Advanced microscopy of star-shaped gold nanoparticles and their adsorption-uptake by macrophages

PubMed Central

Plascencia-Villa, Germán; Bahena, Daniel; Rodríguez, Annette R.; Ponce, Arturo; José-Yacamán, Miguel

2013-01-01

Metallic nanoparticles have diverse applications in biomedicine, as diagnostics, image contrast agents, nanosensors and drug delivery systems. Anisotropic metallic nanoparticles possess potential applications in cell imaging and therapy+diagnostics (theranostics), but controlled synthesis and growth of these anisotropic or branched nanostructures has been challenging and usually require use of high concentrations of surfactants. Star-shaped gold nanoparticles were synthesized in high yield through a seed mediated route using HEPES as a precise shape-directing capping agent. Characterization was performed using advanced electron microscopy techniques including atomic resolution TEM, obtaining a detailed characterization of nanostructure and atomic arrangement. Spectroscopy techniques showed that particles have narrow size distribution, monodispersity and high colloidal stability, with absorbance into NIR region and high efficiency for SERS applications. Gold nanostars showed to be biocompatible and efficiently adsorbed and internalized by macrophages, as revealed by advanced FE-SEM and backscattered electron imaging techniques of complete unstained uncoated cells. Additionally, low voltage STEM and X-ray microanalysis revealed the ultra-structural location and confirmed stability of nanoparticles after endocytosis with high spatial resolution. PMID:23443314

Characterization of barium strontium titanate thin films on sapphire substrate prepared via RF magnetron sputtering system

NASA Astrophysics Data System (ADS)

Jamaluddin, F. W.; Khalid, M. F. Abdul; Mamat, M. H.; Zoolfakar, A. S.; Zulkefle, M. A.; Rusop, M.; Awang, Z.

2018-05-01

Barium Strontium Titanate (Ba0.5Sr0.5TiO3) is known to have a high dielectric constant and low loss at microwave frequencies. These unique features are useful for many electronic applications. This paper focuses on material characterization of BST thin films deposited on sapphire substrate by RF magnetron sputtering system. The sample was then annealed at 900 °C for two hours. Several methods were used to characterize the structural properties of the material such as X-ray diffraction (XRD) and atomic force microscopy (AFM). Field emission scanning electron microscopy (FESEM) was used to analyze the surface morphology of the thin film. From the results obtained, it can be shown that the annealed sample had a rougher surface and better crystallinity as compared to as-deposited sample.

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

PubMed

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

2010-11-01

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

In Vitro Assessment of Early Bacterial Activity on Micro/Nanostructured Ti6Al4V Surfaces.

PubMed

Valdez-Salas, Benjamin; Beltrán-Partida, Ernesto; Castillo-Uribe, Sandra; Curiel-Álvarez, Mario; Zlatev, Roumen; Stoytcheva, Margarita; Montero-Alpírez, Gisela; Vargas-Osuna, Lidia

2017-05-18

It is imperative to understand and systematically compare the initial interactions between bacteria genre and surface properties. Thus, we fabricated a flat, anodized with 80 nm TiO₂ nanotubes (NTs), and a rough Ti6Al4V surface. The materials were characterized using field-emission scanning electron microscopy (FE-SEM), energy dispersive X-ray spectroscopy (EDX) and atomic force microscopy (AFM). We cultured in vitro Staphylococcus epidermidis ( S. epidermidis ) and Pseudomonas aeruginosa ( P. aeruginosa ) to evaluate the bacterial-surface behavior by FE-SEM and viability calculation. In addition, the initial effects of human osteoblasts were tested on the materials. Gram-negative bacteria showed promoted adherence and viability over the flat and rough surface, while NTs displayed opposite activity with altered morphology. Gram-positive bacteria illustrated similar cellular architecture over the surfaces but with promoted surface adhesion bonds on the flat alloy. Rough surfaces supported S. epidermidis viability, whilst NTs exhibited lower vitality. NTs advocated promoted better osteoblast organization with enhanced vitality. Gram-positive bacteria suggested preferred adhesion capability over flat and carbon-rich surfaces. Gram-negative bacteria were strongly disturbed by NTs but largely stimulated by flat and rough materials. Our work proposed that the chemical profile of the material surface and the bacterial cell wall characteristics might play an important role in the bacteria-surface interactions.

Structural, electronic structure and antibacterial properties of graphene-oxide nano-sheets

NASA Astrophysics Data System (ADS)

Sharma, Aditya; Varshney, Mayora; Nanda, Sitansu Sekhar; Shin, Hyun Joon; Kim, Namdong; Yi, Dong Kee; Chae, Keun-Hwa; Ok Won, Sung

2018-04-01

Correlation between the structural/electronic structure properties and bio-activity of graphene-based materials need to be thoroughly evaluated before their commercial implementation in the health and environment precincts. To better investigate the local hybridization of sp2/sp3 orbitals of the functional groups of graphene-oxide (GO) and their execution in the antimicrobial mechanism, we exemplify the antibacterial activity of GO sheets towards the Escherichia coli bacteria (E. coli) by applying the field-emission scanning electron microscopy (FESEM), near edge X-ray absorption fine structure (NEXAFS) and scanning transmission X-ray microscope (STXM) techniques. C K-edge and O K-edge NEXAFS spectra have revealed lesser sp2 carbon atoms in the aromatic ring and attachment of functional oxygen groups at GO sheets. Entrapment of E. coli bacteria by GO sheets is evidenced by FESEM investigations and has also been corroborated by nano-scale imaging of bacteria using the STXM. Spectroscopy evidence of functional oxygen moieties with GO sheets and physiochemical entrapment of E. coli bacteria have assisted us to elaborate the mechanism of cellular oxidative stress-induced disruption of bacterial membrane.

Effect of copper and nickel doping on the optical and structural properties of ZnO

NASA Astrophysics Data System (ADS)

Muǧlu, G. Merhan; Sarıtaş, S.; ćakıcı, T.; Şakar, B.; Yıldırım, M.

2017-02-01

The present study is focused on the Cu doped ZnO and Ni doped ZnO dilute magnetic semiconductor thin films. ZnO:Cu and ZnO:Ni thin films were grown by Chemically Spray Pyrolysis (CSP) method on glass substrates. Optical analysis of the films was done spectral absorption and transmittance measurements by UV-Vis double beam spectrophotometer technique. The structure, morphology, topology and elemental analysis of ZnO:Cu and ZnO:Ni dilute magnetic thin films were investigated by X-ray diffraction (XRD), Raman Analysis, field emission scanning electron microscopy (FE-SEM), energy-dispersive X-ray spectroscopy (EDX), atomic force microscopy (AFM) techniques, respectively. Also The magnetic properties of the ZnO:Ni thin film was investigated by vibrating sample magnetometer (VSM) method. VSM measurements of ZnO:Ni thin film showed that the ferromagnetic behavior.

The Effect of Sodium Dodecyl Sulfate on PEDOT:PSS and Its Application to Organic Photovoltaic Solar Cells.

PubMed

Hwang, Ki-Hwan; Seo, Hyeon Jin; Nam, Sang-Hun; Boo, Jin-Hyo

2015-10-01

Recently, the use of PSS in flexible device electrodes has been reported. PSS treatment consists of a step in which a small amount of surfactant is added to enhance the adhesion between PSS and the substrate or TCO materials. However, basic research into the effect of the surfactant is lacking. We studied the effects of sodium dodecyl sulfate (SDS) at controlled concentrations in aqueous PSS solution and that it enhanced the conductivity in the mixed thin films with surfactant and PSS. The thin films were prepared by the spin coating method. To study the structural effects on the resulting electrical properties, the thin films were investigated by FE-SEM (Field Emission Scanning Electron Microscopy) and AFM (Atomic Force Microscopy). At the same time, the electrical properties were investigated using a 4-point probe and solar simulator.

Au sensitized ZnO nanorods for enhanced liquefied petroleum gas sensing properties

NASA Astrophysics Data System (ADS)

Nakate, U. T.; Bulakhe, R. N.; Lokhande, C. D.; Kale, S. N.

2016-05-01

The zinc oxide (ZnO) nanorods have grown on glass substrate by spray pyrolysis deposition (SPD) method using zinc acetate solution. The phase formation, surface morphology and elemental composition of ZnO films have been investigated using X-ray diffraction, field emission scanning electron microscopy (FE-SEM), atomic force microscopy (AFM) and energy dispersive X-ray (EDX) techniques. The liquefied petroleum gas (LPG) sensing response was remarkably improved by sensitization of gold (Au) surface noble metal on ZnO nanorods film. Maximum LPG response of 21% was observed for 1040 ppm of LPG, for pure ZnO nanorods sample. After Au sensitization on ZnO nanorods film sample, the LPG response greatly improved up to 48% at operating temperature 623 K. The improved LPG response is attributed Au sensitization with spill-over mechanism. Proposed model for LPG sensing mechanism discussed.

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

NASA Astrophysics Data System (ADS)

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

2012-05-01

Described here is how to synthesize one-dimensional ammonium tungsten bronze ((NH4)xWO3) by a facile solvothermal approach in which ethylene glycol and acetic acid were employed as solvents and ammonium paratungstate was used as a starting material, as well as how to develop the near infrared absorption properties of (NH4)xWO3 nanorods for application as a solar light control filter. The as-obtained product was characterized by field emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), thermogravimetry (TG), atomic force microscope (AFM) and UV-Vis-NIR spectra. The SEM and TEM images clearly revealed that the obtained sample possessed rod/fiber-like morphologies with diameters around 120 nm. As determined by UV-Vis-NIR optical measurement, the thin film consisted of (NH4)xWO3 nanoparticles, which can selectively transmit most visible lights, but strongly absorb the near-infrared (NIR) lights and ultraviolet rays. These interesting optical properties make the (NH4)xWO3 nanorods suitable for the solar control windows.Described here is how to synthesize one-dimensional ammonium tungsten bronze ((NH4)xWO3) by a facile solvothermal approach in which ethylene glycol and acetic acid were employed as solvents and ammonium paratungstate was used as a starting material, as well as how to develop the near infrared absorption properties of (NH4)xWO3 nanorods for application as a solar light control filter. The as-obtained product was characterized by field emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), thermogravimetry (TG), atomic force microscope (AFM) and UV-Vis-NIR spectra. The SEM and TEM images clearly revealed that the obtained sample possessed rod/fiber-like morphologies with diameters around 120 nm. As determined by UV-Vis-NIR optical measurement, the thin film consisted of (NH4)xWO3 nanoparticles, which can selectively transmit most visible lights, but strongly absorb the near-infrared (NIR) lights and ultraviolet rays. These interesting optical properties make the (NH4)xWO3 nanorods suitable for the solar control windows. Electronic supplementary information (ESI) available. See DOI: 10.1039/c2nr30612c

Field emission scanning electron microscopy (FE-SEM) as an approach for nanoparticle detection inside cells.

PubMed

Havrdova, M; Polakova, K; Skopalik, J; Vujtek, M; Mokdad, A; Homolkova, M; Tucek, J; Nebesarova, J; Zboril, R

2014-12-01

When developing new nanoparticles for bio-applications, it is important to fully characterize the nanoparticle's behavior in biological systems. The most common techniques employed for mapping nanoparticles inside cells include transmission electron microscopy (TEM) and scanning transmission electron microscopy (STEM). These techniques entail passing an electron beam through a thin specimen. STEM or TEM imaging is often used for the detection of nanoparticles inside cellular organelles. However, lengthy sample preparation is required (i.e., fixation, dehydration, drying, resin embedding, and cutting). In the present work, a new matrix (FTO glass) for biological samples was used and characterized by field emission scanning electron microscopy (FE-SEM) to generate images comparable to those obtained by TEM. Using FE-SEM, nanoparticle images were acquired inside endo/lysosomes without disruption of the cellular shape. Furthermore, the initial steps of nanoparticle incorporation into the cells were captured. In addition, the conductive FTO glass endowed the sample with high stability under the required accelerating voltage. Owing to these features of the sample, further analyses could be performed (material contrast and energy-dispersive X-ray spectroscopy (EDS)), which confirmed the presence of nanoparticles inside the cells. The results showed that FE-SEM can enable detailed characterization of nanoparticles in endosomes without the need for contrast staining or metal coating of the sample. Images showing the intracellular distribution of nanoparticles together with cellular morphology can give important information on the biocompatibility and demonstrate the potential of nanoparticle utilization in medicine. Copyright © 2014 Elsevier Ltd. All rights reserved.

Au particle formation on the electron beam induced membrane

NASA Astrophysics Data System (ADS)

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

2017-02-01

Recently the single molecules such as protein and deoxyribonucleic acid (DNA) have been successfully characterized by using a portable solidstate nanopore (MinION) with an electrical detection technique. However, there have been several reports about the high error rates of the fabricated nanopore device, possibly due to an electrical double layer formed inside the pore channel. The current DNA sequencing technology utilized is based on the optical detection method. In order to utilize the current optical detection technique, we will present the formation of the Au nano-pore with Au particle under the various electron beam irradiations. In order to provide the diffusion of Au atoms, a 2 keV electron beam irradiation has been performed During electron beam irradiations by using field emission scanning electron microscopy (FESEM), Au and C atoms would diffuse together and form the binary mixture membrane. Initially, the Au atoms diffused in the membrane are smaller than 1 nm, below the detection limit of the transmission electron microscopy (TEM), so that we are unable to observe the Au atoms in the formed membrane. However, after several months later, the Au atoms became larger and larger with expense of the smaller particles: Ostwald ripening. Furthermore, we also observe the Au crystalline lattice structure on the binary Au-C membrane. The formed Au crystalline lattice structures were constantly changing during electron beam imaging process due to Spinodal decomposition; the unstable thermodynamic system of Au-C binary membrane. The fabricated Au nanopore with an Au nanoparticle can be utilized as a single molecule nanobio sensor.

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

PubMed

Guerra, I; Cardell, C

2015-10-01

The novel Structural Chemical Analyser (hyphenated Raman spectroscopy and scanning electron microscopy equipped with an X-ray detector) is gaining popularity since it allows 3-D morphological studies and elemental, molecular, structural and electronic analyses of a single complex micro-sized sample without transfer between instruments. However, its full potential remains unexploited in painting heritage where simultaneous identification of inorganic and organic materials in paintings is critically yet unresolved. Despite benefits and drawbacks shown in literature, new challenges have to be faced analysing multifaceted paint specimens. SEM-Structural Chemical Analyser systems differ since they are fabricated ad hoc by request. As configuration influences the procedure to optimize analyses, likewise analytical protocols have to be designed ad hoc. This paper deals with the optimization of the analytical procedure of a Variable Pressure Field Emission scanning electron microscopy equipped with an X-ray detector Raman spectroscopy system to analyse historical paint samples. We address essential parameters, technical challenges and limitations raised from analysing paint stratigraphies, archaeological samples and loose pigments. We show that accurate data interpretation requires comprehensive knowledge of factors affecting Raman spectra. We tackled: (i) the in-FESEM-Raman spectroscopy analytical sequence, (ii) correlations between FESEM and Structural Chemical Analyser/laser analytical position, (iii) Raman signal intensity under different VP-FESEM vacuum modes, (iv) carbon deposition on samples under FESEM low-vacuum mode, (v) crystal nature and morphology, (vi) depth of focus and (vii) surface-enhanced Raman scattering effect. We recommend careful planning of analysis strategies prior to research which, although time consuming, guarantees reliable results. The ultimate goal of this paper is to help to guide future users of a FESEM-Structural Chemical Analyser system in order to increase applications. © 2015 The Authors Journal of Microscopy © 2015 Royal Microscopical Society.

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

PubMed

Hatami, Mehdi

2018-06-01

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

Excimer laser annealing of NiTi shape memory alloy thin film

NASA Astrophysics Data System (ADS)

Xie, Qiong; Huang, Weimin; Hong, Ming Hui; Song, Wendong; Chong, Tow Chong

2003-02-01

NiTi Shape Memory Alloy (SMA) is with great potential for actuation in microsystems. It is particularly suitable for medical applications due to its excellent biocompatibility. In MEMS, local annealing of SMA is required in the process of fabrication. In this paper, local annealing of Ni52Ti48 SMA with excimer laser is proposed for the first time. The Ni52Ti48 thin film in a thickness of 5 μm was deposited on Si (100) wafer by sputtering at room temperature. After that, the thin film was annealed by excimer laser (248nm KrF laser) for the first time. Field-Emission Scanning Electron Microscopy (FESEM) and Atomic Force Microscopy (AFM) were used to characterize the surface profile of the deposited film after laser annealing. The phase transformation was measured by Differential Scanning Calorimeter (DSC) test. It is concluded that NiTi film sputtering on Si(100) substrate at room temperature possesses phase transformation after local laser annealing but with cracks.

A Comprehensive Study of the Polypropylene Fiber Reinforced Fly Ash Based Geopolymer

PubMed Central

Ranjbar, Navid; Mehrali, Mehdi; Behnia, Arash; Javadi Pordsari, Alireza; Mehrali, Mohammad; Alengaram, U. Johnson; Jumaat, Mohd Zamin

2016-01-01

As a cementitious material, geopolymers show a high quasi-brittle behavior and a relatively low fracture energy. To overcome such a weakness, incorporation of fibers to a brittle matrix is a well-known technique to enhance the flexural properties. This study comprehensively evaluates the short and long term impacts of different volume percentages of polypropylene fiber (PPF) reinforcement on fly ash based geopolymer composites. Different characteristics of the composite were compared at fresh state by flow measurement and hardened state by variation of shrinkage over time to assess the response of composites under flexural and compressive load conditions. The fiber-matrix interface, fiber surface and toughening mechanisms were assessed using field emission scan electron microscopy (FESEM) and atomic force microscopy (AFM). The results show that incorporation of PPF up to 3 wt % into the geopolymer paste reduces the shrinkage and enhances the energy absorption of the composites. While, it might reduce the ultimate flexural and compressive strength of the material depending on fiber content. PMID:26807825

A Comprehensive Study of the Polypropylene Fiber Reinforced Fly Ash Based Geopolymer.

PubMed

Ranjbar, Navid; Mehrali, Mehdi; Behnia, Arash; Javadi Pordsari, Alireza; Mehrali, Mohammad; Alengaram, U Johnson; Jumaat, Mohd Zamin

2016-01-01

As a cementitious material, geopolymers show a high quasi-brittle behavior and a relatively low fracture energy. To overcome such a weakness, incorporation of fibers to a brittle matrix is a well-known technique to enhance the flexural properties. This study comprehensively evaluates the short and long term impacts of different volume percentages of polypropylene fiber (PPF) reinforcement on fly ash based geopolymer composites. Different characteristics of the composite were compared at fresh state by flow measurement and hardened state by variation of shrinkage over time to assess the response of composites under flexural and compressive load conditions. The fiber-matrix interface, fiber surface and toughening mechanisms were assessed using field emission scan electron microscopy (FESEM) and atomic force microscopy (AFM). The results show that incorporation of PPF up to 3 wt % into the geopolymer paste reduces the shrinkage and enhances the energy absorption of the composites. While, it might reduce the ultimate flexural and compressive strength of the material depending on fiber content.

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

NASA Astrophysics Data System (ADS)

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

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

Nanostructure of aluminium (Al) - Doped zinc oxide (AZO) thin films

NASA Astrophysics Data System (ADS)

Hussin, Rosniza; Husin, M. Asri

2017-12-01

Aluminium (Al)-doped Zinc Oxide (ZnO) was deposited on glass substrates by using the sol-gel dip coating technique. Next, AZO sol-gel solution was produced via sol-gel method. Al was used as doped element with molar ratios of 1%, 2%, and 3%, while the calcination temperatures were set at 400°C, 500°C, and 600°C for 2 hours. In fact, characterization was carried out in order to determine the effect of calcination temperature and molar ratio of doping by using several techniques, such as X-Ray Diffraction (XRD), Atomic Force Microscopy (AFM), Field Emission Scanning Electron Microscopy (FESEM), and Ultraviolet-Visible spectroscopy (UV-Vis). XRD was performed to investigate the crystal structure in which the ZnO was in wurtzite hexagonal form. Next, Energy Dispersive Spectroscopy (EDS) was used to determine the composition of thin films where the result revealed the existence of zinc, oxygen, and aluminium. The roughness of the deposited film was later measured by using the AFM approach where the findings indicated increment in RMS from 8.496 nm to 35.883 nm as the temperature was increased. Additionally, FESEM was carried out to look into the microstructure surfaces of the deposited AZO thin film for increased temperature caused the particle to grow bigger for all molar ratio of dopant. Lastly, UV-Vis was conducted to study the optical properties of AZO, in which the result demonstrated that AZO thin film possessed the highest transmittance percentage among all samples above 90% with band gap value that ranged from 3.25 eV to 3.32 eV.

