferrea L. seed oil (MFLSO) based polyurethane nanocomposites with different weight % of clay loadings (1%, 2.5% and 5%) have been evaluated as biocompatible materials. The nanocomposites were prepared by ex situ solution technique under high mechanical shearing and ultrasonication at room temperature. The partially exfoliated nanocomposites were characterized by Fourier transform infra-red (FTIR), X-ray diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM) techniques. The mechanical properties such as tensile strength and scratch hardness were improved 2 and 5 times, respectively by nanocomposites formation. Even the impact resistance improved a little. The thermostability of the nanocomposites was enhanced by about 40 degrees C. Biodegradation study confirmed 5-10 fold increase in biodegradation rate for the nanocomposites compared to the pristine polymers. All the nanocomposites showed non-cytotoxicity as evident from RBC hemolysis inhibition observed in anti-hemolytic assay carried over the sterilized films. The study reveals that the epoxy modified MFLSO based polyurethane nanocomposites deserve the potential to be applicable as biomaterials.

Evaluation of the antimicrobial activity and cytotoxicity of phytogenic gold nanoparticles

NASA Astrophysics Data System (ADS)

Sreekanth, T. V. M.; Nagajyothi, P. C.; Supraja, N.; Prasad, T. N. V. K. V.

2015-06-01

Among the nanoscale materials, noble metal nanoparticles have been attracting the scientific community due to their unique properties and selectivity in biological applications. In the present investigation, gold nanoparticles (AuNPs) were synthesized using rhizome extract of Dioscorea batatas through a simple, clean, inexpensive and eco-friendly method. Treating 1 mM chloroauric acid (HAuCl4) with the rhizome extract at 50 °C resulted in the formation of AuNPs. The reduction of AuNPs was observed by the color change of the solution from colorless to dark red wine. The synthesized nanoparticles were characterized using the techniques UV-Vis spectrophotometers, Fourier transform infrared spectroscopy, X-ray diffraction, scanning electron microscopy and transmission electron microscopy. Green synthesized AuNPs were found to be toxic against gram-positive and gram-negative bacteria in liquid media. MTT (dimethyl thiazolyl diphenyl tetrazolium salt) assay showed 21.5 % cell inhibition in lower concentration (0.2 mM) and >50 % cell inhibition after 48 h exposure at higher concentrations (0.8-1 mM).

Electrodeposition of Au/Ag bimetallic dendrites assisted by Faradaic AC-electroosmosis flow

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

Ji, Jianlong; Li, Pengwei; Sang, Shengbo, E-mail: sbsang@tyut.edu.cn

2014-03-15

Au/Ag bimetallic dendrites were synthesized successfully from the corresponding aqueous solution via the AC electrodeposition method. Both of the morphologies and compositions could be tuned by the electrolyte concentration and AC frequency. The prepared bimetallic dendrites were characterized by scanning electron microscopy (SEM), energy dispersive X-ray spectrometer (EDS), transmission electron microscopy (TEM) and UV–vis spectroscopy. The underlying dendrite growth mechanism was then proposed in the context of the Directed Electrochemical Nanowires Assembly (DENA) models. Owing to the unscreened voltage dropping in the electrolyte bulk, electromigration dominates the species flux process, and cations tend to accumulate in areas with strong electricmore » field intensity, such as electrode edges. Moreover, Faradaic AC-electro-osmosis (ACEO) flow could increase the effective diffusion layer thickness in these areas during the electrochemical reaction, and leads to dendrite growth. Further Micro-Raman observations illustrated that the Au/Ag bimetallic dendrites exhibited pronounced surface-enhanced Raman scattering (SERS) activity, using 4-mercaptopyridine (4-MP) as model molecules.« less

Nano-textured high sensitivity ion sensitive field effect transistors

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

Hajmirzaheydarali, M.; Sadeghipari, M.; Akbari, M.