Fabrication of polyamide thin-film nanocomposite membranes with enhanced surface charge for nitrate ion removal from water resources.

PubMed

Ghaee, A; Zerafat, M M; Askari, P; Sabbaghi, S; Sadatnia, B

2017-03-01

Exclusion due to membrane surface charge is considered as one of the main separation mechanisms occurring in charged membranes, which can be varied through various approaches to affect membrane rejection performance. In this study, thin-film composite (TFC) polyamide (PA) membranes were fabricated via interfacial polymerization of m-phenylenediamine (m-PDA) and 2,4-diaminobenzene sulfonic acid with trimesoyl chloride (TMC) on a polysulfone sub-layer. The ability of the prepared membrane to remove nitrate ions from water resources has been investigated. In order to improve membrane permeability, zeolite-PA thin film nanocomposite (TFN) membranes were fabricated by incorporating natural zeolite nanoparticles obtained through ball milling of an Iranian natural zeolite powder in the interfacial polymerization process. The size, morphology and specific surface area of the as-obtained nanozeolite were characterized using particle size analysis, FE-SEM and BET. The functional groups, morphology and surface charge of the membrane were characterized using ATR-FTIR, SEM and zeta potential analyses. Also, field-emission scanning electron microscopy (FE-SEM) and energy dispersive X-ray spectroscopy (EDS) were used to determine the distribution of nanozeolite in TFN membranes. The influence of zeolite addition to surface roughness was accessed by atomic force microscopy. The performance of TFC and TFN membranes was evaluated in terms of pure water flux and nitrate rejection. The results showed that in case of sulfonated diamine, nitrate ions rejection was enhanced from 63% to 85% which could be attributed to surface charge enhancement. TFN permeability was almost doubled by the addition of nanozeolite.

Field-emission scanning electron microscopy and energy-dispersive x-ray analysis to understand the role of tannin-based dyes in the degradation of historical wool textiles.

PubMed

Restivo, Annalaura; Degano, Ilaria; Ribechini, Erika; Pérez-Arantegui, Josefina; Colombini, Maria Perla

2014-10-01

An innovative approach, combining field-emission scanning electron microscopy (FESEM) with energy dispersive X-ray spectroscopy (EDX) analysis, is presented to investigate the degradation mechanisms affecting tannin-dyed wool. In fact, tannin-dyed textiles are more sensitive to degradation then those dyed with other dyestuffs, even in the same conservation conditions. FESEM-EDX was first used to study a set of 48 wool specimens (artificially aged) dyed with several raw materials and mordants, and prepared according to historical dyeing recipes. EDX analysis was performed on the surface of wool threads and on their cross-sections. In addition, in order to validate the model formulated by the analysis of reference materials, several samples collected from historical and archaeological textiles were subjected to FESEM-EDX analysis. FESEM-EDX investigations enabled us to reveal the correlation between elemental composition and morphological changes. In addition, aging processes were clarified by studying changes in the elemental composition of wool from the protective cuticle to the fiber core in cross-sections. Morphological and elemental analysis of wool specimens and of archaeological and historical textiles showed that the presence of tannins increases wool damage, primarily by causing a sulfur decrease and fiber oxidation.

Novel approach for extraction of quercetin using molecular imprinted membranes

NASA Astrophysics Data System (ADS)

Kamarudin, Siti Fatimah; Ahmad, Mohd Noor; Dzahir, Irfan Hatim Mohamed; Nasir, Azalina Mohamed; Ishak, Noorhidayah; Halim, Nurul Farhanah

2017-12-01

Quercetin imprinted membrane (QIM) was synthesized and applied for the extraction of quercetin. The quercetin imprinted membranes (QIM) were fabricated through a non-covalent approach via surface thermal polymerization. Polyvinylidene fluoride (PVDF) microfiltration membrane was used as a support to improve mechanical stability of the membrane. The thin imprinted layer was formed by copolymerization of acrylamide (AA) as functional monomer and ethylene glycol dimethacrylate (EGDMA) as crosslinker in the presence of quercetin as template in tetrahydrofuran (THF) solution. The Atomic Force Microscopy (AFM) and Field Emission Scanning Electron Microscope (FESEM) were used to visualize the surface of membrane. Batch rebinding and binding kinetic experiments proved that the binding properties of the QIM are higher than non-imprinted membranes (NIM). QIM also have higher selectivity towards quercetin compared to sinensetin and rosmarinic acid.

Corrosion Behavior of Zirconium Treated Mild Steel with and Without Organic Coating: a Comparative Study

NASA Astrophysics Data System (ADS)

Ghanbari, Alireza; Attar, Mohammadreza Mohammadzade

2014-10-01

In this study, the anti-corrosion performance of phosphated and zirconium treated mild steel (ZTMS) with and without organic coating was evaluated using AC and DC electrochemical techniques. The topography and morphology of the zirconium treated samples were studied using atomic force microscopy (AFM) and field emission scanning electron microscope (FE-SEM) respectively. The results revealed that the anti-corrosion performance of the phosphate layer was superior to the zirconium conversion layer without an organic coating due to very low thickness and porous nature of the ZTMS. Additionally, the corrosion behavior of the organic coated substrates was substantially different. It was found that the corrosion protection performance of the phosphate steel and ZTMS with an organic coating is in the same order.

The study of structural properties of carbon nanotubes decorated with NiFe₂O₄ nanoparticles and application of nano-composite thin film as H₂S gas sensor.

PubMed

Hajihashemi, R; Rashidi, Ali M; Alaie, M; Mohammadzadeh, R; Izadi, N

2014-11-01

Nano-composite of multiwall carbon nanotube, decorated with NiFe2O4 nanoparticles (NiFe2O4-MWCNT), was synthesized using the sol-gel method. NiFe2O4-MWCNTs were characterized using different methods such as X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), high resolution transmission electron microscopy (HRTEM), atomic force microscopy (AFM) and vibrating sample magnetometer (VSM). The average size of the crystallites is 23.93 nm. The values of the saturation magnetization (MS), coercivity (HC) and retentivity (MR) of NiFe2O4-MWCNTs are obtained as 15 emu g(-1), 21Oe and 5 emu g(-1), respectively. In this research, NiFe2O4-MWCNT thin films were prepared with the spin-coating method. These thin films were used as the H2S gas sensor. The results suggest the possibility of the utilization of NiFe2O4-MWCNT nano-composite, as the H2S detector. The sensor shows appropriate response towards 100 ppm of H2S at 300°C. Copyright © 2014 Elsevier B.V. All rights reserved.

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.

An in vitro 3D model using collagen coated gelatin nanofibers for studying breast cancer metastasis.

PubMed

Janani, G; Pillai, Mamatha M; Selvakumar, R; Bhattacharyya, Amitava; Sabarinath, C

2017-02-07

The study of breast cancer metastasis is limited due to poor knowledge of molecular progression of breast tumor and varied heterogeneity. For a better understanding of tumor metastasis, a reliable 3D in vitro model bridging the gap between 2D cultures and in vivo animal model studies is essential. Our study is focused on two key points: (i) designing a 3D microenvironment for studying metastasis and (ii) simulating the metastasis milieu by inducing epithelial to mesenchymal transition (EMT) and mesenchymal to epithelial transition (MET). An electrospun gelatin nanofiber matrix (EGNF) was fabricated using electrospinning and further dip coated with different concentrations of collagen to obtain surface complexity and mechanical properties, similar to connective tissues. Nanofiber matrices were physically characterized by Fourier transform infrared spectroscopy (FTIR), atomic force microscopy (AFM), and field-emission scanning electron microscopy (FESEM). The FTIR, AFM, and FESEM results indicated the crosslinking and confirmed the presence of pores in the nanofiber matrices. Comparative studies on biocompatibility, cell attachment, and the proliferation of MCF-7 cells on EGNF and collagen coated gelatin nanofibrous matrix (CCGM) revealed higher cellular attachment and proliferation in CCGM. CCGM with human metastatic breast cancer cell line (MCF-7) was taken to study breast cancer metastasis using estrogen (induces EMT) and progesterone (induces MET) hormones for 24 h. Quantitative real-time PCR was used for quantifying the expression of metastasis related genes, and fluorescence microscopy for verifying the invasion of cells to the matrices. The expression of E-cadherin and matrix metalloproteinase 2 (MMP 2) confirmed the occurrence of EMT and MET. Live cell imaging and cellular attachment showed significant increase of cellular invasion in crosslinked 0.15% CCGM that serves as a suitable non-toxic, biocompatible, and affordable scaffold for studying breast cancer metastasis. Our findings suggested that CCGM can be used as a tissue-like 3D model for studying breast cancer metastatic events in vitro.

High-Resolution Scanning Electron Microscopy and Immuno-Gold Labeling of the Nuclear Lamina and Nuclear Pore Complex.

PubMed

Goldberg, Martin W

2016-01-01

Scanning electron microscopy (SEM) is a technique used to image surfaces. Field emission SEMs (feSEMs) can resolve structures that are ~0.5-1.5 nm apart. FeSEM, therefore is a useful technique for imaging molecular structures that exist at surfaces such as membranes. The nuclear envelope consists of four membrane surfaces, all of which may be accessible for imaging. Imaging of the cytoplasmic face of the outer membrane gives information about ribosomes and cytoskeletal attachments, as well as details of the cytoplasmic peripheral components of the nuclear pore complex, and is the most easily accessed surface. The nucleoplasmic face of the inner membrane is easily accessible in some cells, such as amphibian oocytes, giving valuable details about the organization of the nuclear lamina and how it interacts with the nuclear pore complexes. The luminal faces of both membranes are difficult to access, but may be exposed by various fracturing techniques. Protocols are presented here for the preparation, labeling, and feSEM imaging of Xenopus laevis oocyte nuclear envelopes.

Bark extract mediated green synthesis of silver nanoparticles: Evaluation of antimicrobial activity and antiproliferative response against osteosarcoma.

PubMed

Nayak, Debasis; Ashe, Sarbani; Rauta, Pradipta Ranjan; Kumari, Manisha; Nayak, Bismita

2016-01-01

In the current investigation we report the biosynthesis potentials of bark extracts of Ficus benghalensis and Azadirachta indica for production of silver nanoparticle without use of any external reducing or capping agent. The appearance of dark brown color indicated the complete nanoparticle synthesis which was further validated by absorbance peak by UV-vis spectroscopy. The morphology of the synthesized particles was characterized by Field emission- scanning electron microscopy (Fe-SEM) and atomic force microscopy (AFM). The X-ray diffraction (XRD) patterns clearly illustrated the crystalline phase of the synthesized nanoparticles. ATR-Fourier Transform Infrared (ATR-FTIR) spectroscopy was performed to identify the role of various functional groups in the nanoparticle synthesis. The synthesized nanoparticles showed promising antimicrobial activity against Gram negative (Escherichia coli, Pseudomonas aeruginosa and Vibrio cholerae) and Gram positive (Bacillus subtilis) bacteria. The synthesized nano Ag also showed antiproliferative activity against MG-63 osteosarcoma cell line in a dose dependent manner. Thus, these synthesized Ag nanoparticles can be used as a broad spectrum therapeutic agent against osteosarcoma and microorganisms. Copyright © 2015 Elsevier B.V. All rights reserved.

Synthesis and characterization of CdTe nanostructures grown by RF magnetron sputtering method

NASA Astrophysics Data System (ADS)

Akbarnejad, Elaheh; Ghoranneviss, Mahmood; Hantehzadeh, Mohammad Reza

2017-08-01

In this paper, we synthesize Cadmium Telluride nanostructures by radio frequency (RF) magnetron sputtering system on soda lime glass at various thicknesses. The effect of CdTe nanostructures thickness on crystalline, optical and morphological properties has been studied by means of X-ray diffraction (XRD), UV-VIS-NIR spectrophotometry, field emission scanning electron microscopy (FESEM) and atomic force microscopy (AFM), respectively. The XRD parameters of CdTe nanostructures such as microstrain, dislocation density, and crystal size have been examined. From XRD analysis, it could be assumed that increasing deposition time caused the formation of the wurtzite hexagonal structure of the sputtered films. Optical properties of the grown nanostructures as a function of film thickness have been observed. All the films indicate more than 60% transmission over a wide range of wavelengths. The optical band gap values of the films have obtained in the range of 1.62-1.45 eV. The results indicate that an RF sputtering method succeeded in depositing of CdTe nanostructures with high purity and controllable physical properties, which is appropriate for photovoltaic and nuclear detector applications.

Laser-induced damage of coatings on Yb:YAG crystals at cryogenic condition

NASA Astrophysics Data System (ADS)

Wang, He; Zhang, Weili; Chen, Shunli; Zhu, Meiping; He, Hongbo; Fan, Zhengxiu

2011-12-01

As large amounts of heat need to be dissipated during laser operation, some diode pumped solid state lasers (DPSSL), especially Yb:YAG laser, operate at cryogenic condition. This work investigated the laser induced damage of coatings (high-reflective and anti-reflective coatings) on Yb:YAG crystals at cryogenic temperature and room temperature. The results show that the damage threshold of coatings at cryogenic temperature is lower than the one at room temperature. Field-emission scanning electron microscopy (FESEM), optical profiler, step profiler and Atomic force microscope (AFM) were used to obtain the damage morphology, size and depth. Taking alteration of physical parameters, microstructure of coatings and the environmental pollution into consideration, we analyzed the key factor of lowering the coating damage threshold at cryogenic conditions. The results are important to understand the mechanisms leading to damage at cryogenic condition.

Hydroxyapatite nanocrystals: simple preparation, characterization and formation mechanism.

PubMed

Mohandes, Fatemeh; Salavati-Niasari, Masoud; Fathi, Mohammadhossein; Fereshteh, Zeinab

2014-12-01

Crystalline hydroxyapatite (HAP) nanoparticles and nanorods have been successfully synthesized via a simple precipitation method. To control the shape and particle size of HAP nanocrystals, coordination ligands derived from 2-hydroxy-1-naphthaldehyde were first prepared, characterized by Fourier transform infrared (FT-IR) and proton nuclear magnetic resonance ((1)H-NMR) spectroscopies, and finally applied in the synthesis process of HAP. On the other hand, the HAP nanocrystals were also characterized by several techniques including powder X-ray diffraction (XRD), field-emission scanning electron microscopy (FE-SEM) and transmission electron microscopy (TEM). According to the FE-SEM and TEM micrographs, it was found that the morphology and crystallinity of the HAP powders depended on the coordination mode of the ligands. Copyright © 2014 Elsevier B.V. All rights reserved.

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

PubMed

Kumar, Anil; Singhal, Aditi

2009-07-22

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

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

NASA Astrophysics Data System (ADS)

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

2017-01-01

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

Graphene nanosheets preparation using magnetic nanoparticle assisted liquid phase exfoliation of graphite: The coupled effect of ultrasound and wedging nanoparticles.

PubMed

Hadi, Alireza; Zahirifar, Jafar; Karimi-Sabet, Javad; Dastbaz, Abolfazl

2018-06-01

This study aims to investigate a novel technique to improve the yield of liquid phase exfoliation of graphite to graphene sheets. The method is based on the utilization of magnetic Fe 3 O 4 nanoparticles as "particle wedge" to facilitate delamination of graphitic layers. Strong shear forces resulted from the collision of Fe 3 O 4 particles with graphite particles, and intense ultrasonic waves lead to enhanced exfoliation of graphite. High quality of graphene sheets along with the ease of Fe 3 O 4 particle separation from graphene solution which arises from the magnetic nature of Fe 3 O 4 nanoparticles are the unique features of this approach. Initial graphite flakes and produced graphene sheets were characterized by various methods including field emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), Raman spectroscopy, atomic force microscopy (AFM), Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), and Zeta potential analysis. Moreover, the effect of process factors comprising initial graphite concentration, Fe 3 O 4 nanoparticles concentration, sonication time, and sonication power were investigated. Results revealed that graphene preparation yield and the number of layers could be manipulated by the presence of magnetic nanoparticles. Copyright © 2018 Elsevier B.V. All rights reserved.

Self-sterilizing ormosils surfaces based on photo-synzthesized silver nanoparticles.

PubMed

Gonçalves, Lidiane Patrícia; Miñán, Alejandro; Benítez, Guillermo; de Mele, Mónica Fernández Lorenzo; Vela, María Elena; Schilardi, Patricia L; Ferreira-Neto, Elias Paiva; Noveletto, Júlia Cristina; Correr, Wagner Rafael; Rodrigues-Filho, Ubirajara Pereira

2018-04-01

Medical device-related infections represent a major healthcare complication, resulting in potential risks for the patient. Antimicrobial materials comprise an attractive strategy against bacterial colonization and biofilm proliferation. However, in most cases these materials are only bacteriostatic or bactericidal, and consequently they must be used in combination with other antimicrobials in order to reach the eradication condition (no viable microorganisms). In this study, a straightforward and robust antibacterial coating based on Phosphotungstate Ormosil doped with core-shell (SiO 2 @TiO 2 ) was developed using sol-gel process, chemical tempering, and Ag nanoparticle photoassisted synthesis (POrs-CS-Ag). The coating was characterized by X-ray Fluorescence Spectroscopy (XRF), Field Emission Scanning Electron Microscopy (FE-SEM), Atomic Force Microscopy (AFM) and X-ray Photoelectron Microscopy (XPS). The silver free coating displays low antibacterial activity against Staphylococcus aureus and Pseudomonas aeruginosa, in opposition to the silver loaded ones, which are able to completely eradicate these strains. Moreover, the antimicrobial activity of these substrates remains high until three reutilization cycles, which make them a promising strategy to develop self-sterilizing materials, such as POrs-CS-Ag-impregnated fabric, POrs-CS-Ag coated indwelling metals and polymers, among other materials. Copyright © 2017 Elsevier B.V. All rights reserved.

Spatial organization of cellulose microfibrils and matrix polysaccharides in primary plant cell walls as imaged by multichannel atomic force microscopy.

PubMed

Zhang, Tian; Zheng, Yunzhen; Cosgrove, Daniel J

2016-01-01

We used atomic force microscopy (AFM), complemented with electron microscopy, to characterize the nanoscale and mesoscale structure of the outer (periclinal) cell wall of onion scale epidermis - a model system for relating wall structure to cell wall mechanics. The epidermal wall contains ~100 lamellae, each ~40 nm thick, containing 3.5-nm wide cellulose microfibrils oriented in a common direction within a lamella but varying by ~30 to 90° between adjacent lamellae. The wall thus has a crossed polylamellate, not helicoidal, wall structure. Montages of high-resolution AFM images of the newly deposited wall surface showed that single microfibrils merge into and out of short regions of microfibril bundles, thereby forming a reticulated network. Microfibril direction within a lamella did not change gradually or abruptly across the whole face of the cell, indicating continuity of the lamella across the outer wall. A layer of pectin at the wall surface obscured the underlying cellulose microfibrils when imaged by FESEM, but not by AFM. The AFM thus preferentially detects cellulose microfibrils by probing through the soft matrix in these hydrated walls. AFM-based nanomechanical maps revealed significant heterogeneity in cell wall stiffness and adhesiveness at the nm scale. By color coding and merging these maps, the spatial distribution of soft and rigid matrix polymers could be visualized in the context of the stiffer microfibrils. Without chemical extraction and dehydration, our results provide multiscale structural details of the primary cell wall in its near-native state, with implications for microfibrils motions in different lamellae during uniaxial and biaxial extensions. © 2015 The Authors The Plant Journal © 2015 John Wiley & Sons Ltd.

A comparative study on the effects of ultrathin luminescent graphene oxide quantum dot (GOQD) and graphene oxide (GO) nanosheets on the interfacial interactions and mechanical properties of an epoxy composite.