2016-02-07

Nano-textured gate engineered ion sensitive field effect transistors (ISFETs), suitable for high sensitivity pH sensors, have been realized. Utilizing a mask-less deep reactive ion etching results in ultra-fine poly-Si features on the gate of ISFET devices where spacing of the order of 10 nm and less is achieved. Incorporation of these nano-sized features on the gate is responsible for high sensitivities up to 400 mV/pH in contrast to conventional planar structures. The fabrication process for this transistor is inexpensive, and it is fully compatible with standard complementary metal oxide semiconductor fabrication procedure. A theoretical modeling has also been presented to predict themore » extension of the diffuse layer into the electrolyte solution for highly featured structures and to correlate this extension with the high sensitivity of the device. The observed ultra-fine features by means of scanning electron microscopy and transmission electron microscopy tools corroborate the theoretical prediction.« less

An analysis of FtsZ assembly using small angle X-ray scattering and electron microscopy.

PubMed

Kuchibhatla, Anuradha; Abdul Rasheed, A S; Narayanan, Janaky; Bellare, Jayesh; Panda, Dulal

2009-04-09

Small angle X-ray scattering (SAXS) was used for the first time to study the self-assembly of the bacterial cell division protein, FtsZ, with three different additives: calcium chloride, monosodium glutamate and DEAE-dextran hydrochloride in solution. The SAXS data were analyzed assuming a model form factor and also by a model-independent analysis using the pair distance distribution function. Transmission electron microscopy (TEM) was used for direct observation of the FtsZ filaments. By sectioning and negative staining with glow discharged grids, very high bundling as well as low bundling polymers were observed under different assembly conditions. FtsZ polymers formed different structures in the presence of different additives and these additives were found to increase the bundling of FtsZ protofilaments by different mechanisms. The combined use of SAXS and TEM provided us a significant insight of the assembly of FtsZ and microstructures of the assembled FtsZ polymers.

Amino acid-functionalized multi-walled carbon nanotubes for improving compatibility with chiral poly(amide-ester-imide) containing L-phenylalanine and L-tyrosine linkages

NASA Astrophysics Data System (ADS)

Abdolmaleki, Amir; Mallakpour, Shadpour; Borandeh, Sedigheh

2013-12-01

Amino acid functionalized multi-walled carbon nanotubes (f-MWCNTs)/poly(amide-ester-imide) (PAEI) composites were fabricated by solution mixing method. Proper functionalization and mixing strategy of MWCNTs provides the best opportunity for better distribution and bonding of nanoparticles to the polymer matrix. MWCNTs have been chemically modified with L-phenylalanine to improve their compatibility with L-phenylalanine based PAEI. Field emission scanning electron microscopy micrographs of composite revealed that f-MWCNTs made a good interaction with polymer chains by wrapping the polymer around them, and transmission electron microscopy results confirmed well dispersion with nano size of f-MWCNTs in the polymer matrix. In addition, thermal analysis showed good enhancement in thermal properties of composites compared to pure polymer. Thermal stability of the composites containing f-MWCNTs was enhanced due to their good dispersion and improved interfacial interaction between the amino acid based PAEI matrix and f-MWCNTs.

Wet etching mechanism and crystallization of indium-tin oxide layer for application in light-emitting diodes

NASA Astrophysics Data System (ADS)

Su, Shui-Hsiang; Kong, Hsieng-Jen; Tseng, Chun-Lung; Chen, Guan-Yu

2018-01-01

In the article, we describe the etching mechanism of indium-tin oxide (ITO) film, which was wet-etched using a solution of hydrochloric acid (HCl) and ferric chloride (FeCl3). The etching mechanism is analyzed at various etching durations of ITO films by scanning electron microscopy (SEM), high-resolution transmission electron microscopy (HR-TEM), and selective area diffraction (SAD) analysis. In comparison with the crystalline phase of SnO2, the In2O3 phase can be more easily transformed to In3+ and can form an inverted conical structure during the etching process. By adjusting the etching duration, the residual ITO is completely removed to show a designed pattern. This is attributed to the negative Gibbs energy of In2O3 transformed to In3+. The result also corresponds to the finding of energy-dispersive X-ray spectroscopy (EDS) analysis that the Sn/In ratio increases with increasing etching duration.

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

PubMed

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

2010-06-15

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

Trimethylamine Sensors Based on Au-Modified Hierarchical Porous Single-Crystalline ZnO Nanosheets

PubMed Central

Zheng, Hanxiong; Sun, Yufeng; Li, Minqiang; Liu, Jinhuai

2017-01-01

It is of great significance for dynamic monitoring of foods in storage or during the transportation process through on-line detecting trimethylamine (TMA). Here, TMA were sensitively detected by Au-modified hierarchical porous single-crystalline ZnO nanosheets (HPSCZNs)-based sensors. The HPSCZNs were synthesized through a one-pot wet-chemical method followed by an annealing treatment. Polyethyleneimine (PEI) was used to modify the surface of the HPSCZNs, and then the PEI-modified samples were mixed with Au nanoparticles (NPs) sol solution. Electrostatic interactions drive Au nanoparticles loading onto the surface of the HPSCZNs. The Au-modified HPSCZNs were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and energy dispersive spectrum (EDS), respectively. The results show that Au-modified HPSCZNs-based sensors exhibit a high response to TMA. The linear range is from 10 to 300 ppb; while the detection limit is 10 ppb, which is the lowest value to our knowledge. PMID:28640226

Chitosan nanocomposite films based on Ag-NP and Au-NP biosynthesis by Bacillus Subtilis as packaging materials.

PubMed

Youssef, Ahmed M; Abdel-Aziz, Mohamed S; El-Sayed, Samah M

2014-08-01

Chitosan-silver (CS-Ag) and Chitosan-gold (CS-Au) nanocomposites films were synthesized by a simple chemical method. A local bacterial isolate identified as Bacillus subtilis ss subtilis was found to be capable to synthesize both silver nanoparticles (Ag-NP) and gold nanoparticles (Au-NP) from silver nitrate (AgNO3) and chloroauric acid (AuCl(4-)) solutions, respectively. The biosynthesis of both Ag-NP and Au-NP characterize using UV/vis spectroscopy, scanning electron microscopy (SEM), transmission electron microscopy (TEM) and X-ray diffraction (XRD), and then added to chitosan by different ratios (0.5, 1 and 2%). The prepared chitosan nanocomposites films were characterize using UV, XRD, SEM and TEM. Moreover, the antibacterial activity of the prepared films was evaluated against gram positive (Staphylococcus aureus) and gram negative bacteria (Pseudomonas aerugenosa), fungi (Aspergillus niger) and yeast (Candida albicans). Therefore, these materials can be potential used as antimicrobial agents in packaging applications. Copyright © 2014 Elsevier B.V. All rights reserved.

Preparation of biocompatible magnetite-carboxymethyl cellulose nanocomposite: characterization of nanocomposite by FTIR, XRD, FESEM and TEM.

PubMed

Habibi, Neda

2014-10-15

The preparation and characterization of magnetite-carboxymethyl cellulose nano-composite (M-CMC) material is described. Magnetite nano-particles were synthesized by a modified co-precipitation method using ferrous chloride tetrahydrate and ferric chloride hexahydrate in ammonium hydroxide solution. The M-CMC nano-composite particles were synthesized by embedding the magnetite nanoparticles inside carboxymethyl cellulose (CMC) using a freshly prepared mixture of Fe3O4 with CMC precursor. Morphology, particle size, and structural properties of magnetite-carboxymethyl cellulose nano-composite was accomplished using X-ray powder diffraction (XRD), transmission electron microscopy (TEM), Fourier transformed infrared (FTIR) and field emission scanning electron microscopy (FESEM) analysis. As a result, magnetite nano-particles with an average size of 35nm were obtained. The biocompatible Fe3O4-carboxymethyl cellulose nano-composite particles obtained from the natural CMC polymers have a potential range of application in biomedical field. Copyright © 2014 Elsevier B.V. All rights reserved.

Chemo-Mechanical Characteristics of Mud Formed from Environmental Dust Particles in Humid Ambient Air

PubMed Central

Hassan, Ghassan; Yilbas, B. S.; Said, Syed A. M.; Al-Aqeeli, N.; Matin, Asif

2016-01-01

Mud formed from environmental dust particles in humid ambient air significantly influences the performance of solar harvesting devices. This study examines the characterization of environmental dust particles and the chemo-mechanics of dry mud formed from dust particles. Analytical tools, including scanning electron microscopy, atomic force microscopy, energy dispersive spectroscopy, particle sizing, and X-ray diffraction, are used to characterize dry mud and dust particles. A micro/nano tribometer is used to measure the tangential force and friction coefficient while tensile tests are carried out to assess the binding forces of dry mud pellets. After dry mud is removed, mud residuals on the glass surface are examined and the optical transmittance of the glass is measured. Dust particles include alkaline compounds, which dissolve in water condensate and form a mud solution with high pH (pH = 7.5). The mud solution forms a thin liquid film at the interface of dust particles and surface. Crystals form as the mud solution dries, thus, increasing the adhesion work required to remove dry mud from the surface. Optical transmittance of the glass is reduced after dry mud is removed due to the dry mud residue on the surface. PMID:27445272

Chemo-Mechanical Characteristics of Mud Formed from Environmental Dust Particles in Humid Ambient Air.