PubMed

Karimi, B; Ramezanzadeh, B

2017-05-01

The reinforcement effect of graphene oxide nanosheets on the mechanical properties of an epoxy coating has been extensively studied. However, the effect of graphene oxide quantum dot (GOQD) as a new unique carbon based nanomaterial (with lateral dimension of 5-6nm and thickness of one carbon atom) on the mechanical properties of epoxy coating has not been reported and compared with GO yet. So this study aims at fabrication of a high-performance polymer composite with unique mechanical properties using GOQD nanosheets. GO and GOQD were obtained through two different strategies of "top-down" synthesis from an expandable graphite by a modified Hummers' method and an easy "bottom-up" method by carbonizing citric acid, respectively. The morphology, size distribution, microstructure and chemistry of the GO and GOQD were compared by utilizing X-ray diffraction (XRD) analysis, atomic force microscopy (AFM), high resolution-transmission electron microscopy (HR-TEM), high resolution field-emission scanning electron microscopy (FE-SEM), thermal gravimetric analysis (TGA), Fourier transform infrared spectroscopy (FT-IR), X-ray photoelectron spectroscopy (XPS). Results obtained from these analyses confirmed successful synthesize of GOQD and GO nanosheets. The reinforcement effect of GO and GOQD nanosheets on the mechanical properties of the epoxy coating was studied by dynamic mechanical thermal analysis (DMTA) and tensile test. It was found that the GOQD could remarkably enhance the energy of break, Young's modulus, tensile stress and interfacial interactions compared to the neat epoxy and the one reinforced with GO nanosheets. GOQD improved the fracture toughness by factor of 175% and 700% compared to the GO/Epoxy and neat epoxy, respectively. Copyright © 2017 Elsevier Inc. All rights reserved.

Effect of fabrication parameters on morphological and optical properties of highly doped p-porous silicon

NASA Astrophysics Data System (ADS)

Zare, Maryam; Shokrollahi, Abbas; Seraji, Faramarz E.

2011-09-01

Porous silicon (PS) layers were fabricated by anodization of low resistive (highly doped) p-type silicon in HF/ethanol solution, by varying current density, etching time and HF concentration. Atomic force microscopy (AFM) and field emission scanning electron microscope (FESEM) analyses were used to investigate the physical properties and reflection spectrum was used to investigate the optical behavior of PS layers in different fabrication conditions. Vertically aligned mesoporous morphology is observed in fabricated films and with HF concentration higher than 20%. The dependence of porosity, layer thickness and rms roughness of the PS layer on current density, etching time and composition of electrolyte is also observed in obtained results. Correlation between reflectivity and fabrication parameters was also explored. Thermal oxidation was performed on some mesoporous layers that resulted in changes of surface roughness, mean height and reflectivity of the layers.

Anchoring of Cu(II) onto surface of porous metal-organic framework through post-synthesis modification for the synthesis of benzimidazoles and benzothiazoles

NASA Astrophysics Data System (ADS)

Kardanpour, Reihaneh; Tangestaninejad, Shahram; Mirkhani, Valiollah; Moghadam, Majid; Mohammadpoor-Baltork, Iraj; Zadehahmadi, Farnaz

2016-03-01

Efficient synthesis of various benzimidazoles and benzothiazoles under mild conditions catalyzed by Cu(II) anchored onto UiO-66-NH2 metal organic framework is reported. In this manner, first, the aminated UiO-66 was modified with thiophene-2-carbaldehyde and then the prepared Schiff base was reacted with CuCl2. The prepared catalyst was characterized by FT-IR, UV-vis, X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), N2 adsorption, inductively coupled plasma atomic emission spectroscopy (ICP-AES) and field emission scanning electron microscopy (FE-SEM). The UiO-66-NH2-TC-Cu was applied as a highly efficient catalyst for synthesis of benzimidazole and benzothiazole derivatives by the reaction of aldehydes with 1,2-diaminobenzene or 2-aminothiophenol. The Cu(II)-containing MOF was reused several times without any appreciable loss of its efficiency.

Efficient alkene epoxidation catalyzed by molybdenyl acetylacetonate supported on aminated UiO-66 metal-organic framework

NASA Astrophysics Data System (ADS)

Kardanpour, Reihaneh; Tangestaninejad, Shahram; Mirkhani, Valiollah; Moghadam, Majid; Mohammadpoor-Baltork, Iraj; Zadehahmadi, Farnaz

2015-03-01

Metal-organic frameworks (MOFs) containing Mo Schiff base complexes were prepared by post-synthesis method and applied as efficient catalysts in the epoxidation of alkenes with tert-BuOOH. In this manner, UiO-66-NH2 (UiO=University of Oslo) MOF was reacted with salicylaldehyde and thiophene-2-carbaldehyde to produce bidentate Schiff bases. Then, the Schiff base ligands were used for immobilization of molybdenyl acetylacetonate. These new catalysts were characterized by FT-IR, UV-vis spectroscopic techniques, X-ray diffraction (XRD), BET, inductively coupled plasma atomic emission spectroscopy (ICP-AES) and field emission scanning electron microscopy (FE-SEM). These catalytic systems showed excellent activity in the epoxidation of alkenes such as cyclic and linear ones with tert-butyl hydroperoxide (TBHP) in 1,2-dichloroethane, and reused several times without any appreciable loss of their activity.

Direct Growth of CuO Nanorods on Graphitic Carbon Nitride with Synergistic Effect on Thermal Decomposition of Ammonium Perchlorate.

PubMed

Tan, Linghua; Xu, Jianhua; Li, Shiying; Li, Dongnan; Dai, Yuming; Kou, Bo; Chen, Yu

2017-05-02

Novel graphitic carbon nitride/CuO (g-C₃N₄/CuO) nanocomposite was synthesized through a facile precipitation method. Due to the strong ion-dipole interaction between copper ions and nitrogen atoms of g-C₃N₄, CuO nanorods (length 200-300 nm, diameter 5-10 nm) were directly grown on g-C₃N₄, forming a g-C₃N₄/CuO nanocomposite, which was confirmed via X-ray diffraction (XRD), transmission electron microscopy (TEM), field emission scanning electron microscopy (FESEM), and X-ray photoelectron spectroscopy (XPS). Finally, thermal decomposition of ammonium perchlorate (AP) in the absence and presence of the prepared g-C₃N₄/CuO nanocomposite was examined by differential thermal analysis (DTA), and thermal gravimetric analysis (TGA). The g-C₃N₄/CuO nanocomposite showed promising catalytic effects for the thermal decomposition of AP. Upon addition of 2 wt % nanocomposite with the best catalytic performance (g-C₃N₄/20 wt % CuO), the decomposition temperature of AP was decreased by up to 105.5 °C and only one decomposition step was found instead of the two steps commonly reported in other examples, demonstrating the synergistic catalytic activity of the as-synthesized nanocomposite. This study demonstrated a successful example regarding the direct growth of metal oxide on g-C₃N₄ by ion-dipole interaction between metallic ions, and the lone pair electrons on nitrogen atoms, which could provide a novel strategy for the preparation of g-C₃N₄-based nanocomposite.

Nucleation, aggregative growth and detachment of metal nanoparticles during electrodeposition at electrode surfaces† †Electronic supplementary information (ESI) available: S1 Scharifker–Hills model, S2 tapping mode-atomic force microscopy (TM-AFM) image of AM grade HOPG, after exposure to a droplet of 50 mM KNO3, S3 distribution of induction times, S4 results of the modified Cottrell fits at different potentials, S5 FE-SEM images of HOPG after control tip breaking, S6 extended current–time trace. See DOI: 10.1039/c4sc02792b Click here for additional data file.

PubMed Central

Lazenby, Robert A.; Kirkman, Paul M.

2015-01-01

The nucleation and growth of metal nanoparticles (NPs) on surfaces is of considerable interest with regard to creating functional interfaces with myriad applications. Yet, key features of these processes remain elusive and are undergoing revision. Here, the mechanism of the electrodeposition of silver on basal plane highly oriented pyrolytic graphite (HOPG) is investigated as a model system at a wide range of length scales, spanning electrochemical measurements from the macroscale to the nanoscale using scanning electrochemical cell microscopy (SECCM), a pipette-based approach. The macroscale measurements show that the nucleation process cannot be modelled as either truly instantaneous or progressive, and that step edge sites of HOPG do not play a dominant role in nucleation events compared to the HOPG basal plane, as has been widely proposed. Moreover, nucleation numbers extracted from electrochemical analysis do not match those determined by atomic force microscopy (AFM). The high time and spatial resolution of the nanoscale pipette set-up reveals individual nucleation and growth events at the graphite basal surface that are resolved and analysed in detail. Based on these results, corroborated with complementary microscopy measurements, we propose that a nucleation-aggregative growth-detachment mechanism is an important feature of the electrodeposition of silver NPs on HOPG. These findings have major implications for NP electrodeposition and for understanding electrochemical processes at graphitic materials generally. PMID:29560200

Fabrication of Ti-0.48Al Alloy by Centrifugal Casting.

PubMed

Park, Jong Bum; Lee, Jung-Il; Ryu, Jeong Ho

2018-09-01

Many of the unique properties of TiAl alloys that make are attractive for use in high-temperature structural applications also make it challenging to process them into useful products. Cast TiAl is rapidly nearing commercialization, particularly in the vehicle industry, owing to its low production cost. In this study, the centrifugal casting of a TiAl (Ti-48%Al, mole fraction) turbocharger was simulated and an experimental casting was created in vacuum using an induction melting furnace coupled to a ceramic composite mold. Numerical simulation results agreed with the experiment. The crystal structure, microstructure, and chemical composition of the TiAl prepared by centrifugal casting were studied by X-ray diffractometry, optical microscopy, field emission scanning electron microscopy (FE-SEM) and energy dispersive spectroscopy (EDS). FE-SEM and EDS examinations of the TiAl casting revealed that the thickness of the oxide layer (α-case) was typically less than 35 μm.

Transdermal delivery of raloxifene HCl via ethosomal system: Formulation, advanced characterizations and pharmacokinetic evaluation.

PubMed

Mahmood, Syed; Mandal, Uttam Kumar; Chatterjee, Bappaditya

2018-05-05

Raloxifene HCl belongs to a class of selective estrogen receptor modulators (SERMs) which is used for the management of breast cancer. The major problem reported with raloxifene is its poor bioavailability which is only up to 2%. The main objective of the present work was to formulate raloxifene loaded ethosomal preparation for transdermal application and compare it with an oral formulation of the drug. Five ethosomal formulations with different concentrations of ethanol and a conventional liposomes formulation were prepared by rotary evaporation method. The prepared systems were characterised by high resolution transmission electron microscopy (HRTEM), force emission electron microscopy (FESEM), atomic force microscopy (AFM), X-ray diffraction (XRD) and 31 P NMR study. All these advanced characterization study established that the ethosome formulation was well defined by its size, shape and its bilayer formation. Transdermal flux of the optimized ethosome formulation was 22.14 ± 0.83 µg/ml/cm 2 which was 21 times higher when compared to the conventional liposomes. Confocal microscopy study revealed an enhanced permeation of coumarin-6 dye loaded ethosomes to much deeper layers of skin when compared with conventional liposomes. The gel was found to be pseudoplastic with elastic behaviour. In-vivo studies on rats showed a higher bioavailability of RXL (157% times) for ethosomal formulation when compared with the oral formulation. In conclusion, RXL loaded ethosomal formulation via transdermal route showed superior drug delivery properties as compared to oral formulation. Copyright © 2018 Elsevier B.V. All rights reserved.

Characterization of two-dimensional hexagonal boron nitride using scanning electron and scanning helium ion microscopy

NASA Astrophysics Data System (ADS)

Guo, Hongxuan; Gao, Jianhua; Ishida, Nobuyuki; Xu, Mingsheng; Fujita, Daisuke

2014-01-01

Characterization of the structural and physical properties of two-dimensional (2D) materials, such as layer number and inelastic mean free path measurements, is very important to optimize their synthesis and application. In this study, we characterize the layer number and morphology of hexagonal boron nitride (h-BN) nanosheets on a metallic substrate using field emission scanning electron microscopy (FE-SEM) and scanning helium ion microscopy (HIM). Using scanning beams of various energies, we could analyze the dependence of the intensities of secondary electrons on the thickness of the h-BN nanosheets. Based on the interaction between the scanning particles (electrons and helium ions) and h-BN nanosheets, we deduced an exponential relationship between the intensities of secondary electrons and number of layers of h-BN. With the attenuation factor of the exponential formula, we calculate the inelastic mean free path of electrons and helium ions in the h-BN nanosheets. Our results show that HIM is more sensitive and consistent than FE-SEM for characterizing the number of layers and morphology of 2D materials.

Accurate Assessment of the Oxygen Reduction Electrocatalytic Activity of Mn/Polypyrrole Nanocomposites Based on Rotating Disk Electrode Measurements, Complemented with Multitechnique Structural Characterizations

PubMed Central

Sánchez, Carolina Ramírez; Taurino, Antonietta; Bozzini, Benedetto

2016-01-01

This paper reports on the quantitative assessment of the oxygen reduction reaction (ORR) electrocatalytic activity of electrodeposited Mn/polypyrrole (PPy) nanocomposites for alkaline aqueous solutions, based on the Rotating Disk Electrode (RDE) method and accompanied by structural characterizations relevant to the establishment of structure-function relationships. The characterization of Mn/PPy films is addressed to the following: (i) morphology, as assessed by Field-Emission Scanning Electron Microscopy (FE-SEM) and Atomic Force Microscope (AFM); (ii) local electrical conductivity, as measured by Scanning Probe Microscopy (SPM); and (iii) molecular structure, accessed by Raman Spectroscopy; these data provide the background against which the electrocatalytic activity can be rationalised. For comparison, the properties of Mn/PPy are gauged against those of graphite, PPy, and polycrystalline-Pt (poly-Pt). Due to the literature lack of accepted protocols for precise catalytic activity measurement at poly-Pt electrode in alkaline solution using the RDE methodology, we have also worked on the obtainment of an intralaboratory benchmark by evidencing some of the time-consuming parameters which drastically affect the reliability and repeatability of the measurement. PMID:28042491

Effect of precursor concentration and film thickness deposited by layer on nanostructured TiO2 thin films

NASA Astrophysics Data System (ADS)

Affendi, I. H. H.; Sarah, M. S. P.; Alrokayan, Salman A. H.; Khan, Haseeb A.; Rusop, M.

2018-05-01

Sol-gel spin coating method is used in the production of nanostructured TiO2 thin film. The surface topology and morphology was observed using the Atomic Force Microscopy (AFM) and Field Emission Scanning Electron Microscopy (FESEM). The electrical properties were investigated by using two probe current-voltage (I-V) measurements to study the electrical resistivity behavior, hence the conductivity of the thin film. The solution concentration will be varied from 14.0 to 0.01wt% with 0.02wt% interval where the last concentration of 0.02 to 0.01wt% have 0.01wt% interval to find which concentrations have the highest conductivity then the optimized concentration's sample were chosen for the thickness parameter based on layer by layer deposition from 1 to 6 layer. Based on the result, the lowest concentration of TiO2, the surface becomes more uniform and the conductivity will increase. As the result, sample of 0.01wt% concentration have conductivity value of 1.77E-10 S/m and will be advanced in thickness parameter. Whereas in thickness parameter, the 3layer deposition were chosen as its conductivity is the highest at 3.9098E9 S/m.

Combined effects of Ag nanoparticles and oxygen plasma treatment on PLGA morphological, chemical, and antibacterial properties.

PubMed

Fortunati, Elena; Mattioli, Samantha; Visai, Livia; Imbriani, Marcello; Fierro, Josè Luis G; Kenny, Josè Maria; Armentano, Ilaria

2013-03-11

The purpose of this study is to investigate the combined effects of oxygen plasma treatments and silver nanoparticles (Ag) on PLGA in order to modulate the surface antimicrobial properties through tunable bacteria adhesion mechanisms. PLGA nanocomposite films, produced by solvent casting with 1 wt % and 7 wt % of Ag nanoparticles were investigated. The PLGA and PLGA/Ag nanocomposite surfaces were treated with oxygen plasma. Surface properties of PLGA were investigated by field emission scanning electron microscopy (FESEM), atomic force microscopy (AFM), static contact angle (CA), and high resolution X-ray photoelectron spectroscopy (XPS). Antibacterial tests were performed using an Escherichia coli RB (a Gram negative) and Staphylococcus aureus 8325-4 (a Gram positive). The PLGA surface becomes hydrophilic after the oxygen treatment and its roughness increases with the treatment time. The surface treatment and the Ag nanoparticle introduction have a dominant influence on the bacteria adhesion and growth. Oxygen-treated PLGA/Ag systems promote higher reduction of the bacteria viability in comparison to the untreated samples and neat PLGA. The combination of Ag nanoparticles with the oxygen plasma treatment opens new perspectives for the studied biodegradable systems in biomedical applications.

An investigation of GaN thin films on AlN on sapphire substrate by sol-gel spin coating method

NASA Astrophysics Data System (ADS)

Amin, Nur Fahana Mohd; Ng, Sha Shiong

2017-12-01

In this research, the gallium nitride (GaN) thin films were deposited on aluminium nitride on sapphire (AlN/Al2O3) substrate by sol-gel spin coating method. Simple ethanol-based precursor with the addition of diethanolamine solution was used. The structural and morphology properties of synthesized GaN thin films were characterized by using X-ray Diffraction, Field-Emission Scanning Electron Microscopy and Atomic Force Microscopy. While the elemental compositions and the lattice vibrational properties of the films were investigated by means of the Energy Dispersive X-ray spectroscopy and Raman spectroscopy. All the results revealed that the wurtzite structure GaN thin films with GaN(002) preferred orientation and smooth surface morphology were successfully grown on AlN/Al2O3 substrate by using inexpensive and simplified sol-gel spin coating technique. The sol-gel spin coated GaN thin film with lowest oxygen content was also achieved.FESEM images show that GaN thin films with uniform and packed grains were formed. Based on the obtained results, it can be concluded that wurtzite structure GaN thin films were successfully deposited on AlN/Al2O3 substrate.

Effect of Ti Substrate Ion Implantation on the Physical Properties of Anodic TiO2 Nanotubes

NASA Astrophysics Data System (ADS)

Jedi-Soltanabadi, Zahra; Ghoranneviss, Mahmood; Ghorannevis, Zohreh; Akbari, Hossein

2018-03-01

The influence of nitrogen-ion implantation on the titanium (Ti) surface is studied. The nontreated Ti and the Ti treated with ion implantation were anodized in an ethylene-glycol-based electrolyte solution containing 0.3 wt% ammonium fluoride (NH4F) and 3 vol% deionized (DI) water at a potential of 60 V for 1 h at room temperature. The current density during the growth of the TiO2 nanotubes was monitored in-situ. The surface roughnesses of the Ti substrates before and after the ion implantation were investigated with atomic force microscopy (AFM). The surface roughness was lower for the treated Ti substrate. The morphology of the anodic TiO2 nanotubes was studied by using field-emission scanning electron microscopy (FESEM). Clearly, the titanium nanotubes grown on the treated substrate were longer. In addition, some ribs were observed on their walls. The optical band gap of the anodic TiO2 nanotubes was characterized by using a diffuse reflection spectral (DRS) analysis. The anodic TiO2 nanotubes grown on the treated Ti substrate revealed a band gap energy of approximately 3.02 eV.

Self-assembled chiral helical nanofibers by amphiphilic dipeptide derived from d- or l-threonine and application as a template for the synthesis of Au and Ag nanoparticles.

PubMed

Zhang, Han; Xin, Xia; Sun, Jichao; Zhao, Liupeng; Shen, Jinglin; Song, Zhaohua; Yuan, Shiling

2016-12-15

The discovery of a class of self-assembling peptides that spontaneously undergo self-organization into well-ordered structures opened a new avenue for molecular fabrication of biological materials. In this paper, the structure controlled helical nanofibers were prepared by two artificial β-sheet dipeptides with long alkyl chains derived from l- and d-threonine (Thr) and sodium hydroxide (NaOH). These helical nanofibers have been characterized using transmission electron microscopy (TEM), field emission scanning electron microscopy (FE-SEM), atomic force microscopy (AFM), circular dichroism (CD), Fourier transform infrared (FT-IR) spectroscopy, and X-ray powder diffraction (XRD). It was demonstrated that the helicity of the nanofibers could be easily controlled by changing the chirality of the constituent amino acids in the peptide species (d- or l-threonine). Moreover, the hydrogen bonding interactions between the amide groups as well as the hydrophobic interactions among the alkyl chains play important roles in the self-assembly process. It also can be observed that with the passage of time, the hydrogen bonding interactions between the individual nanofiber induced the conversion from nanofibers to nanobelts. Particularly, gold and silver nanoparticles performed good catalytic ability were synthesized using the assembled nanofibers as template. Copyright © 2016 Elsevier Inc. All rights reserved.

Titanium composite conversion coating formation on CRS In the presence of Mo and Ni ions: Electrochemical and microstructure characterizations

NASA Astrophysics Data System (ADS)

Eivaz Mohammadloo, H.; Sarabi, A. A.

2016-11-01

There have been an increasing interest in finding a replacement for the chromating process due to environmental and health concerns. Hence, in this study Chrome-free chemical conversion coatings were deposited on the surface of cold-rolled steel (CRS) on the basis of Titanium (TiCC), Titanium-Nickel (TiNiCC) and titanium-molybdate (TiMoCC) based conversion coating solutions. The surface characterization was performed by field emission scanning electron microscope (FESEM), X-ray photoelectron spectroscopy (XPS), atomic force microscopy (AFM) and contact angle measuring device. Also, the corrosion behavior was assessed by the means of potentiodynamic polarization and electrochemical impedance spectroscopy (EIS) measurements. FESEM and AFM study show that the TiNiCC is denser and more uniform than that TiCC and TiMoCC since, TiMoCC conversion coating presents network feature, and there were abundant micro-cracks on the surface of the coating. XPS results confirmed the precipitation of Ti and Ni oxide/hydroxide, Mn dioxide/trioxide on the surface of different Ti-based conversion coatings. Electrochemical results revealed that all Ti-based conversion coatings have better anti-corrosion properties than bare CRS. Moreover, TiNiCC treatment inhibited the corrosion of CRS to a significant degree (polarization resistance (Rp) = 5510 Ω cm2) in comparison with TiCC (Rp = 2705 Ω cm2) and TiMoCC (Rp = 805 Ω cm2).

The ultrastructure of subgingival dental plaque, revealed by high-resolution field emission scanning electron microscopy.

PubMed

Holliday, Richard; Preshaw, Philip M; Bowen, Leon; Jakubovics, Nicholas S

2015-01-01

To explore the ultrastructure of subgingival dental plaque using high-resolution field emission scanning electron microscopy (FE-SEM) and to investigate whether extracellular DNA (eDNA) could be visualised in ex vivo samples. Ten patients were recruited who fulfilled the inclusion criteria (teeth requiring extraction with radiographic horizontal bone loss of over 50% and grade II/III mobility). In total, 12 teeth were extracted using a minimally traumatic technique. Roots were sectioned using a dental air turbine handpiece, under water cooling to produce 21 samples. Standard fixation and dehydration protocols were followed. For some samples, gold-labelled anti-DNA antibodies were applied before visualising biofilms by FE-SEM. High-resolution FE-SEMs of subgingival biofilm were obtained in 90% of the samples. The sectioning technique left dental plaque biofilms undisturbed. Copious amounts of extracellular material were observed in the plaque, which may have been eDNA as they had a similar appearance to labelled eDNA from in vitro studies. There was also evidence of membrane vesicles and open-ended tubular structures. Efforts to label eDNA with immune-gold antibodies were unsuccessful and eDNA was not clearly labelled. High-resolution FE-SEM images were obtained of undisturbed subgingival ex vivo dental plaque biofilms. Important structural features were observed including extracellular polymeric material, vesicles and unusual open tubule structures that may be remnants of lysed cells. The application of an eDNA immune-gold-labelling technique, previously used successfully in in vitro samples, did not clearly identify eDNA in ex vivo samples. Further studies are needed to characterise the molecular composition of the observed extracellular matrix material.

The ultrastructure of subgingival dental plaque, revealed by high-resolution field emission scanning electron microscopy

PubMed Central

Holliday, Richard; Preshaw, Philip M; Bowen, Leon; Jakubovics, Nicholas S

2015-01-01

Objectives/Aims: To explore the ultrastructure of subgingival dental plaque using high-resolution field emission scanning electron microscopy (FE-SEM) and to investigate whether extracellular DNA (eDNA) could be visualised in ex vivo samples. Materials and Methods: Ten patients were recruited who fulfilled the inclusion criteria (teeth requiring extraction with radiographic horizontal bone loss of over 50% and grade II/III mobility). In total, 12 teeth were extracted using a minimally traumatic technique. Roots were sectioned using a dental air turbine handpiece, under water cooling to produce 21 samples. Standard fixation and dehydration protocols were followed. For some samples, gold-labelled anti-DNA antibodies were applied before visualising biofilms by FE-SEM. Results: High-resolution FE-SEMs of subgingival biofilm were obtained in 90% of the samples. The sectioning technique left dental plaque biofilms undisturbed. Copious amounts of extracellular material were observed in the plaque, which may have been eDNA as they had a similar appearance to labelled eDNA from in vitro studies. There was also evidence of membrane vesicles and open-ended tubular structures. Efforts to label eDNA with immune-gold antibodies were unsuccessful and eDNA was not clearly labelled. Conclusions: High-resolution FE-SEM images were obtained of undisturbed subgingival ex vivo dental plaque biofilms. Important structural features were observed including extracellular polymeric material, vesicles and unusual open tubule structures that may be remnants of lysed cells. The application of an eDNA immune-gold-labelling technique, previously used successfully in in vitro samples, did not clearly identify eDNA in ex vivo samples. Further studies are needed to characterise the molecular composition of the observed extracellular matrix material. PMID:29607057

Synthesis and characterization of copper zinc oxide nanoparticles obtained via metathesis process

NASA Astrophysics Data System (ADS)

Phoohinkong, Weerachon; Foophow, Tita; Pecharapa, Wisanu

2017-09-01

Copper-doped zinc oxide nanoparticles were successfully synthesized by grinding copper acetate and zinc acetate powder with different starting molar ratios in combined with sodium hydroxide. The effect of initial copper and zinc molar ratios on the product samples was investigated and discussed. Relevant ligand coordination type of reactant acetate salt precursors and product samples were investigated by Fourier transform infrared spectroscopy (FTIR). The particle shapes and surface morphologies were characterized by field emission scanning electron microscopy (FESEM) and transmission electron microscopy (TEM). Phase structures of prepared samples were studied by x-ray powder diffraction (XRD) and x-ray absorption near-edge spectroscopy (XANES) was applied to investigate the local structure of Cu and Zn environment atoms. The results demonstrate that the, particle size of as-synthesized products affected by copper concentration in the precursor trend to gradually decreases from nanorod shape with diameter around 50-100 nm to irregular particle structure around 5 nm associated with an increase in the concentration of copper in precursor. Moreover, it is noticed that shape and morphology of the products are strongly dependent on Cu:Zn ratios during the synthesis. Nanocrystallines Cu-doped ZnO by the substitution in Zn site with a high crystallization degree of hexagonal wurtzite structure were obtained. This synthesis technique is suggested as a potential effective technique for preparing copper zinc oxide nanoparticles with various atomic ratio in wide range of applications. Contribution at the 4th Southeast Asia Conference on Thermoelectrics 2016 (SACT 2016), 15-18 December 2016, Da Nang City, Vietnam.

The structural properties of flower-like ZnO nanostructures on porous silicon

NASA Astrophysics Data System (ADS)

Eswar, Kevin Alvin; Suhaimi, Mohd Husairi Fadzillah; Guliling, Muliyadi; Mohamad, Maryam; Khusaimi, Zuraida; Rusop, M.; Abdullah, Saifollah

2018-05-01

The flower-like zinc oxide (ZnO) were successfully synthesized on porous silicon (PSi) via hydrothermal method. The characteristic of ZnO nanostructures was investigated using field emission scanning microscopy (FESEM) and X-ray diffraction (X-Ray). The FESEM images show the flower-like ZnO nanostructures composed ZnO nanoparticles. The X-ray diffraction shows that strong intensity of (100), (002) and (101) peaks. The structural analysis revealed that the peaks angles were shifted due to the stress or imperfection of the crystalline of ZnO nanostructures. The crystalline sizes in range of 42.60 to 54.09 nm were produced.

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

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

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

2013-02-15

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

Imaging interactions of metal oxide nanoparticles with macrophage cells by ultra-high resolution scanning electron microscopy techniques.

PubMed

Plascencia-Villa, Germán; Starr, Clarise R; Armstrong, Linda S; Ponce, Arturo; José-Yacamán, Miguel

2012-11-01

Use of engineered metal oxide nanoparticles in a plethora of biological applications and custom products has warned about some possible dose-dependent cytotoxic effects. Macrophages are key components of the innate immune system used to study possible toxic effects and internalization of different nanoparticulate materials. In this work, ultra-high resolution field emission scanning electron microscopy (FE-SEM) was used to offer new insights into the dynamical processes of interaction of nanomaterials with macrophage cells dosed with different concentrations of metal oxide nanoparticles (CeO(2), TiO(2) and ZnO). The versatility of FE-SEM has allowed obtaining a detailed characterization of processes of adsorption and endocytosis of nanoparticles, by using advanced analytical and imaging techniques on complete unstained uncoated cells, including secondary electron imaging, high-sensitive backscattered electron imaging, X-ray microanalysis and stereoimaging. Low voltage BF/DF-STEM confirmed nanoparticle adsorption and internalization into endosomes of CeO(2) and TiO(2), whereas ZnO develop apoptosis after 24 h of interaction caused by dissolution and invasion of cell nucleus. Ultra-high resolution scanning electron microscopy techniques provided new insights into interactions of inorganic nanoparticles with macrophage cells with high spatial resolution.

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

NASA Astrophysics Data System (ADS)

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

2018-05-01

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

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.

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.

Synthesis and characterization of single-crystalline zinc tin oxide nanowires

NASA Astrophysics Data System (ADS)

Shi, Jen-Bin; Wu, Po-Feng; Lin, Hsien-Sheng; Lin, Ya-Ting; Lee, Hsuan-Wei; Kao, Chia-Tze; Liao, Wei-Hsiang; Young, San-Lin

2014-05-01

Crystalline zinc tin oxide (ZTO; zinc oxide with heavy tin doping of 33 at.%) nanowires were first synthesized using the electrodeposition and heat treatment method based on an anodic aluminum oxide (AAO) membrane, which has an average diameter of about 60 nm. According to the field emission scanning electron microscopy (FE-SEM) results, the synthesized ZTO nanowires are highly ordered and have high wire packing densities. The length of ZTO nanowires is about 4 μm, and the aspect ratio is around 67. ZTO nanowires with a Zn/(Zn + Sn) atomic ratio of 0.67 (approximately 2/3) were observed from an energy dispersive spectrometer (EDS). X-ray diffraction (XRD) and corresponding selected area electron diffraction (SAED) patterns demonstrated that the ZTO nanowire is hexagonal single-crystalline. The study of ultraviolet/visible/near-infrared (UV/Vis/NIR) absorption showed that the ZTO nanowire is a wide-band semiconductor with a band gap energy of 3.7 eV.

Synthesis and characterization of single-crystalline zinc tin oxide nanowires.

PubMed

Shi, Jen-Bin; Wu, Po-Feng; Lin, Hsien-Sheng; Lin, Ya-Ting; Lee, Hsuan-Wei; Kao, Chia-Tze; Liao, Wei-Hsiang; Young, San-Lin

2014-01-01

Crystalline zinc tin oxide (ZTO; zinc oxide with heavy tin doping of 33 at.%) nanowires were first synthesized using the electrodeposition and heat treatment method based on an anodic aluminum oxide (AAO) membrane, which has an average diameter of about 60 nm. According to the field emission scanning electron microscopy (FE-SEM) results, the synthesized ZTO nanowires are highly ordered and have high wire packing densities. The length of ZTO nanowires is about 4 μm, and the aspect ratio is around 67. ZTO nanowires with a Zn/(Zn + Sn) atomic ratio of 0.67 (approximately 2/3) were observed from an energy dispersive spectrometer (EDS). X-ray diffraction (XRD) and corresponding selected area electron diffraction (SAED) patterns demonstrated that the ZTO nanowire is hexagonal single-crystalline. The study of ultraviolet/visible/near-infrared (UV/Vis/NIR) absorption showed that the ZTO nanowire is a wide-band semiconductor with a band gap energy of 3.7 eV.

SeO2 adsorption on CaO surface: DFT and experimental study on the adsorption of multiple SeO2 molecules

NASA Astrophysics Data System (ADS)

Fan, Yaming; Zhuo, Yuqun; Li, Liangliang

2017-10-01

SeO2 adsorption mechanisms on CaO surface were firstly investigated by both density functional theory (DFT) calculations and adsorption experiments. Adsorption of multiple SeO2 on the CaO (001) surface was investigated using slab model. Based on the results of adsorption energy and surface property, a double-layer adsorption mechanisms were proposed. In experiments, the SeO2 adsorption products were prepared in a U-shaped quartz reactor at 200 °C. The surface morphology was investigated by field emission scanning electron microscopy (FE-SEM). The superficial and total SeO2 mass fractions were measured by X-ray photoelectron spectroscopy (XPS) and inductively coupled plasma atomic emission spectroscopy (ICP-AES), respectively. The surface valence state and bulk structure are determined by XPS and X-Ray Diffraction (XRD). The experimental results are in good agreement with the DFT results. In conclusion, the fundamental SeO2 chemisorption mechanisms on CaO surface were suggested.

Ultrasonication of Bismuth Telluride Nanocrystals Fabricated by Solvothermal Method

NASA Technical Reports Server (NTRS)

Chu, Sang-Hyon; Choi, Sang H.; Kim, Jae-Woo; King, Glen C.; Elliott, James R.

2006-01-01

The objective of this study is to evaluate the effect of ultrasonication on bismuth telluride nanocrystals prepared by solvothermal method. In this study, a low dimensional nanocrystal of bismuth telluride (Bi2Te3) was synthesized by a solvothermal process in an autoclave at 180 C and 200 psi. During the solvothermal reaction, organic surfactants effectively prevented unwanted aggregation of nanocrystals in a selected solvent while controlling the shape of the nanocrystal. The atomic ratio of bismuth and tellurium was determined by energy dispersive spectroscopy (EDS). The cavitational energy created by the ultrasonic probe was varied by the ultrasonication process time, while power amplitude remained constant. The nanocrystal size and its size distribution were measured by field emission scanning electron microscopy (FESEM) and a dynamic light scattering system. When the ultrasonication time increased, the average size of bismuth telluride nanocrystal gradually increased due to the direct collision of nanocrystals. The polydispersity of the nanocrystals showed a minimum when the ultrasonication was applied for 5 min. Keywords: bismuth telluride, nanocrystal, low-dimensional, ultrasonication, solvothermal

Immobilization of bacterial S-layer proteins from Caulobacter crescentus on iron oxide-based nanocomposite: synthesis and spectroscopic characterization of zincite-coated Fe₂O₃ nanoparticles.

PubMed

Habibi, Neda

2014-05-05

Zinc oxide was coated on Fe2O3 nanoparticles using sol-gel spin-coating. Caulobacter crescentus have a crystalline surface layer (S-layer), which consist of one protein or glycoprotein species. The immobilization of bacterial S-layers obtained from C. crescentus on zincite-coated nanoparticles of iron oxide was investigated. The SDS PAGE results of S-layers isolated from C. crescentus showed the weight of 50 KDa. Nanoparticles of the Fe2O3 and zinc oxide were synthesized by a sol-gel technique. Fe2O3 nanoparticles with an average size of 50 nm were successfully prepared by the proper deposition of zinc oxide onto iron oxide nanoparticles surface annealed at 450 °C. The samples were characterized by field-emission scanning electron microscope (FESEM), atomic force microscopy (AFM), powder X-ray diffraction (XRD) and Fourier-transform infrared spectroscopy (FT-IR). Copyright © 2014 Elsevier B.V. All rights reserved.

Direct synthesis of nitrogen-containing carbon nanotubes on carbon paper for fuel cell electrode

NASA Astrophysics Data System (ADS)

Yin, Wong Wai; Daud, Wan Ramli Wan; Mohamad, Abu Bakar; Kadhum, Abdul Amir Hassan; Majlan, Edy Herianto; Shyuan, Loh Kee

2012-06-01

Organic catalyst has recently been identified as the potential substitution for expensive platinum electrocatalyst for fuel cell application. Numerous studies have shown that the nitrogen-containing carbon nanotubes (N-CNT) can be synthesized through spray pyrolysis or floating chemical vapor deposition (CVD) technique using various type of organometallic as precursors. This paper presents the method of synthesis and the initial findings of the growth of N-CNT directly on carbon paper using a modified CVD technique. In this research, nickel (II) phthalocyanines (Ni-Pc) as precursor was dissolved in ethanol solvent, stirred and sonicated to become homogenized. The solution was poured into a bubbler and heated up to allow the mixture to vaporize. Subsequently, the solution vapor was flowed into the tubical reactor maintained at 900°C. Carbon paper sputtered with nickel nanoparticles was used as the substrate. The synthesized sample was examined through Field Emission Scanning Electron Microscopy (FESEM), Atomic Force Microscopy (AFM) and Fourier Transform Infra-Red (FTIR). Long, entangled and compartmentalized nanotubes with tube diameter ranging 23-27 nm were found covered the carbon paper surface with approximate of 5.5-6.0 μm in thickness. EDX analysis has successfully showed the presence of nitrogen in the carbon nanotube. FTIR analysis showed the presence of the C-N bond on CNT.

Analysis of the interphase of a polyamide bonded to chromic acid anodized Ti-6AL-4V

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

Guinta, R.K.; Kander, R.G.

2000-01-06

Structural adhesive joints, when tested as made, typically fail cohesively through the centerline of the adhesive. However, in any study of adhesive joint durability, failure near the adhesive/substrate interface becomes an important consideration. In the current study, an interfacially debonding adhesive test, the notched coating adhesion (NCA) test, was applied to LaRC(trademark) PETI-5 adhesive bonded to chronic acid anodized (CAA) Ti-6Al-4V. Post-failure analysis of the interphase region included X-ray photoelectron spectroscopy (XPS), Auger electron spectroscopy (AES), field emission scanning electron microscopy (FE-SEM), and atomic force microscopy (AFM). Mechanical interlocking between an adhesive and a substrate occurs when the liquid adhesivemore » flows into interstices of the substrate, solidifies, and becomes locked in place. Mechanical interlocking is believed to significantly contribute to the adhesion of substrates that exhibit microroughness, such as metal surfaces treated with chromic acid anodization or sodium hydroxide anodization. Filbey and Wightman found that an epoxy penetrated the pores of CAA Ti-6Al-4V, one of the limited number of pore penetration studies that have been reported. In the current study, the penetration of PETI-5 into the pores of CAA Ti-6Al-4V is investigated through analysis of adhesive/substrate failure surfaces.« less

Study of the highly ordered TiO2 nanotubes physical properties prepared with two-step anodization

NASA Astrophysics Data System (ADS)

Pishkar, Negin; Ghoranneviss, Mahmood; Ghorannevis, Zohreh; Akbari, Hossein

2018-06-01

Highly ordered hexagonal closely packed titanium dioxide nanotubes (TiO2 NTs) were successfully grown by a two-step anodization process. The TiO2 NTs were synthesized by electrochemical anodization of titanium foils in an ethylene glycol based electrolyte solution containing 0.3 wt% NH4F and 2 vol% deionized (DI) water at constant potential (50 V) for 1 h at room temperature. Physical properties of the TiO2 NTs, which were prepared via one and two-step anodization, were investigated. Atomic Force Microscopy (AFM) analysis revealed that anodization and subsequently peeled off the TiO2 NTs caused to the periodic pattern on the Ti surface. In order To study the nanotubes morphology, Field Emission Scanning Electron Microscopy (FESEM) was used, which was revealed that the two-step anodization resulted highly ordered hexagonal TiO2 NTs. Crystal structures of the TiO2 NTs were mainly anatase, determined by X-ray diffraction analysis. Optical studies were performed by Diffuse Reflection Spectra (DRS) and Photoluminescence (PL) analysis showed that the band gap of TiO2 NTs prepared via two-step anodization was lower than the band gap of samples prepared by one-step anodization process.