PubMed

Hassan, Ghassan; Yilbas, B S; Said, Syed A M; Al-Aqeeli, N; Matin, Asif

2016-07-22

Mud formed from environmental dust particles in humid ambient air significantly influences the performance of solar harvesting devices. This study examines the characterization of environmental dust particles and the chemo-mechanics of dry mud formed from dust particles. Analytical tools, including scanning electron microscopy, atomic force microscopy, energy dispersive spectroscopy, particle sizing, and X-ray diffraction, are used to characterize dry mud and dust particles. A micro/nano tribometer is used to measure the tangential force and friction coefficient while tensile tests are carried out to assess the binding forces of dry mud pellets. After dry mud is removed, mud residuals on the glass surface are examined and the optical transmittance of the glass is measured. Dust particles include alkaline compounds, which dissolve in water condensate and form a mud solution with high pH (pH = 7.5). The mud solution forms a thin liquid film at the interface of dust particles and surface. Crystals form as the mud solution dries, thus, increasing the adhesion work required to remove dry mud from the surface. Optical transmittance of the glass is reduced after dry mud is removed due to the dry mud residue on the surface.

Room-temperature synthesis of Zn(0.80)Cd(0.20)S solid solution with a high visible-light photocatalytic activity for hydrogen evolution.

PubMed

Wang, Dong-Hong; Wang, Lei; Xu, An-Wu

2012-03-21

Visible light photocatalytic H(2) production from water splitting is of great significance for its potential applications in converting solar energy into chemical energy. In this study, a series of Zn(1-x)Cd(x)S solid solutions with a nanoporous structure were successfully synthesized via a facile template-free method at room temperature. The obtained solid solutions were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM), ultraviolet-visible (UV-vis) diffuse reflectance spectroscopy, X-ray photoelectron spectroscopy (XPS), energy-dispersive X-ray spectroscopy (EDS) and N(2) adsorption-desorption analysis. The solid solutions show efficient photocatalytic activity for H(2) evolution from aqueous solutions containing sacrificial reagents S(2-) and SO(3)(2-) under visible-light irradiation without a Pt cocatalyst, and loading of the Pt cocatalyst further improves the visible-light photocatalytic activity. The optimal photocatalyst with x = 0.20 prepared at pH = 7.3 displays the highest activity for H(2) evolution. The bare and 0.25 wt% Pt loaded Zn(0.80)Cd(0.20)S nanoparticles exhibit a high H(2) evolution rate of 193 μmol h(-1) and 458 μmol h(-1) under visible-light irradiation (λ ≥ 420 nm), respectively. In addition, the bare and 0.25 wt% Pt loaded Zn(0.80)Cd(0.20)S catalysts show a high H(2) evolution rate of 252 and 640 μmol h(-1) under simulated solar light irradiation, respectively. Moreover, the Zn(0.80)Cd(0.20)S catalyst displays a high photocatalytic stability for H(2) evolution under long-term light irradiation. The incorporation of Cd in the solid solution leads to the visible light absorption, and the high content of Zn in the solid solution results in a relatively negative conduction band, a modulated band gap and a rather wide valence bandwidth, which are responsible for the excellent photocatalytic performance of H(2) production and for the high photostability. This journal is © The Royal Society of Chemistry 2012

New hardware and workflows for semi-automated correlative cryo-fluorescence and cryo-electron microscopy/tomography.