Effect of copper concentration in the electrolyte on the surface morphology and the microstructure of CuInSe2 films

NASA Astrophysics Data System (ADS)

Hung, Pin-Kun; Kuo, Ting-Wei; Huang, Kuo-Chan; Wang, Na-Fu; Hsieh, Po-Tsung; Houng, Mau-Phon

2012-07-01

The surface morphology and the microstructure of CuInSe2 precursor films have been investigated by co-electrodeposition with different [Cu2+] concentrations from 2 mM to 4 mM. The characteristic of the precursor films was examined using field-emission scanning electron microscopy (FE-SEM), energy dispersive X-ray spectroscopy (EDS), glancing incidence angle X-ray diffraction (GIXRD) and micro-Raman spectrometer, respectively. The surface morphology of the precursor films become more smoother and compact with choice of appropriate [Cu2+] concentration (3-3.5 mM) in the electrolyte. The relation between surface morphology and [Cu2+] concentration is also considered in terms of electrodeposition nucleation mechanisms using the mathematical models of Scharifker and Hills. It is suggested that the higher [Cu2+] concentrations can provide more numbers of nucleation sites on the surface of the electrode. Results simulated from the Rietveld refinement method suggest that decreasing dCusbnd Se is related to charge transfer from interstitial copper atoms and can affect the film microstructure. Micro-Raman spectrum also shows that the excess Cu atoms in the precursor films does not contribute significantly to large amounts of secondary phases but rather exists in the crystallite structure as other defect types.

Nanoscale semiconductor Pb1-xSnxSe (x = 0.2) thin films synthesized by electrochemical atomic layer deposition

NASA Astrophysics Data System (ADS)

Lin, Shaoxiong; Zhang, Xin; Shi, Xuezhao; Wei, Jinping; Lu, Daban; Zhang, Yuzhen; Kou, Huanhuan; Wang, Chunming

2011-04-01

In this paper the fabrication and characterization of IV-VI semiconductor Pb1-xSnxSe (x = 0.2) thin films on gold substrate by electrochemical atomic layer deposition (EC-ALD) method at room temperature are reported. Cyclic voltammetry (CV) is used to determine approximate deposition potentials for each element. The amperometric I-t technique is used to fabricate the semiconductor alloy. The elements are deposited in the following sequence: (Se/Pb/Se/Pb/Se/Pb/Se/Pb/Se/Sn …), each period is formed using four ALD cycles of PbSe followed by one cycle of SnSe. Then the deposition manner above is cyclic repeated till a satisfactory film with expected thickness of Pb1-xSnxSe is obtained. The morphology of the deposit is observed by field emission scanning electron microscopy (FE-SEM). X-ray diffraction (XRD) pattern is used to study its crystalline structure; X-ray photoelectron spectroscopy (XPS) of the deposit indicates an approximate ratio 1.0:0.8:0.2 of Se, Pb and Sn, as the expected stoichiometry for the deposit. Open-circuit potential (OCP) studies indicate a good p-type property, and the good optical activity makes it suitable for fabricating a photoelectric switch.

Realization of improved metallization-Ti/Al/Ti/W/Au ohmic contacts to n-GaN for high temperature application

NASA Astrophysics Data System (ADS)

Motayed, A.; Davydov, A. V.; Boettinger, W. J.; Josell, D.; Shapiro, A. J.; Levin, I.; Zheleva, T.; Harris, G. L.

2005-05-01

Tungsten metal layer was used for the first time as an effective diffusion barrier for the standard Ti/Al/Ti/Au ohmic metallization scheme to obtain thermally stable ohmic contact suitable for high temperature applications. Comparative studies were performed on three distinct metallization schemes: 1) standard GaN/Ti/Al/Ti/Au, 2) GaN/Ti/Al/W/Au, and 3) GaN/Ti/Al/Ti/W/Au. For the GaN with doping level of 5 × 1017 cm-3, the lowest specific contact resistance for the Ti/Al/Ti/W/Au metallization scheme annealed in argon at 750 °C for 30 sec was 5 × 10-6 .cm2, which is comparable to the standard Ti/Al/Ti/Au scheme. X-ray diffractions (XRD), auger electron spectroscopy (AES) depth profiling, field-emission scanning electron microscopy (FE-SEM), atomic force microscopy (AFM), and cross-sectional transmission electron microscopy (TEM) revealed that the Ti/Al/Ti/W/Au metallization has superior morphology and microstructural properties compared to standard Ti/Al/Ti/Au metallizations. Remarkably, this metallization was able to withstand thermal aging at 500 °C for 50 hrs with only marginal morphological and electrical deterioration. These studies revealed that the utilization of a compound diffusion barrier stack, as in the Ti/Al/Ti/W/Au metallization, yields electrically, structurally, and morphologically superior metallizations with exceptional thermal stability.

Biosynthesis of silver nanoparticles from Cavendish banana peel extract and its antibacterial and free radical scavenging assay: a novel biological approach

NASA Astrophysics Data System (ADS)

Kokila, T.; Ramesh, P. S.; Geetha, D.

2015-12-01

Biosynthesis of metallic silver nanoparticles has now become an alternative to physical and chemical approaches. In the present study, silver nanoparticles (AgNPs) were synthesized from Cavendish banana peel extract (CBPE) and characterized by UV-visible spectroscopy, X-ray diffraction (XRD), Fourier transform infrared (FT-IR) spectroscopy, Atomic force microscopy (AFM), Field emission scanning electronic microscope (FESEM), Dynamic light scattering (DLS) and zeta potential (ZP). The AgNPs formation was confirmed by UV-visible spectroscopy through color conversion due to surface plasma resonance band at 430 nm. The effect of pH on nanoparticle synthesis was determined by adjusting the various pH of the reaction mixtures. The crystalline nature of nanoparticles was confirmed from the XRD pattern, and the grain size was found to be around 34 nm. To identify the compounds responsible for the bioreduction of Ag+ ion and the stabilization of AgNPs produced, the functional group present in Cavendish banana peel extract was investigated using FTIR. AFM has proved to be very helpful in determining morphological features and the diameter of AgNPs in the range of 23-30 nm was confirmed by FESEM. DLS studies revealed that the average size of AgNPs was found to be around 297 nm. Zeta potential value for AgNPs obtained was -11 mV indicating the moderate stability of synthesized nanoparticles. The antibacterial activity of the nanoparticles was studied against Gram-positive and Gram-negative bacteria. Biosynthesized AgNPs showed a strong DPPH radical and ABTS scavengers compared to the aqueous peel extract of Cavendish banana.

The Effect of Cu:Ag Atomic Ratio on the Properties of Sputtered Cu–Ag Alloy Thin Films

PubMed Central

Hsieh, Janghsing; Hung, Shunyang

2016-01-01

Cu–Ag thin films with various atomic ratios were prepared using a co-sputtering technique, followed by rapid thermal annealing at various temperatures. The films’ structural, mechanical, and electrical properties were then characterized using X-ray diffractometry (XRD), atomic force microscopy (AFM), FESEM, nano-indentation, and TEM as functions of compositions and annealing conditions. In the as-deposited condition, the structure of these films transformed from a one-phase to a dual-phase state, and the resistivity shows a twin-peak pattern, which can be explained in part by Nordheim’s Rule and the miscibility gap of Cu–Ag alloy. After being annealed, the films’ resistivity followed the mixture rule in general, mainly due to the formation of a dual-phase structure containing Ag-rich and Cu-rich phases. The surface morphology and structure also varied as compositions and annealing conditions changed. The recrystallization of these films varied depending on Ag–Cu compositions. The annealed films composed of 40 at % to 60 at % Cu had higher hardness and lower roughness than those with other compositions. Particularly, the Cu50Ag50 film had the highest hardness after being annealed. From the dissolution testing, it was found that the Cu-ion concentration was about 40 times higher than that of Ag. The galvanic effect and over-saturated state could be the cause of the accelerated Cu dissolution and the reduced dissolution of the Ag. PMID:28774033

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

Pan Qingtao; Huang Kai; Ni Shibing

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

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

NASA Astrophysics Data System (ADS)

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

2018-05-01

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

TEM Study of SAFARI-2000 Aerosols

NASA Technical Reports Server (NTRS)

Buseck, Peter R.

2004-01-01

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

Template confined synthesis of amorphous carbon nanotubes and its confocal Raman microscopy

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

Maity, Supratim; Roychowdhury, Tuhin; Chattopadhyay, Kalyan Kumar, E-mail: kalyan-chattopadhyay@yahoo.com

2014-04-24

Amorphous carbon nanotubes (aCNTs) were synthesized by AAO (anodic aluminum oxide) template at a temperature 500 °C in nitrogen atmosphere using the citric acid as a carbon source without the help of any catalyst particles. Morphological analysis of the as prepared samples was carried out by field emission scanning electron microscopy (FESEM). Confocal Raman imaging has been studied and an attempt has been made to find out the graphitic (sp{sup 2}) and disordered phase of the CNTs.

Direct Growth of CuO Nanorods on Graphitic Carbon Nitride with Synergistic Effect on Thermal Decomposition of Ammonium Perchlorate

PubMed Central

Tan, Linghua; Xu, Jianhua; Li, Shiying; Li, Dongnan; Dai, Yuming; Kou, Bo; Chen, Yu

2017-01-01

Novel graphitic carbon nitride/CuO (g-C3N4/CuO) nanocomposite was synthesized through a facile precipitation method. Due to the strong ion-dipole interaction between copper ions and nitrogen atoms of g-C3N4, CuO nanorods (length 200–300 nm, diameter 5–10 nm) were directly grown on g-C3N4, forming a g-C3N4/CuO nanocomposite, which was confirmed via X-ray diffraction (XRD), transmission electron microscopy (TEM), field emission scanning electron microscopy (FESEM), and X-ray photoelectron spectroscopy (XPS). Finally, thermal decomposition of ammonium perchlorate (AP) in the absence and presence of the prepared g-C3N4/CuO nanocomposite was examined by differential thermal analysis (DTA), and thermal gravimetric analysis (TGA). The g-C3N4/CuO nanocomposite showed promising catalytic effects for the thermal decomposition of AP. Upon addition of 2 wt % nanocomposite with the best catalytic performance (g-C3N4/20 wt % CuO), the decomposition temperature of AP was decreased by up to 105.5 °C and only one decomposition step was found instead of the two steps commonly reported in other examples, demonstrating the synergistic catalytic activity of the as-synthesized nanocomposite. This study demonstrated a successful example regarding the direct growth of metal oxide on g-C3N4 by ion-dipole interaction between metallic ions, and the lone pair electrons on nitrogen atoms, which could provide a novel strategy for the preparation of g-C3N4-based nanocomposite. PMID:28772844

Imaging interactions of metal oxide nanoparticles with macrophage cells by ultra-high resolution scanning electron microscopy techniques†

PubMed Central

Plascencia-Villa, Germán; Starr, Clarise R.; Armstrong, Linda S.; Ponce, Arturo

2016-01-01

Use of engineered metal oxide nanoparticles in a plethora of biological applications and custom products has warned about some possible dose-dependent cytotoxic effects. Macrophages are key components of the innate immune system used to study possible toxic effects and internalization of different nanoparticulate materials. In this work, ultra-high resolution field emission scanning electron microscopy (FE-SEM) was used to offer new insights into the dynamical processes of interaction of nanomaterials with macrophage cells dosed with different concentrations of metal oxide nanoparticles (CeO2, TiO2 and ZnO). The versatility of FE-SEM has allowed obtaining a detailed characterization of processes of adsorption and endocytosis of nanoparticles, by using advanced analytical and imaging techniques on complete unstained uncoated cells, including secondary electron imaging, high-sensitive backscattered electron imaging, X-ray microanalysis and stereoimaging. Low voltage BF/DF-STEM confirmed nanoparticle adsorption and internalization into endosomes of CeO2 and TiO2, whereas ZnO develop apoptosis after 24 h of interaction caused by dissolution and invasion of cell nucleus. Ultra-high resolution scanning electron microscopy techniques provided new insights into interactions of inorganic nanoparticles with macrophage cells with high spatial resolution. PMID:23023106

The Evaluation of Hydroxyapatite (HA) Coated and Uncoated Porous Tantalum for Biomedical Material Applications

NASA Astrophysics Data System (ADS)

Safuan, Nadia; Sukmana, Irza; Kadir, Mohammed Rafiq Abdul; Noviana, Deni

2014-04-01

Porous tantalum has been used as an orthopedic implant for bone defects as it has a good corrosion resistance and fatigue behaviour properties. However, there are some reports on the rejection of porous Ta after the implantation. Those clinical cases refer to the less bioactivity of metallic-based materials. This study aims to evaluate hydroxyapatite coated and uncoated porous Tantalum in order to improve the biocompatibility of porous tantalum implant and osseointegration. Porous tantalum was used as metallic-base substrate and hydroxyapatite coating has been done using plasma-spraying technique. Scanning Electron Microscopy (SEM) and Field Emission Scanning Electron Microscopy (FESEM) techniques were utilizes to investigate the coating characteristics while Confocal Raman Microscopy to investigate the interface and image. The effect of coating to the corrosion behaviour was assessed by employing potentiodynamic polarization tests in simulated body fluid at 37±1 °C. Based on SEM and FESEM results, the morphologies as well the weight element consists in the uncoated and hydroxyapatite coated porous tantalum were revealed. The results indicated that the decrease in corrosion current density for HA coated porous Ta compared to the uncoated porous Ta. This study concluded that by coating porous tantalum with HA supports to decrease the corrosion rate of pure porous.

Silver nanoparticles embedded mesoporous SiO2 nanosphere: an effective anticandidal agent against Candida albicans 077

NASA Astrophysics Data System (ADS)

Qasim, M.; Singh, Braj R.; Naqvi, A. H.; Paik, P.; Das, D.

2015-07-01

Candida albicans is a diploid fungus that causes common infections such as denture stomatitis, thrush, urinary tract infections, etc. Immunocompromised patients can become severely infected by this fungus. Development of an effective anticandidal agent against this pathogenic fungus, therefore, will be very useful for practical application. In this work, Ag-embedded mesoporous silica nanoparticles (mSiO2@AgNPs) have successfully been synthesized and their anticandidal activities against C. albicans have been studied. The mSiO2@AgNPs nanoparticles (d ˜ 400 nm) were designed using pre-synthesized Ag nanoparticles and tetraethyl orthosilicate (TEOS) as a precursor for SiO2 in the presence of cetyltrimethyl ammonium bromide (CTAB) as an easily removable soft template. A simple, cost-effective, and environmentally friendly approach has been adopted to synthesize silver (Ag) nanoparticles using silver nitrate and leaf extract of Azadirachta indica. The mesopores, with size-equivalent diameter of the micelles (d = 4-6 nm), were generated on the SiO2 surface by calcination after removal of the CTAB template. The morphology and surface structure of mSiO2@AgNPs were characterized through x-ray diffraction (XRD), Fourier-transform infrared spectroscopy (FTIR), particle size analysis (PSA), atomic force microscopy (AFM), field emission scanning electron microscopy (FESEM), Brunauer-Emmett-Teller (BET) and high-resolution transmission electron microscopy (HRTEM). The HRTEM micrograph reveals the well-ordered mesoporous structure of the SiO2 sphere. The antifungal activities of mSiO2@AgNPs on the C. albicans cell have been studied through microscopy and are seen to increase with increasing dose of mSiO2@AgNPs, suggesting mSiO2@AgNPs to be a potential antifungal agent for C. albicans 077.

Structural and biological evaluation of a multifunctional SWCNT-AgNPs-DNA/PVA bio-nanofilm.

PubMed

Subbiah, Ramesh P; Lee, Haisung; Veerapandian, Murugan; Sadhasivam, Sathya; Seo, Soo-Won; Yun, Kyusik

2011-04-01

A bio-nanofilm consisting of a tetrad nanomaterial (nanotubes, nanoparticles, DNA, polymer) was fabricated utilizing in situ reduction and noncovalent interactions and it displayed effective antibacterial activity and biocompatibility. This bio-nanofilm was composed of homogenous silver nanoparticles (AgNPs) coated on single-walled carbon nanotubes (SWCNTs), which were later hybridized with DNA and stabilized in poly(vinyl alcohol) (PVA) in the presence of a surfactant with the aid of ultrasonication. Electron microscopy and bio-AFM (atomic force microscopy) images were used to assess the morphology of the nanocomposite (NC) structure. Functionalization and fabrication were examined using FT-Raman spectroscopy by analyzing the functional changes in the bio-nanofilm before and after fabrication. UV-visible spectroscopy and X-ray powder diffraction (XRD) confirmed that AgNPs were present in the final NC on the basis of its surface plasmon resonance (370 nm) and crystal planes. Thermal gravimetric analysis was used to measure the percentage weight loss of SWCNT (17.5%) and final SWCNT-AgNPs-DNA/PVA (47.7%). The antimicrobial efficiency of the bio-nanofilm was evaluated against major pathogenic organisms. Bactericidal ratios, zone of inhibition, and minimum inhibitory concentration were examined against gram positive and gram negative bacteria. A preliminary cytotoxicity analysis was conducted using A549 lung cancer cells and IMR-90 fibroblast cells. Confocal laser microscopy, bio-AFM, and field emission scanning electron microscopy (FE-SEM) images demonstrated that the NCs were successfully taken up by the cells. These combined results indicate that this bio-nanofilm was biocompatible and displayed antimicrobial activity. Thus, this novel bio-nanofilm holds great promise for use as a multifunctional tool in burn therapy, tissue engineering, and other biomedical applications.

In situ preparation of MgCo2O4 nanosheets on Ni-foam as a binder-free electrode for high performance hybrid supercapacitors.

PubMed

Vijayakumar, Subbukalai; Nagamuthu, Sadayappan; Ryu, Kwang-Sun

2018-05-15

A binder-free, MgCo2O4 nanosheet-like architecture was prepared on Ni-foam using a hydrothermal method. MgCo2O4/Ni-foam was characterized by X-ray diffraction, field emission scanning electron microscopy (FESEM), and transmission electron microscopy techniques. The FESEM image revealed a nanosheet array-like architecture. The MgCo2O4 nanosheets grown on Ni-foam exhibited the maximum specific capacity of 947 C g-1 at a specific current of 2 A g-1. Approximately 96% of the specific capacity was retained from the maximum specific capacity after 5000 continuous charge-discharge cycles. This hybrid device exhibited a maximum specific capacity of 52 C g-1 at a specific current of 0.5 A g-1, and also exhibited a maximum specific energy of 12.99 W h kg-1 at a specific power of 448.7 W kg-1. These results confirmed that the binder-free MgCo2O4 nanosheets grown on Ni-foam are a suitable positive electrode material for hybrid supercapacitors.

Fabrication of TiO2 nanostructures on porous silicon for thermoelectric application

NASA Astrophysics Data System (ADS)

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

2017-09-01

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

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

NASA Astrophysics Data System (ADS)

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

2017-10-01

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

Cytotoxicity Evaluation and Magnetic Characteristics of Mechano-thermally Synthesized CuNi Nanoparticles for Hyperthermia

NASA Astrophysics Data System (ADS)

Amrollahi, P.; Ataie, A.; Nozari, A.; Seyedjafari, E.; Shafiee, A.

2015-03-01

CuNi alloys are very well known, both in academia and industry, based on their wide range of applications. In the present investigation, the previously synthesized Cu0.5Ni0.5 nanoparticles (NPs) by mechano-thermal method were studied more extensively. Phase composition and morphology of the samples were studied by employing x-ray diffraction (XRD), field-emission scanning electron microscopy (FESEM), and transmission electron microscopy (TEM) techniques. The Curie temperature ( T c) was determined by differential scanning calorimetry (DSC). In vitro cytotoxicity was studied through methyl-thiazolyl-tetrazolium (MTT) assay. XRD and FESEM results indicated the formation of single-phase Cu0.5Ni0.5. TEM micrographs showed that the mean particle size of powders is 20 nm. DSC results revealed that T c of mechano-thermally synthesized Cu0.5Ni0.5 is 44 °C. The MTT assay results confirmed the viability and proliferation of human bone marrow stem cells in contact with Cu0.5Ni0.5 NPs. In summary, the fabricated particles were demonstrated to have potential in low concentrations for cancer treatment applications.

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

PubMed

Baniasad, Arezou; Ghorbani, Mohsen

2016-05-01

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

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

NASA Astrophysics Data System (ADS)

Hansora, D. P.; Shimpi, N. G.; Mishra, S.

2015-12-01

This work represents a state-of-the-art technique developed for the preparation of graphene from graphite-metal electrodes by the arc-discharge method carried out in a continuous flow of water. Because of continuous arcing of graphite-metal electrodes, the graphene sheets were observed in water with uniformity and little damage. These nanosheets were subjected to various purification steps such as acid treatment, oxidation, water washing, centrifugation, and drying. The pure graphene sheets were analyzed using Raman spectrophotometry, x-ray diffraction (XRD), field emission-scanning electron microscopy (FE-SEM), and tunneling electron microscopy (TEM). Peaks of Raman spectra were recorded at (1300-1400 cm-1) and (1500-1600 cm-1) for weak D-band and strong G-band, respectively. The XRD pattern showed 85.6% crystallinity of pure graphite, whereas pure graphene was 66.4% crystalline. TEM and FE-SEM micrographs revealed that graphene sheets were overlapped to each other and layer-by-layer formation was also observed. Beside this research work, we also reviewed recent developments of graphene and related nanomaterials along with their preparations, properties, functionalizations, and potential applications.

Performance of RF sputtered p-Si/n-ZnO nanoparticle thin film heterojunction diodes in high temperature environment

NASA Astrophysics Data System (ADS)

Singh, Satyendra Kumar; Hazra, Purnima

2017-04-01

In this article, temperature-dependent current-voltage characteristics of n-ZnO/p-Si nanoparticle thin film heterojunction diode grown by RF sputtering technique are analyzed in the temperature range of 300-433 k to investigate the performance of the device in high temperature environment. The microstructural, morphological, optical and temptrature dependent electrical properties of as-grown nanoparticle thin film were characterized by X-ray diffractometer (XRD), atomic force microscopy (AFM), field emmision scanning electron microscopy (FESEM), energy-dispersive X-ray spectroscopy (EDX), variable angle ellipsometer and semiconductor device analyzer. XRD spectra of as-grown ZnO films are exhibited that highly c-axis oriented ZnO nanostructures are grown on p- Si〈100〉 substrate whereas AFM and FESEM images confirm the homogeneous deposition of ZnO nanoparticles on surface of Si substratewith minimum roughness.The optical propertiesof as-grown ZnO nanoparticles have been measured in the spectral range of 300-800 nm using variable angle ellipsometer.To measure electrical parameters of the device prototype in the temperature range of room temperature (300 K) to 433 K, large area ohmic contacts were fabricated on both side of the ZnO/Si heterostructure. From the current-voltage charcteristics of ZnO/Si heterojunction device, it is observed that the device exhibits rectifing nature at room temperature. However, with increase in temperature, reverse saturation current and barrier height are found to increase, whereas ideality factor is started decreasing. This phenomenon confirms that barrier inhomogeneities are present at the interface of ZnO/Si heterojunction, as a result of lattice constant and thermal coefficient mismatch between Si and ZnO. Therefore, a modified value of Richardson constant [33.06 Acm-2K-2] has been extracted from the temperature-dependent electrical characteristics after assuming the Gaussian distribution of special barrier height inhomogeneities across the Si/ZnO interface which is close to its theoretical value [32 Acm-2K-2]. This result indicates that regardless of presence of barrier height inmogeneities, ZnO/Si heterojunction diode still hasability to perform well in high temperature environment.

Bone healing and mineralization, implant corrosion, and trace metals after nickel-titanium shape memory metal intramedullary fixation.

PubMed

Ryhänen, J; Kallioinen, M; Serlo, W; Perämäki, P; Junila, J; Sandvik, P; Niemelä, E; Tuukkanen, J

1999-12-15

Its shape memory effect, superelasticity, and good wear and damping properties make the NiTi shape memory alloy a material with fascinating potential for orthopedic surgery. It provides a possibility for making self-locking, self-expanding, and self-compressing implants. Problems, however, may arise because of its high nickel content. The purpose of this work was to determine the corrosion of NiTi in vivo and to evaluate the possible deleterious effects of NiTi on osteotomy healing, bone mineralization, and the remodeling response. Femoral osteotomies of 40 rats were fixed with either NiTi or stainless steel (StSt) intramedullary nails. The rats were killed at 2, 4, 8, 12, 26, and 60 weeks. Bone healing was examined with radiographs, peripheral quantitative computed tomography, (pQCT) and histologically. The corrosion of the retrieved implants was analyzed by electron microscopy (FESEM). Trace metals from several organs were determined by graphite furnace atomic absorption spectrometry (GF-AAS) or by inductively coupled plasma-atomic emission spectrometry (ICP-AES). There were more healed bone unions in the NiTi than in the StSt group at early (4 and 8 weeks) time points. Callus size was equal between the groups. The total and cortical bone mineral densities did not differ between the NiTi and StSt groups. Mineral density in both groups was lower in the osteotomy area than in the other areas along the nail. Density in the nail area was lower than in the proximal part of the operated femur or the contralateral femur. Bone contact to NiTi was close. A peri-implant lamellar bone sheet formed in the metaphyseal area after 8 weeks, indicating good tissue tolerance. The FESEM assessment showed surface corrosion changes to be more evident in the StSt implants. There were no statistically significant differences in nickel concentration between the NiTi and StSt groups in any of the organs. NiTi appears to be an appropriate material for further intramedullary use because it has good biocompatibility in bone tissue. Copyright 1999 John Wiley & Sons, Inc.

Effect of RF power density on micro- and macro-structural properties of PECVD grown hydrogenated nanocrystalline silicon thin films

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

Gokdogan, Gozde Kahriman, E-mail: gozdekahriman@gmail.com; Anutgan, Tamila, E-mail: tamilaanutgan@karabuk.edu.tr

2016-03-25

This contribution provides the comparison between micro- and macro-structure of hydrogenated nanocrystalline silicon (nc-Si:H) thin films grown by plasma enhanced chemical vapor deposition (PECVD) technique under different RF power densities (P{sub RF}: 100−444 mW/cm{sup 2}). Micro-structure is assessed through grazing angle X-ray diffraction (GAXRD), while macro-structure is followed by surface and cross-sectional morphology via field emission scanning electron microscopy (FE-SEM). The nanocrystallite size (∼5 nm) and FE-SEM surface conglomerate size (∼40 nm) decreases with increasing P{sub RF}, crystalline volume fraction reaches maximum at 162 mW/cm{sup 2}, FE-SEM cross-sectional structure is columnar except for the film grown at 162 mW/cm{sup 2}. The dependence of previously determinedmore » ‘oxygen content–refractive index’ correlation on obtained macro-structure is investigated. Also, the effect of P{sub RF} is discussed in the light of plasma parameters during film deposition process and nc-Si:H film growth models.« less

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

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

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

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

Influence of gamma irradiation on polymerization of pyrrole and glucose oxidase immobilization onto poly (pyrrole)/poly (vinyl alcohol) matrix

NASA Astrophysics Data System (ADS)

Idris, Sarada; A. Bakar, Ahmad Ashrif; Thevy Ratnam, Chantara; Kamaruddin, Nur Hasiba; Shaari, Sahbudin

2017-04-01

This paper describes the immobilization of glucose oxidase, GOx onto polymer matrix comprising of poly(pyrrole), PPy and poly(vinyl alcohol), PVA using gamma irradiation technique. Py/PVA-GOx film was prepared by spreading PVA:GOx, 1:1 solution onto dried pyrrole film and exposed to gamma irradiation from cobalt 60 source at doses ranging from 0 to 60 kGy. The films were subjected to structural and morphological analyses by using Fourier transform infrared spectroscopy (FTIR), X-ray photoelectron spectroscopy (XPS), Scanning electron microscope (SEM), Field emission scanning electron microscope (FESEM) and Atomic-force microscopy (AFM) techniques. Similar studies were also made on pristine pyrrole film which served as control. The SEM and FTIR spectra of Py/PVA-GOx film revealed that pyrrole has been successfully polymerized through irradiation-induced reactions. The results on the morphological properties of the samples characterize using FESEM, SEM and AFM further confirmed the occurrence of radiation-induced modification of Py/PVA-GOx film. The FTIR spectra showed the existence of intermolecular interaction between polymer matrix and GOx indicating that GOx had been successfully immobilized onto Ppy/PVA matrix by radiation-induced reactions. Results revealed that radiation induced reactions such as polymerization of pyrrole, crosslinking of PVA, grafting between the adjacent PVA and pyrrole molecules as well as immobilization of GOx onto Ppy/PVA matrix occurred simultaneously upon gamma irradiation. The optimum dose for GOx immobilization in the polymer matrix found to be 40 kGy. Therefore it is clear that this irradiation technique offered a simple single process to produce Py/PVA-GOx film without additional crosslinking and polymerization agents.

Phase Competition Induced Bio-Electrochemical Resistance and Bio-Compatibility Effect in Nanocrystalline Zr x -Cu100-x Thin Films.

PubMed

Badhirappan, Geetha Priyadarshini; Nallasivam, Vignesh; Varadarajan, Madhuri; Leobeemrao, Vasantha Priya; Bose, Sivakumar; Venugopal, Elakkiya; Rajendran, Selvakumar; Angleo, Peter Chrysologue

2018-07-01

Nano-crystalline Zrx-Cu100-x (x = 20-100 at.%) thin films with thickness ranging from 50 to 185 nm were deposited by magnetron co-sputtering with individual Zr and Cu targets. The as-sputtered thin films were characterized by Field Emission Scanning Electron Microscope (FE-SEM), Atomic Force Microscopy (AFM) and Glancing Incidence X-ray Diffraction (GIXRD) for structural and morphological properties. The crystallite size was found to decrease from 57 nm to 37 nm upon increasing the Zr content from 20 to 30 at.% with slight increase in the lattice strain from 0.17 to 0.33%. Further, increase in Zr content to 40 at.% leads to increase in the crystallite size to 57 nm due to stabilization of C10Zr7 phase along with the presence of nanocrystalline Cu-Zr phase. A bimodal distribution of grain size was observed from FE-SEM micrograph was attributed to the highest surface roughness in Zr30Cu70 thin films comprised of Cu10Zr7, Cu9Zr2, Cu-Zr intermetallic phases. In-vitro electrochemical behaviors of nano-crystalline Zrx-Cu100-x thin films in simulated body fluid (SBF) were investigated using potentiodynamic polarization studies. Electrochemical impedance spectroscopy (EIS) data fitting by equivalent electrical circuit fit model suggests that inner bulk layer contributes to high bio-corrosion resistance in Zrx-Cu100-x thin films with increase in Zr content. The results of cyto-compatibility assay suggested that Zr-Cu thin film did not introduce cytotoxicity to osteoblast cells, indicating its suitability as a bio-coating for minimally invasive medical devices.

The optimization of CNT-PVA nanocomposite for mild steel coating: Effect of CNTs concentration on the corrosion rate of mild steel

NASA Astrophysics Data System (ADS)

Maryam, M.; Ibrahim, N. M. A. A.; Eswar, K. A.; Guliling, M.; Suhaimi, M. H. F.; Khusaimi, Z.; Abdullah, S.; Rusop, M.

2018-05-01

Carbon Nanotubes (CNTs) are molecular-scale tubes of graphitic carbon which have outstanding mechanical and magnetic properties with extraordinary strength. It can be said that CNTs can be used in coating application to prevent corrosion and lower the rate of corrosion on steel. However, CNT alone cannot be used for coating purposes. Therefore, by combining it with polymer to produce a nanocomposite thin film, it can be used for nanocoating on mild steel substrate. Polyvinyl alcohol (PVA) was chosen due to its high strength and high modulus polymer fibers and has the possibilities of improving the physicochemical properties of carbon nanotubes. Carbon nanotubes and polyvinyl alcohol (CNT-PVA) nanocomposite were prepared by using sol-gel method and coated as thin film on mild steel substrate by using spin coating. Sol-gel is a convenient technique used for the production of nanocomposite aqueous solution. Five samples were prepared at the different concentration of CNTs-PVA to verify the corrosion rate application. The samples were then characterized by Field Emission Scanning Electron Microscopy (FESEM) and Atomic Force Microscopy (AFM) obtaining the structural properties, surface morphology and topography of samples. Raman spectroscopy was used to determine the microraman spectra of CNTs which showed the quality and purity of samples. Finally, corrosion test was done to measure the corrosion rate of samples at the different concentration of CNTs/PVA nanocomposite.

Effect of perfluorodecyltrichlorosilane on the surface properties and anti-corrosion behavior of poly(dimethylsiloxane)-ZnO coatings

NASA Astrophysics Data System (ADS)

Arukalam, Innocent O.; Meng, Meijiang; Xiao, Haigang; Ma, Yuantai; Oguzie, Emeka E.; Li, Ying

2018-03-01

Poly(dimethylsiloxane)-ZnO coatings modified with different amounts of perfluorodecyltrichlorosilane (FDTS) were prepared using sol-gel technique. The results of field emission scanning electron microscopy (FESEM) and atomic force microscopy (AFM) examinations showed that the surface structures and roughness of the coatings were respectively influenced by the increasing addition of FDTS. The water contact angle measurements showed maximum value of 130.52° with the 0.10 g FDTS-modified coating sample. The X-ray photoelectron spectroscopy (XPS) results indicated the coatings' hydrophobicity was also influenced by surface chemistry. The FTIR-ATR characterization results showed there was remarkable increase in the crystallinity of 0.10 g FDTS-modified coating after modification, and was confirmed by differential scanning calorimetry (DSC) analysis of crystallization temperature and the X-ray diffraction (XRD) results with an estimation of 71.29% percent crystallinity. The mechanical properties of the coatings were also conducted. The EIS measurements for anti-corrosion behavior showed that 0.10 g FDTS-modified coating had the highest barrier performance and lowest rate of degradation. Indeed, the obtained data have demonstrated that 0.10 g (≈ 0.18%) FDTS produced the most significantly effect on the surface and barrier properties of the coatings and thus, can effectively be used for anti-corrosion application in the marine environments.

Penicillin biosensor based on a capacitive field-effect structure functionalized with a dendrimer/carbon nanotube multilayer.

PubMed

Siqueira, José R; Abouzar, Maryam H; Poghossian, Arshak; Zucolotto, Valtencir; Oliveira, Osvaldo N; Schöning, Michael J

2009-10-15

Silicon-based sensors incorporating biomolecules are advantageous for processing and possible biological recognition in a small, reliable and rugged manufactured device. In this study, we report on the functionalization of field-effect (bio-)chemical sensors with layer-by-layer (LbL) films containing single-walled carbon nanotubes (SWNTs) and polyamidoamine (PAMAM) dendrimers. A capacitive electrolyte-insulator-semiconductor (EIS) structure modified with carbon nanotubes (EIS-NT) was built, which could be used as a penicillin biosensor. From atomic force microscopy (AFM) and field-emission scanning electron microscopy (FESEM) images, the LbL films were shown to be highly porous due to interpenetration of SWNTs into the dendrimer layers. Capacitance-voltage (C/V) measurements pointed to a high pH sensitivity of ca. 55 mV/pH for the EIS-NT structures. The biosensing ability towards penicillin of an EIS-NT-penicillinase biosensor was also observed as the flat-band voltage shifted to lower potentials at different penicillin concentrations. A dynamic response of penicillin concentrations, ranging from 5.0 microM to 25 mM, was evaluated for an EIS-NT with the penicillinase enzyme immobilized onto the surfaces, via constant-capacitance (ConCap) measurements, achieving a sensitivity of ca. 116 mV/decade. The presence of the nanostructured PAMAM/SWNT LbL film led to sensors with higher sensitivity and better performance.

Effect of thickness on surface morphology, optical and humidity sensing properties of RF magnetron sputtered CCTO thin films

NASA Astrophysics Data System (ADS)

Ahmadipour, Mohsen; Ain, Mohd Fadzil; Ahmad, Zainal Arifin

2016-11-01

In this study, calcium copper titanate (CCTO) thin films were deposited on ITO substrates successfully by radio frequency (RF) magnetron sputtering method in argon atmosphere. The CCTO thin films present a polycrystalline, uniform and porous structure. The surface morphology, optical and humidity sensing properties of the synthesized CCTO thin films have been studied by X-ray diffraction (XRD), atomic force microscopy (AFM), field emission scanning electron microscopy (FESEM), energy-dispersive X-ray spectroscopy (EDX), UV-vis spectrophotometer and current-voltage (I-V) analysis. XRD and AFM confirmed that the intensity of peaks and pore size of CCTO thin films were enhanced by increasing the thin films. Tauc plot method was adopted to estimate the optical band gaps. The surface structure and energy band gaps of the deposited films were affected by film thickness. Energy band gap of the layers were 3.76 eV, 3.68 eV and 3.5 eV for 200 nm, 400 nm, and 600 nm CCTO thin films layer, respectively. The humidity sensing properties were measured by using direct current (DC) analysis method. The response times were 12 s, 22 s, and 35 s while the recovery times were 500 s, 600 s, and 650 s for 200 nm, 400 nm, and 600 nm CCTO thin films, respectively at humidity range of 30-90% relative humidity (RH).

Highly sensitive NO2 sensor using brush-coated ZnO nanoparticles

NASA Astrophysics Data System (ADS)

Chandra, Lalit; Dwivedi, R.; Mishra, V. N.

2017-10-01

This work reports the sensing properties of a ZnO nanoparticle (NP) based gas sensor. A sol-gel method was used for the synthesis of ZnO nanoparticles, and a brush coating technique for applying these in a thick film over the gold electrode. The structural properties of the ZnO film so developed have been studied using energy dispersive x-ray spectroscopy (EDS), x-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM) and atomic force microscopy (AFM), revealing a hexagonal wurtzite structure having particle size of ~25 to ~110 nm and roughness of ~136.303 nm. The sensitivity of the sensor to NO2, H2, CO, ethanol and propanol gases in the temperature range from 150 to 350 °C has been tested. Among all these gases, sensitivity to NO2 was found to be highest, at around fifty times greater than the next highest sensitivity, for ethanol gas. The sensor’s response to NO2 gas has been measured at ~945.12%/ppt (parts per thousand), with fast response time and recovery time at operating temperature 280 °C. The obtained result has been discussed with the help of surface and subsurface adsorption and desorption of NO2 molecules at the available trap sites (oxygen ions) on the ZnO nanoparticle surface. This sensor also exhibits excellent repeatability.

Improving protein resistance of α-Al 2O 3 membranes by modification with POEGMA brushes

NASA Astrophysics Data System (ADS)

He, Huating; Jing, Wenheng; Xing, Weihong; Fan, Yiqun

2011-11-01

A kind of protein-resistant ceramic membrane is prepared by grafting poly(oligo (ethylene glycol) methyl ether methacrylate) (POEGMA) brushes onto the surfaces and pore walls of α-Al2O3 membrane (AM) by surface-initiated atom-transfer radical polymerization (SI-ATRP). Contact-angle, Fourier-transform infrared spectroscopy (FTIR), thermogravimetric analysis (TGA) and field-emission scanning electron microscopy (FESEM) were measured to confirm that the surfaces and pore walls of the ceramic porous membranes have been modified by the brushes with this method successfully. The protein interaction behavior with the POEGMA modified membranes (AM-POEGMA) was studied by the model protein of bovine serum albumin (BSA). A protein-resistant mechanism of AM-POEGMA was proposed to describe an interesting phenomenon discovered in the filtration experiment, in which the initial flux filtrating BSA solution is higher than the pure water flux. The fouling of AM-POEGMA was easier to remove than AM for the action of POEGMA brushes, indicated that the ceramic porous membranes modified with POEGMA brushes exhibit excellent protein resistance.

Surface studies on superhydrophobic and oleophobic polydimethylsiloxane-silica nanocomposite coating system

NASA Astrophysics Data System (ADS)

Basu, Bharathibai J.; Dinesh Kumar, V.; Anandan, C.