PubMed

Schorb, Martin; Gaechter, Leander; Avinoam, Ori; Sieckmann, Frank; Clarke, Mairi; Bebeacua, Cecilia; Bykov, Yury S; Sonnen, Andreas F-P; Lihl, Reinhard; Briggs, John A G

2017-02-01

Correlative light and electron microscopy allows features of interest defined by fluorescence signals to be located in an electron micrograph of the same sample. Rare dynamic events or specific objects can be identified, targeted and imaged by electron microscopy or tomography. To combine it with structural studies using cryo-electron microscopy or tomography, fluorescence microscopy must be performed while maintaining the specimen vitrified at liquid-nitrogen temperatures and in a dry environment during imaging and transfer. Here we present instrumentation, software and an experimental workflow that improves the ease of use, throughput and performance of correlated cryo-fluorescence and cryo-electron microscopy. The new cryo-stage incorporates a specially modified high-numerical aperture objective lens and provides a stable and clean imaging environment. It is combined with a transfer shuttle for contamination-free loading of the specimen. Optimized microscope control software allows automated acquisition of the entire specimen area by cryo-fluorescence microscopy. The software also facilitates direct transfer of the fluorescence image and associated coordinates to the cryo-electron microscope for subsequent fluorescence-guided automated imaging. Here we describe these technological developments and present a detailed workflow, which we applied for automated cryo-electron microscopy and tomography of various specimens. Copyright © 2016 The Authors. Published by Elsevier Inc. All rights reserved.

Scanning ultrafast electron microscopy

PubMed Central

Yang, Ding-Shyue; Mohammed, Omar F.; Zewail, Ahmed H.

2010-01-01

Progress has been made in the development of four-dimensional ultrafast electron microscopy, which enables space-time imaging of structural dynamics in the condensed phase. In ultrafast electron microscopy, the electrons are accelerated, typically to 200 keV, and the microscope operates in the transmission mode. Here, we report the development of scanning ultrafast electron microscopy using a field-emission-source configuration. Scanning of pulses is made in the single-electron mode, for which the pulse contains at most one or a few electrons, thus achieving imaging without the space-charge effect between electrons, and still in ten(s) of seconds. For imaging, the secondary electrons from surface structures are detected, as demonstrated here for material surfaces and biological specimens. By recording backscattered electrons, diffraction patterns from single crystals were also obtained. Scanning pulsed-electron microscopy with the acquired spatiotemporal resolutions, and its efficient heat-dissipation feature, is now poised to provide in situ 4D imaging and with environmental capability. PMID:20696933

Hydrogen production from water-glucose solution over NiO/La-NaTaO3 photocatalyst

NASA Astrophysics Data System (ADS)

Mardian, R.; Husin, H.; Pontas, K.; Zaki, M.; Asnawi, T. M.; Ahmadi

2018-03-01

This paper reports the evaluation of La-NaTaO3 photocatalyst performance in producing hydrogen from water-glucose solution. The main goal of the studies is to investigate the influence of glucose as a sacrificial reagent on the photocatalytic efficiency in water splitting reactions under ultraviolet (UV) irradiation. Photocatalyst has been fabricated via sol-gel method and being confirmed using x-ray diffraction (XRD) and scanning electron microscopy (SEM). Nickel loaded La-NaTaO3 photocatalyst are prepared by impregnation method. It was observed that the prepared photocatalysts displayed particle sizes in the 30-250 nm range with orthorhombic structure. Their photocatalytic activity for hydrogen production via water splitting was conducted in a Pyrex glass reactor under UV light irradiation. The aqueous solution contained glucose employed as a renewable organic scavenger. A significant improvement in hydrogen production was observed in glucose-water mixtures and NiO loaded photocatalyst. The prepared La-NaTaO3 showed that the highest activity for hydrogen generation of 35.1 mmol h-1.g-1 was obtained at 0.10 mol.L-1 glucose and 0.3 wt.% NiO. This suggests the important role played by the glucose as electron donor and loading nickel on La-NaTaO3 as a cocatalyst increasing electron storage and suppressing electron-hole recombination.