2012-11-01

Superhydrophobic and oleophobic polydimethylsiloxane (PDMS)-silica nanocomposite double layer coating was fabricated by applying a thin layer of low surface energy fluoroalkyl silane (FAS) as topcoat. The coatings exhibited WCA of 158-160° and stable oleophobic property with oil CA of 79°. The surface morphology was characterized by field emission scanning electron microscopy (FESEM) and surface chemical composition was determined by energy dispersive X-ray spectrometery (EDX) and X-ray photoelectron spectroscopy (XPS). FESEM images of the coatings showed micro-nano binary structure. The improved oleophobicity was attributed to the combined effect of low surface energy of FAS and roughness created by the random distribution of silica aggregates. This is a facile, cost-effective method to obtain superhydrophobic and oleophobic surfaces on larger area of various substrates.

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

NASA Astrophysics Data System (ADS)

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

2017-11-01

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

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

NASA Astrophysics Data System (ADS)

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

2017-05-01

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

Efficacy of ferulic acid encapsulated chitosan nanoparticles against Candida albicans biofilm.

PubMed

Panwar, Richa; Pemmaraju, Suma C; Sharma, Asvene K; Pruthi, Vikas

2016-06-01

Candida albicans, an opportunistic fungal pathogen is a major causative agent of superficial to systemic life-threating biofilm infections on indwelling medical devices. These biofilms acts as double edge swords owing to their resistance towards antibiotics and immunological barriers. To overcome this threat ferulic acid encapsulated chitosan nanoparticles (FA-CSNPs) were formulated to assess its efficacy as an antibiofilm agent against C. albicans. These FA-CSNPs were synthesized using ionotropic gelation method and observed through field emission scanning electron microscopy (FESEM) and fluorescent microscopy. Assessment of successful encapsulation and stability of ferulic acid into chitosan nanoparticles was made using Fourier transform infrared spectrum (FTIR), (1)H NMR and thermal analyses. Synthesized FA-CSNPs, were found to be cytocompatible, when tested using Human Embryonic Kidney (HEK-293) cell lines. XTT assay revealed that FA-CSNPs reduced the cell metabolic activity of C. albicans upto 22.5% as compared to native ferulic acid (63%) and unloaded CSNPs (88%) after 24 h incubation. Disruption of C. albicans biofilm architecture was visualized by FESEM. Results highlighted the potential of FA-CSNPs to be used as an effective alternative to the conventional antifungal therapeutics. Copyright © 2016 Elsevier Ltd. All rights reserved.

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

PubMed

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

2017-08-29

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

Contribution of a new generation field-emission scanning electron microscope in the understanding of a 2099 Al-Li alloy.

PubMed

Brodusch, Nicolas; Trudeau, Michel; Michaud, Pierre; Rodrigue, Lisa; Boselli, Julien; Gauvin, Raynald

2012-12-01

Aluminum-lithium alloys are widespread in the aerospace industry. The new 2099 and 2199 alloys provide improved properties, but their microstructure and texture are not well known. This article describes how state-of-the-art field-emission scanning electron microscopy (FE-SEM) can contribute to the characterization of the 2099 aluminum-lithium alloy and metallic alloys in general. Investigations were carried out on bulk and thinned samples. Backscattered electron imaging at 3 kV and scanning transmission electron microscope imaging at 30 kV along with highly efficient microanalysis permitted correlation of experimental and expected structures. Although our results confirm previous studies, this work points out possible substitutions of Mg and Zn with Li, Al, and Cu in the T1 precipitates. Zinc and magnesium are also present in "rice grain"-shaped precipitates at the grain boundaries. The versatility of the FE-SEM is highlighted as it provides information in the macro- and microscales with relevant details. Its ability to probe the distribution of precipitates from nano- to microsizes throughout the matrix makes FE-SEM an essential technique for the characterization of metallic alloys.

Cobalt ferrite nano-composite coated on glass by Doctor Blade method for photo-catalytic degradation of an azo textile dye Reactive Red 4: XRD, FESEM and DRS investigations.

PubMed

Habibi, Mohammad Hossein; Parhizkar, Janan

2015-11-05

Cobalt ferrite nano-composite was prepared by hydrothermal route using cobalt nitrate, iron nitrate and ethylene glycol as chelating agent. The nano-composite was coated on glass by Doctor Blade method and annealed at 300 °C. The structural, optical, and photocatalytic properties have been studied by powder X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM) and UV-visible spectroscopy (UV-Vis DRS). Powder XRD analysis confirmed formation of CoFe2O4 spinel phase. The estimated particle size from FESEM data was 50 nm. The calculated energy band gaps, obtained by Tauc relation from UV-Vis absorption spectra was 1.3 eV. Photocatalytic degradation of Reactive Red 4 as an azo textile was investigated in aqueous solution under irradiation showed 68.0% degradation of the dye within 100 min. The experimental enhanced activity compare to pure Fe2O3 can be ascribed to the formation of composite, which was mainly attributable to the transfer of electron and hole to the surface of composite and hinder the electron hole recombination. Copyright © 2015 Elsevier B.V. All rights reserved.

Properties of Cement Mortar and Ultra-High Strength Concrete Incorporating Graphene Oxide Nanosheets.

PubMed

Lu, Liulei; Ouyang, Dong

2017-07-20

In this work, the effect of graphene oxide nanosheet (GONS) additives on the properties of cement mortar and ultra-high strength concrete (UHSC) is reported. The resulting GONS-cement composites were easy to prepare and exhibited excellent mechanical properties. However, their fluidity decreased with increasing GONS content. The UHSC specimens were prepared with various amounts of GONSs (0-0.03% by weight of cement). Results indicated that using 0.01% by weight of cement GONSs caused a 7.82% in compressive strength after 28 days of curing. Moreover, adding GONSs improved the flexural strength and deformation ability, with the increase in flexural strength more than that of compressive strength. Furthermore, field-emission scanning electron microscopy (FE-SEM) was used to observe the morphology of the hardened cement paste and UHSC samples. FE-SEM observations showed that the GONSs were well dispersed in the matrix and the bonding of the GONSs and the surrounding cement matrix was strong. Furthermore, FE-SEM observation indicated that the GONSs probably affected the shape of the cement hydration products. However, the growth space for hydrates also had an important effect on the morphology of hydrates. The true hydration mechanism of cement composites with GONSs needs further study.

Effect of annealing temperature on physical properties of solution processed nickel oxide thin films

NASA Astrophysics Data System (ADS)

Sahoo, Pooja; Thangavel, R.

2018-05-01

In this report, NiO thin films were prepared at different annealing temperatures from nickel acetate precursor by sol-gel spin coating method. These films were characterized by different analytical techniques to obtain their structural, optical morphological and electrical properties using X-ray diffractometer (XRD), Field emission scanning electron microscopy (FESEM), UV-Vis NIR double beam spectrophotometer and Keithley 2450 source meter respectively. FESEM images clearly indicates the formation of a homogenous and porous films. Due to their porosity, they can be used in sensing applications. The optical absorption spectra elucidated that the films are highly transparent and have a suitable band gap which are in similar agreement with earlier reports. The current enhancement under illumination shows the suitability of nanostructured NiO thin films in its application in photovoltaics.

Cobalt-doped carbon xerogel with different initial pH values toward oxygen reduction

NASA Astrophysics Data System (ADS)

Fitri, Azim; Loh, Kee Shyuan; Puspasari, Ifa; Mohamad, Abu Bakar

2017-12-01

In this study, cobalt-doped carbon xerogel (Co-CX) was synthesized via sol-gel polymerization resorcinol-formaldehyde, catalyzed with cobalt nitrate, followed by drying and carbonization process under nitrogen gas flow. The effect of initial pH value (5.5, 6.5 and 7.5) and the type of carbon precursors on the morphology of Co-CX have been investigated with Field Emission-Transmission Electron Microscopy (FESEM). The catalytic activity of Co-CX for the oxygen reduction reaction (ORR) in 0.1 M KOH has been studied by using a rotating ring-disk electrode (RRDE) technique. FESEM revealed that Co doping promotes the formation of more pores. While the conditions allow obtaining xerogel with higher porosity at pH 7.5. The RRDE result display that Co-CX exhibited good catalytic activity tends to favor two electrons pathway.

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

NASA Astrophysics Data System (ADS)

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

2018-05-01

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

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

NASA Astrophysics Data System (ADS)

Kafashan, Hosein

2018-04-01

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

Designing of silk and ZnO based antibacterial and noncytotoxic bionanocomposite films and study of their mechanical and UV absorption behavior.

PubMed

Kiro, Anamika; Bajpai, Jaya; Bajpai, A K

2017-01-01

Bionanocomposites of sericin and polyvinyl alcohol (PVA) were prepared by solution casting method and zinc oxide nanoparticles were impregnated within the polymer blend matrix through homogenous phase reaction between zinc chloride and sodium hydroxide at high temperature following an ex-situ co-precipitation method. The prepared bionanocomposites were characterized using Fourier Transform Infrared Spectroscopy, X-ray diffraction, Field Emission Scanning Electron Microscopy, Transmission Electron Microscopy and Atomic Force Microscopy techniques. The presence of characteristic groups of sericin and ZnO nanoparticles was ascertained by the FTIR spectra. XRD analysis confirmed the impregnation of ZnO nanoparticles and sericin within the PVA matrix. XRD and FESEM of the bionanocomposites provided information about their semicrystalline nature, crystallite size of the particles, and irregular rough surfaces. The TEM confirmed the size of ZnO particles to be in the nanometer range. AFM confirmed the platykurtic nature of the surface while the negative surface skewness shows the predominance of valleys over peaks suggesting for the planar nature of the surface of the bionanocomposites. UV absorption properties of bionanocomposite films were determined by UV absorption spectroscopy. UV absorption increased with increasing amount of ZnO nanoparticles in the nanocomposites. Sericin was found to absorb UV-C radiations between 200-290nm which is mainly due to aromatic amino acids like tryptophan, tyrosine and phenylalanine. The ZnO nanoparticles and sericin protein showed antimicrobial properties as evident from the inhibition zones obtained against Staphylococcus aureus and Escherichia coli. The bionanocomposite was found to be noncytotoxic which was proved by in vitro cytotoxicity test. Microhardness of bionanocomposite films increased with increase in the amount of ZnO nanoparticles in the sericin and PVA matrix. Copyright © 2016 Elsevier Ltd. All rights reserved.

Optical, structural and electrochromic behavior studies on nanocomposite thin film of aniline, o-toluidine and WO3

NASA Astrophysics Data System (ADS)

Najafi-Ashtiani, Hamed; Bahari, Ali

2016-08-01

In the field of materials for electrochromic (EC) applications much attention was paid to the derivatives of aniline. We report on the optical, structural and electrochromic properties of electrochromic thin film based on composite of WO3 nanoparticles and copolymer of aniline and o-toluidine prepared by electrochemical polymerization method on fluorine doped tin oxide (FTO) coated glass. The thin film was studied by X-ray diffraction (XRD) and Fourier transforms infrared (FTIR) spectroscopy. The morphology of prepared thin film was characterized by field emission scanning electron microscopy (FESEM), atomic force microscopy (AFM) and the thermal gravimetric analysis (TGA) as well. The optical spectra of nanocomposite thin film were characterized in the 200-900 nm wavelength range and EC properties of nanocomposite thin film were studied by cyclic voltammetry (CV). The calculation of optical band gaps of thin film exhibited that the thin film has directly allowed transition with the values of 2.63 eV on first region and 3.80 eV on second region. Dispersion parameters were calculated based on the single oscillator model. Finally, important parameters such as dispersion energy, oscillator energy and lattice dielectric constant were determined and compared with the data from other researchers. The nonlinear optical properties such as nonlinear optical susceptibility, nonlinear absorption coefficient and nonlinear refractive index were extracted. The obtained results of nanocomposite thin film can be useful for the optoelectronic applications.

An effective and novel pore sealing agent to enhance the corrosion resistance performance of Al coating in artificial ocean water

NASA Astrophysics Data System (ADS)

Lee, Han-Seung; Singh, Jitendra Kumar; Ismail, Mohamed A.

2017-02-01

A new technique was accepted to fill the porosity of Al coating applied by arc thermal spray process to enhance corrosion resistance performance in artificial ocean water. The porosity is the inherent property of arc thermal spray coating process. In this study, applied coating was treated with different concentrations of ammonium phosphate mono basic (NH4H2PO4: AP) solution thereafter dried at room temperature and kept in humidity chamber for 7d to deposit uniform film. The corrosion resistance of Al coating and treated samples have been evaluated using electrochemical impedance spectroscopy (EIS) and potentiodynamic techniques with exposure periods in artificial ocean water. Electrochemical techniques, X-ray diffraction (XRD), Raman spectroscopy, atomic force microscopy (AFM) and field emission-scanning electron microscopy (FE-SEM) indicated that phosphate ion would have been retarding corrosion of Al coating effectively. The formation of AHP (Ammonium Aluminum Hydrogen Phosphate Hydrate: NH4)3Al5H6(PO4)8.18H2O) on Al coating surface after treatment with AP is nano sized, crystalline and uniformly deposited but after exposure them in artificial ocean water, they form AHPH (Aluminum hydroxide phosphate hydrate Al3(PO4)2(OH)3(H2O)5) that is very protective, adherent, uniform and plate like morphology of corrosion products. The AHPH is sparingly soluble and adherent to surface and imparted improved corrosion resistance.

The photocatalytic properties of hollow (GaN)1-x(ZnO)x composite nanofibers synthesized by electrospinning

NASA Astrophysics Data System (ADS)

Wang, Ding; Zhang, Minglu; Zhuang, Huaijuan; Chen, Xu; Wang, Xianying; Zheng, Xuejun; Yang, Junhe

2017-02-01

(GaN)1-x(ZnO)x composite nanofibers with hollow structure were prepared by initial electrospinning, and the subsequent calcination and nitridation. The structure and morphology characteristics of samples were investigated by X-ray diffraction (XRD), field-emission scanning electron microscopy (FE-SEM), energy dispersive X-ray spectroscopy (EDS) and transmission electron microscopy (TEM). The characterization results showed the phase transition from ZnGa2O4 to (GaN)1-x(ZnO)x solid-solution under ammonia atmosphere. The preparation conditions were explored and the optimum nitridation temperature and holding time are 750 °C and 2 h, respectively. The photocatalytic properties of (GaN)1-x(ZnO)x with different Ga:Zn atomic ratios were investigated by degrading Rhodamine B under the visible light irradiation. The photocatalytic activity sequence is (GaN)1-x(ZnO)x (Ga:Zn = 1:2) > (GaN)1-x(ZnO)x (Ga:Zn = 1:3) > ZnO nanofibers > (GaN)1-x(ZnO)x (Ga:Zn = 1:4) > (GaN)1-x(ZnO)x (Ga:Zn = 1:1). The photocatalytic mechanism of the (GaN)1-x(ZnO)x hollow nanofibers was further studied by UV-vis diffuse reflectance spectra. The excellent photocatalytic performance of (GaN)1-x(ZnO)x hollow nanofibers was attributed to the narrow band gap and high surface area of porous nanofibers with hollow structure.

Identification of the mechanism that confers superhydrophobicity on 316L stainless steel

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

Escobar, Ana M.; Llorca-Isern, Nuria; Rius-Ayra, Oriol

This study develops a rapid method to confer superhydrophobicity on 316L stainless steel surfaces with an amphiphilic reagent such as dodecanoic acid. The highest contact angle (approaching 173°) was obtained after forming hierarchical structures with a non-aqueous electrolyte by an electrolytic process. Our goal was to induce superhydrophobicity directly on 316L stainless steel substrates and to establish which molecules cause the effect. The superhydrophobic behaviour is analysed by contact angle measurements, scanning electron microscopy (SEM), IR spectroscopy and atomic force microscopy (AFM). The growth mechanism is analysed using FE-SEM, TOF-SIMS and XPS in order to determine the molecules involved inmore » the reaction and the growth. The TOF-SIMS analysis revealed that the Ni{sup 2+} ions react with lauric acid to create an ester on the stainless steel surface. - Highlights: • This study develops a rapid and facile approach to impart superhydrophobicity properties to 316L stainless steel surfaces with an amphiphilic reagent such as dodecanoic acid. Surface character changes from superhydrophilicity to superhydrophobicity. • This process changes the surface character from superhydrophilicity to superhydrophobicity. • The process based on electrolysis of a nickel salt in lauric acid provides superhydrophobic behaviour in 316L stainless steel. • The growth mechanism is proposed as a mode island (Volmert- Weber mode). • TOF-SIMS and XPS provided the identification of the molecules involved in the surface modification reaction on AISI 316L inducing superhydrophobicity.« less

Inhibition of hydroxyapatite growth by casein, a potential salivary phosphoprotein homologue.

PubMed

Romero, Maria J R H; Nakashima, Syozi; Nikaido, Toru; Ichinose, Shizuko; Sadr, Alireza; Tagami, Junji

2015-08-01

Salivary phosphoproteins are essential in tooth mineral regulation but are often overlooked in vitro. This study aimed to evaluate the effect of casein, as a salivary phosphoprotein homologue, on the deposition and growth of hydroxyapatite (HA) on tooth surfaces. Hydroxyapatite growth was quantified using seeded crystal systems. Artificial saliva (AS) containing HA powder and 0, 10, 20, 50, or 100 μg ml(-1) of casein, or 100 μg ml(-1) of dephosphorylated casein (Dcasein), was incubated for 0-8 h at 37°C, pH 7.2. Calcium concentrations were measured using atomic absorption spectroscopy (AAS). Surface precipitation of HA on bovine enamel and dentine blocks, incubated in similar conditions for 7 d, was examined using field emission scanning electron microscopy (FE-SEM) and transmission electron microscopy (TEM) with selected area electron diffraction (SAED). Casein adsorption was assessed using modified Lowry assays and zeta-potential measurements. The AAS results revealed a concentration-dependent inhibition of calcium consumption. Hydroxyapatite precipitation occurred when no casein was present, whereas precipitation of HA was apparently completely inhibited in casein-containing groups. Adsorption data demonstrated increasingly negative zeta-potential with increased casein concentration and an affinity constant similar to proline-rich proteins with Langmuir modelling. Casein inhibited the deposition and growth of HA primarily through the binding of esterized phosphate to HA active sites, indicating its potential as a mineral-regulating salivary phosphoprotein homologue in vitro. © 2015 Eur J Oral Sci.

Effect of structural evolution on mechanical properties of ZrO2 coated Ti-6Al-7Nb-biomedical application

NASA Astrophysics Data System (ADS)

Zalnezhad, E.

2016-05-01

Zirconia (ZrO2) nanotube arrays were fabricated by anodizing pure zirconium (Zr) coated Ti-6Al-7Nb in fluoride/glycerol electrolyte at a constant potential of 60 V for different times. Zr was deposited atop Ti-6Al-7Nb via a physical vapor deposition magnetron sputtering (PVDMS) technique. Structural investigations of coating were performed utilizing X-ray diffraction (XRD) analysis. Field emission scanning electron microscopy (FESEM) and atomic force microscopy (AFM) were used to characterize the morphology and microstructure of coatings. Unannealed ZrO2 nanotube arrays were amorphous. Monoclinic and tetragonal ZrO2 appeared when the coated substrates were heat treated at 450 °C and 650 °C, while monoclinic ZrO2 was found at 850 °C and 900 °C. Mechanical properties, including nanohardness and modulus of elasticity, were evaluated at different annealing temperatures using a nanoindentation test. The nanoindentation results show that the nanohardness and modulus of elasticity for Ti-6AL-7Nb increased by annealing ZrO2 coated substrate at 450 °C. The nanohardness and modulus of elasticity for coated substrate decreased with annealing temperatures of 650, 850, and 900 °C. At an annealing temperature of 900 °C, cracks in the ZrO2 thin film coating occurred. The highest nanohardness and elastic modulus values of 6.34 and 218 GPa were achieved at an annealing temperature of 450 °C.

An effective and novel pore sealing agent to enhance the corrosion resistance performance of Al coating in artificial ocean water

PubMed Central

Lee, Han-Seung; Singh, Jitendra Kumar; Ismail, Mohamed A.