Effect of cold rolling on the microstructural evolution of new β-typed Ti–6Mo–6V–5Cr–3Sn–2.5Zr alloys

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

Choi, Gwnaghyo; Lee, Kwangmin, E-mail: kmlee@jnu.a

A Ti–6Mo–6V–5Cr–3Sn–2.5Zr (wt.%) alloy was designed as a new metastable β-Ti alloy. The effect that cold rolling had on the microstructural evolution of the material was investigated via optical microscopy (OM), X-ray diffraction (XRD), electron back-scattered diffraction (EBSD) and transmission electron microscopy (TEM) measurements. A single β phase formed in the alloy after solution treatment at 780 °C for 30 min followed by water quenching. The solution-treated alloy was cold rolled with thickness reductions of 10%, 30%, 50% and 70%, and the hardness values increased as the thickness of the specimen decreased. The textures of the cold rolled specimen weremore » characterized according to the 〈110〉 partial parallel to the rolling direction as the rolling reduction increased. The crystallographic orientation showed principal α-fiber textures for (111)〈110〉 and (112)〈110〉. The cold deformation led to the appearance of martensite α″ phases, particularly stress-induced martensite (SIM) α″ phases. - Highlights: • Effect of cold rolling on new β-typed Ti-6Mo-6V-5Cr-3Sn-2.5Zr alloy was studied. • A single β phase was obtained after solution treatment at 780 °C for 30 min. • α-Fiber textures became dominated with the increase in cold rolling reduction. • A stress-induced α″ martensite was caused by cold rolling.« less

Micro/Nano Multilayered Scaffolds of PLGA and Collagen by Alternately Electrospinning for Bone Tissue Engineering

NASA Astrophysics Data System (ADS)

Kwak, Sanghwa; Haider, Adnan; Gupta, Kailash Chandra; Kim, Sukyoung; Kang, Inn-Kyu

2016-07-01

The dual extrusion electrospinning technique was used to fabricate multilayered 3D scaffolds by stacking microfibrous meshes of poly(lactic acid-co-glycolic acid) (PLGA) in alternate fashion to micro/nano mixed fibrous meshes of PLGA and collagen. To fabricate the multilayered scaffold, 35 wt% solution of PLGA in THF-DMF binary solvent (3:1) and 5 wt% solution of collagen in hexafluoroisopropanol (HFIP) with and without hydroxyapatite nanorods (nHA) were used. The dual and individual electrospinning of PLGA and collagen were carried out at flow rates of 1.0 and 0.5 mL/h, respectively, at an applied voltage of 20 kV. The density of collagen fibers in multilayered scaffolds has controlled the adhesion, proliferation, and osteogenic differentiation of MC3T3-E1 cells. The homogeneous dispersion of glutamic acid-modified hydroxyapatite nanorods (nHA-GA) in collagen solution has improved the osteogenic properties of fabricated multilayered scaffolds. The fabricated multilayered scaffolds were characterized using FT-IR, X-ray photoelectron spectroscopy, and transmission electron microscopy (TEM). The scanning electron microscopy (FE-SEM) was used to evaluate the adhesion and spreads of MC3T3-E1 cells on multilayered scaffolds. The activity of MC3T3-E1 cells on the multilayered scaffolds was evaluated by applying MTT, alkaline phosphatase, Alizarin Red, von Kossa, and cytoskeleton F-actin assaying protocols. The micro/nano fibrous PLGA-Col-HA scaffolds were found to be highly bioactive in comparison to pristine microfibrous PLGA and micro/nano mixed fibrous PLGA and Col scaffolds.

Serial block face scanning electron microscopy--the future of cell ultrastructure imaging.

PubMed

Hughes, Louise; Hawes, Chris; Monteith, Sandy; Vaughan, Sue

2014-03-01

One of the major drawbacks in transmission electron microscopy has been the production of three-dimensional views of cells and tissues. Currently, there is no one suitable 3D microscopy technique that answers all questions and serial block face scanning electron microscopy (SEM) fills the gap between 3D imaging using high-end fluorescence microscopy and the high resolution offered by electron tomography. In this review, we discuss the potential of the serial block face SEM technique for studying the three-dimensional organisation of animal, plant and microbial cells.

Applications of microscopy to genetic therapy of cystic fibrosis and other human diseases.

PubMed

Moninger, Thomas O; Nessler, Randy A; Moore, Kenneth C

2006-01-01

Gene therapy has become an extremely important and active field of biomedical research. Microscopy is an integral component of this effort. This chapter presents an overview of imaging techniques used in our facility in support of cystic fibrosis gene therapy research. Instrumentation used in these studies includes light and confocal microscopy, transmission electron microscopy, and scanning electron microscopy. Techniques outlined include negative staining, cryo-electron microscopy, three-dimentional reconstruction, enzyme cytochemistry, immunocytochemistry, and fluorescence imaging.