2017-01-01

A new technique was accepted to fill the porosity of Al coating applied by arc thermal spray process to enhance corrosion resistance performance in artificial ocean water. The porosity is the inherent property of arc thermal spray coating process. In this study, applied coating was treated with different concentrations of ammonium phosphate mono basic (NH4H2PO4: AP) solution thereafter dried at room temperature and kept in humidity chamber for 7d to deposit uniform film. The corrosion resistance of Al coating and treated samples have been evaluated using electrochemical impedance spectroscopy (EIS) and potentiodynamic techniques with exposure periods in artificial ocean water. Electrochemical techniques, X-ray diffraction (XRD), Raman spectroscopy, atomic force microscopy (AFM) and field emission-scanning electron microscopy (FE-SEM) indicated that phosphate ion would have been retarding corrosion of Al coating effectively. The formation of AHP (Ammonium Aluminum Hydrogen Phosphate Hydrate: NH4)3Al5H6(PO4)8.18H2O) on Al coating surface after treatment with AP is nano sized, crystalline and uniformly deposited but after exposure them in artificial ocean water, they form AHPH (Aluminum hydroxide phosphate hydrate Al3(PO4)2(OH)3(H2O)5) that is very protective, adherent, uniform and plate like morphology of corrosion products. The AHPH is sparingly soluble and adherent to surface and imparted improved corrosion resistance. PMID:28157233

Morphology and topography study of graphene synthesized from plant oil

NASA Astrophysics Data System (ADS)

Robaiah, M.; Rusop, M.; Abdullah, S.; Khusaimi, Z.; Azhan, H.; Laila, M. O.; Salifairus, M. J.; Asli, N. A.

2018-05-01

The graphene is material consists of bonded atom carbon atoms in sheet form one atom thick. The different types of carbon sources which are refined corn oil, palm oil and waste cooking palm oil were used as carbon feedstock to supply carbon atom for synthesizing graphene on the nickel substrate by thermal chemical vapour deposition. The substrate and carbon sources were placed in double zone furnaces. The carbon sources and the substrate were heated at 300 °C and 900 °C respectively. The both furnaces were switched off after synthesis time for cooling process finish. The formation of the graphene on the Ni surface appears due to segregation and precipitation of a high amount of carbon from the source material during the cooling process. FESEM, AFM, UV-VIS Spectroscopy and Raman Spectroscopy were used to characterize and synthesized graphene.

Poly-l-cysteine/electrospun copper oxide nanofibers-zinc oxide nanoparticles nanocomposite as sensing element of an electrochemical sensor for simultaneous determination of adenine and guanine in biological samples and evaluation of damage to dsDNA and DNA purine bases by UV radiation.

PubMed

Arvand, Majid; Sayyar Ardaki, Masoomeh

2017-09-15

A new nanocomposite film constructed of poly-l-cysteine/zinc oxide nanoparticles-electrospun copper oxide nanofibers (PLC/ZnO-NPs-CuO-NFs) was prepared on the surface of the graphite electrode (GE). The novel electrode was successfully applied for the simultaneous determination of guanine (G) and adenine (A), two of the most important components of DNA and RNA. The PLC/ZnO-NPs-CuO-NFs/GE enhanced the anodic peak currents of the purine bases conspicuously and could determine them sensitively and separately in 0.1 M phosphate buffer solution at the physiological pH (7.0). The synthesized nanofibers, nanoparticles and nanocomposite were characterized by different methods such as Fourier transform infrared spectroscopy (FT-IR), transmission electron microscopy (TEM), scanning electron microscopy (SEM), field emission scanning electron microscopy (FE-SEM), atomic force microscopy (AFM), X-ray diffraction (XRD) and energy dispersive X-ray analysis (EDS). Under the optimum operating conditions, linear calibration curves were obtained in the range of 0.05-6.78 and 0.01-3.87 μM with a detection limit of 12.48 and 1.25 nM for G and A, respectively. The proposed method was applied to quantify A and G in three different DNA samples with satisfactory results. In addition, damage to human blood double-stranded DNA (dsDNA) and DNA purine bases (liberated in previously hydrolyzed human blood dsDNA) caused by UV-C and UV-B were evaluated. The results demonstrated that the proposed biosensing platform not only provides a novel and sensitive approach to detecting DNA damage, but also can be used for simultaneous determination of purine bases and major products of DNA oxidative damage. Copyright © 2017 Elsevier B.V. All rights reserved.

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

PubMed

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

2012-03-01

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

Physical properties of agave cellulose graft polymethyl methacrylate

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

Rosli, Noor Afizah; Ahmad, Ishak; Abdullah, Ibrahim

2013-11-27

The grafting polymerization of methyl methacrylate and Agave cellulose was prepared and their structural analysis and morphology were investigated. The grafting reaction was carried out in an aqueous medium using ceric ammonium nitrate as an initiator. The structural analysis of the graft copolymers was carried out by Fourier transform infrared and X-ray diffraction. The graft copolymers were also characterized by field emission scanning electron microscopy (FESEM). An additional peak at 1732 cm{sup −1} which was attributed to the C=O of ester stretching vibration of poly(methyl methacrylate), appeared in the spectrum of grafted Agave cellulose. A slight decrease of crystallinity indexmore » upon grafting was found from 0.74 to 0.68 for cellulose and grafted Agave cellulose, respectively. Another evidence of grafting showed in the FESEM observation, where the surface of the grafted cellulose was found to be roughed than the raw one.« less

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

NASA Astrophysics Data System (ADS)

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

2016-07-01

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

Fe-tannic acid complex dye as photo sensitizer for different morphological ZnO based DSSCs

NASA Astrophysics Data System (ADS)

Çakar, Soner; Özacar, Mahmut

2016-06-01

In this paper we have synthesized different morphological ZnO nanostructures via microwave hydrothermal methods at low temperature within a short time. We described different morphologies of ZnO at different Zn(NO3)2/KOH mole ratio. The ZnO nanostructures were characterized via X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM) and UV-vis spectrophotometry. All ZnO structures have hexagonal wurtzite type structures. The FESEM images showed various morphologies of ZnO such as plate, rod and nanoparticles. Dye sensitized solar cells have been assembled by these different morphological structures photo electrode and tannic acid or Fe-tannic acid complex dye as sensitizer. We have achieved at maximum efficiencies of photovoltaic cells prepared with ZnO plate in all dye systems. The conversion efficiencies of dye sensitized solar cells are 0.37% and 1.00% with tannic acid and Fe-tannic acid complex dye, respectively.

Studies of antibacterial efficacy of different biopolymer protected silver nanoparticles synthesized under reflux condition

NASA Astrophysics Data System (ADS)

Su, Chia Hung; Velusamy, Palaniyandi; Kumar, Govindarajan Venkat; Adhikary, Shritama; Pandian, Kannaiyan; Anbu, Periyasamy

2017-01-01

In the present study, a simple method to impregnate silver nanoparticles (AgNPs) into carboxymethyl cellulose (CMC) and sodium alginate (SA) is reported for the first time. Single step synthesis of carboxymethyl cellulose (CMC) and sodium alginate (SA) biopolymer protected silver nanoparticles (AgNPs) using aniline as a reducing agent under reflux conditions was investigated. The synthesized nanoparticles were characterized by UV-Vis spectrophotometry, X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR) and field emission scanning electron microscopy (FESEM). The FESEM results of CMC@AgNPs and SA@AgNPs showed the formation of spherical nanoparticles sized 30-60 nm. Testing of the antibiofilm efficacy of the polymer protected AgNPs against different bacterial strains such as Klebsiella pneumoniae MTCC 4032 and Streptococcus pyogenes MTCC 1924 revealed that the biopolymer protected AgNPs had excellent antibiofilm activity.

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

PubMed

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

2014-06-01

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

Passive optical limiting studies of nanostructured Cu doped ZnO-PVA composite thin films

NASA Astrophysics Data System (ADS)

Tamgadge, Y. S.; Sunatkari, A. L.; Talwatkar, S. S.; Pahurkar, V. G.; Muley, G. G.

2016-01-01

We prepared undoped and Cu doped ZnO semiconducting nanoparticles (NPs) by chemical co-precipitation method and obtained Cu doped ZnO-polyvinyl alcohol (PVA) nanocomposite thin films by spin coating to investigate third order nonlinear optical and optical limiting properties under cw laser excitation. Powder samples of NPs were characterized by X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM), energy dispersive spectroscopy, transmission electron microscopy, ultraviolet-visible (UV-vis) and Fourier transform infrared spectroscopy. XRD pattern and FE-SEM micrograph revealed the presence of hexagonal wurtzite phase ZnO NPs having uniform morphology with average particle size of 20 nm. The presence of excitons and absorption peaks in the range 343-360 nm, revealed by UV-vis study, were attributed to excitons in n = 1 quantum state. Third order NLO properties of all composite thin films were investigated by He-Ne continuous wave (cw) laser of wavelength 632.8 nm using Z-scan technique. Thermally stimulated enhanced values of nonlinear refraction and absorption coefficients were obtained which may be attributed to self-defocusing effect, reverse saturable absorption, weak free carrier absorption and surface states properties originated from thermo optic effect. Optical limiting properties have been studied using cw diode laser of wavelength 808 nm and results are presented.

Dielectrophoretic immobilization of proteins: Quantification by atomic force microscopy.

PubMed

Laux, Eva-Maria; Knigge, Xenia; Bier, Frank F; Wenger, Christian; Hölzel, Ralph

2015-09-01

The combination of alternating electric fields with nanometer-sized electrodes allows the permanent immobilization of proteins by dielectrophoretic force. Here, atomic force microscopy is introduced as a quantification method, and results are compared with fluorescence microscopy. Experimental parameters, for example the applied voltage and duration of field application, are varied systematically, and the influence on the amount of immobilized proteins is investigated. A linear correlation to the duration of field application was found by atomic force microscopy, and both microscopical methods yield a square dependence of the amount of immobilized proteins on the applied voltage. While fluorescence microscopy allows real-time imaging, atomic force microscopy reveals immobilized proteins obscured in fluorescence images due to low S/N. Furthermore, the higher spatial resolution of the atomic force microscope enables the visualization of the protein distribution on single nanoelectrodes. The electric field distribution is calculated and compared to experimental results with very good agreement to atomic force microscopy measurements. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Novel Weed-Extracted Silver Nanoparticles and Their Antibacterial Appraisal against a Rare Bacterium from River and Sewage Treatment Plan.

PubMed

Syafiuddin, Achmad; Hadibarata, Tony; Beng Hong Kueh, Ahmad; Razman Salim, Mohd

2017-12-26

This is the first investigation to demonstrate the use of biochemical contents present within Cyperus rotundus , Eleusin indica , Euphorbia hirta , Melastoma malabathricum , Clidemia hirta and Pachyrhizus erosus extracts for the reduction of silver ion to silver nanoparticles (AgNPs) form. In addition, the antibacterial capability of the synthesized AgNPs and plant extracts alone against a rare bacterium, Chromobacterium haemolyticum ( C. haemolyticum ), was examined. Moreover, ultraviolet-visible spectroscopy (UV-vis), Fourier transform infrared spectroscopy (FTIR), field emission scanning electron microscopy (FESEM), energy-dispersive X-ray spectroscopy (EDX) and inductively coupled plasma atomic emission spectroscopy (ICPOES) of the synthesized AgNPs were characterized. The smallest AgNPs can be produced when Cyperus rotundus extracts were utilized. In addition, this study has found that the synthesis efficiencies using all plant extracts are in the range of 72% to 91% with the highest percentage achieved when Eleusin indica extract was employed. All synthesized AgNPs have antibacterial capability against all examined bacteria depending on their size and bacteria types. Interestingly, Melastoma malabathricum and Clidemia hirta extracts have demonstrated an antibacterial ability against C. haemolyticum .

Novel Weed-Extracted Silver Nanoparticles and Their Antibacterial Appraisal against a Rare Bacterium from River and Sewage Treatment Plan

PubMed Central

Hadibarata, Tony; Beng Hong Kueh, Ahmad; Razman Salim, Mohd

2017-01-01

This is the first investigation to demonstrate the use of biochemical contents present within Cyperus rotundus, Eleusin indica, Euphorbia hirta, Melastoma malabathricum, Clidemia hirta and Pachyrhizus erosus extracts for the reduction of silver ion to silver nanoparticles (AgNPs) form. In addition, the antibacterial capability of the synthesized AgNPs and plant extracts alone against a rare bacterium, Chromobacterium haemolyticum (C. haemolyticum), was examined. Moreover, ultraviolet-visible spectroscopy (UV-vis), Fourier transform infrared spectroscopy (FTIR), field emission scanning electron microscopy (FESEM), energy-dispersive X-ray spectroscopy (EDX) and inductively coupled plasma atomic emission spectroscopy (ICPOES) of the synthesized AgNPs were characterized. The smallest AgNPs can be produced when Cyperus rotundus extracts were utilized. In addition, this study has found that the synthesis efficiencies using all plant extracts are in the range of 72% to 91% with the highest percentage achieved when Eleusin indica extract was employed. All synthesized AgNPs have antibacterial capability against all examined bacteria depending on their size and bacteria types. Interestingly, Melastoma malabathricum and Clidemia hirta extracts have demonstrated an antibacterial ability against C. haemolyticum. PMID:29278389

Effect of annealing temperature on optical properties of binary zinc tin oxide nano-composite prepared by sol-gel route using simple precursors: structural and optical studies by DRS, FT-IR, XRD, FESEM investigations.

PubMed

Habibi, Mohammad Hossein; Mardani, Maryam

2015-02-25

Binary zinc tin oxide nano-composite was synthesized by a facile sol-gel method using simple precursors from the solutions consisting of zinc acetate, tin(IV) chloride and ethanol. Effect of annealing temperature on optical and structural properties was investigated using X-ray diffraction (XRD), diffuse reflectance spectra (DRS), field emission scanning electron microscopy (FESEM) and Fourier transform infrared spectroscopy (FTIR). XRD results revealed the existence of the ZnO and SnO2 phases. FESEM results showed that binary zinc tin oxide nano-composites ranges from 56 to 60 nm in diameter at 400°C and 500°C annealing temperatures respectively. The optical band gap was increased from 2.72 eV to 3.11 eV with the increasing of the annealing temperature. FTIR results confirmed the presence of zinc oxide and tin oxide and the broad absorption peaks at 3426 and 1602 cm(-1) can be ascribed to the vibration of absorptive water, and the absorption peaks at 546, 1038 and 1410 cm(-1) are due to the vibration of Zn-O or Sn-O groups in binary zinc tin oxide. Copyright © 2014 Elsevier B.V. All rights reserved.

Biosynthesis of highly porous bacterial cellulose nanofibers

NASA Astrophysics Data System (ADS)

Hosseini, Hadi; Kokabi, Mehrdad; Mousavi, Seyyed Mohammad

2018-01-01

Bacterial cellulose nanofibers (BCNFs) as a sustainable and biodegradable polymer has drawn tremendous research attention in tissue engineering, bacterial sensors and drug delivery due to its extraordinary properties such as high purity, high crystallinity, high water absorption capacity and excellent mechanical strength in the wet state. This awesome properties, is attributed to BCNFs structure, therefore its characterization is important. In this work, the bacterial strain, Gluconacetobacter xylinus (PTCC 1734, obtained from Iranian Research Organization for Science and Technology (IROST)), was used to produce BCNFs hydrogel using bacterial fermentation under static condition at 29 °C for 10 days in the incubator. Then, the biosynthesized BCNFs wet gel, were dried at ambient temperature and pressure and characterized using Brunauer-Emmett-Teller (BET) and Field emission scanning electron microscopy (FE-SEM) analysis. FESEM image displayed highly interconnected and porous structure composed of web-like continuous, nanofibers with an average diameter of 48.5±2.1 nm. BET result analysis depicted BCNFs dried at ambient conditions had IV isotherm type, according to the IUPAC classification, indicating that BCNFs dried at ambient condition is essentially mesoporous. On the other hand, BET results depicted, mesoporous structure is around 85%. In addition, Specific surface area (SBET) obtained 81.45 m2/g. These results are in accordance with the FESEM observation.

Properties of Cement Mortar and Ultra-High Strength Concrete Incorporating Graphene Oxide Nanosheets

PubMed Central

Ouyang, Dong

2017-01-01

In this work, the effect of graphene oxide nanosheet (GONS) additives on the properties of cement mortar and ultra-high strength concrete (UHSC) is reported. The resulting GONS-cement composites were easy to prepare and exhibited excellent mechanical properties. However, their fluidity decreased with increasing GONS content. The UHSC specimens were prepared with various amounts of GONSs (0–0.03% by weight of cement). Results indicated that using 0.01% by weight of cement GONSs caused a 7.82% in compressive strength after 28 days of curing. Moreover, adding GONSs improved the flexural strength and deformation ability, with the increase in flexural strength more than that of compressive strength. Furthermore, field-emission scanning electron microscopy (FE-SEM) was used to observe the morphology of the hardened cement paste and UHSC samples. FE-SEM observations showed that the GONSs were well dispersed in the matrix and the bonding of the GONSs and the surrounding cement matrix was strong. Furthermore, FE-SEM observation indicated that the GONSs probably affected the shape of the cement hydration products. However, the growth space for hydrates also had an important effect on the morphology of hydrates. The true hydration mechanism of cement composites with GONSs needs further study. PMID:28726750

Preparation of PVDF/SiO2 composite membrane for salty oil emulsion separation: Physicochemical properties changes and its impact on fouling propensity

NASA Astrophysics Data System (ADS)

Ngang, H. P.; Ahmad, A. L.; Low, S. C.; Ooi, B. S.

2017-06-01

In this study, polyvinylidene fluoride (PVDF)/silica (SiO2) composite membranes were prepared by diffusion induced phase separation through direct blending method. The roles of SiO2 particles concentration on membrane physicochemical properties were evaluated through oil emulsion separation under high ionic strength environment whereby hydrophobic interaction is prevalent. Membranes were characterized using field emission scanning electron microscope (FESEM), atomic force microscopy (AFM), contact angle measurement, membrane porosity and pore size distribution. It was expected that by adding the monodispersed SiO2, it will render the membrane with hydrophilic characteristic. However, it is concomitantly changing the physical properties of the membrane. Addition of SiO2 caused the changes to the physicochemical properties of the composite membrane and its effects on the fouling propensity were evaluated. It was found that the mean pore size of the membranes increased with the increase of SiO2 concentration. The addition of hydrophilic SiO2 had accelerated the precipitation of the membrane dope solution resulting in changes of membrane cross section morphology. FESEM images showed the membrane cross-section morphology of PVDF/SiO2 composite membrane had gradually changed from finger-like to macrovoid-like structure with the increased of SiO2 concentration. The hydrophilicity of the PVDF/SiO2 composite membrane was enhanced which is a desired property for water purification. However, the changes in physical properties (pore size, porosity, and surface roughness) had played more dominant role in the oil emulsion fouling behaviour rather than hydrophilicity enhancement. Due to the salting out effect under high ionic strength environment, hydrophobic interaction played an important role in the oil adsorption. The increment in membrane pore size, porosity, and surface roughness after incorporation of SiO2 particles had encountered more serious relative flux reduction and lower flux recovery ratio.

Laser-Induced Breakdown Spectroscopy (LIBS) for Monitoring the Formation of Hydroxyapatite Porous Layers

PubMed Central

Sola, Daniel; Paulés, Daniel; Grima, Lorena

2017-01-01

Laser-induced breakdown spectroscopy (LIBS) is applied to characterize the formation of porous hydroxyapatite layers on the surface of 0.8CaSiO3-0.2Ca3(PO4)2 biocompatible eutectic glass immersed in simulated body fluid (SBF). Compositional and structural characterization analyses were also conducted by field emission scanning electron microscopy (FESEM), energy dispersive X-ray spectroscopy (EDX), and micro-Raman spectroscopy. PMID:29211006

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

NASA Astrophysics Data System (ADS)

Kazemizadeh, Fatemeh; Malekfar, Rasoul

2018-02-01

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

Influence of substrate mineralogy on bacterial mineralization of calcium carbonate: implications for stone conservation.

PubMed

Rodriguez-Navarro, Carlos; Jroundi, Fadwa; Schiro, Mara; Ruiz-Agudo, Encarnación; González-Muñoz, María Teresa

2012-06-01

The influence of mineral substrate composition and structure on bacterial calcium carbonate productivity and polymorph selection was studied. Bacterial calcium carbonate precipitation occurred on calcitic (Iceland spar single crystals, marble, and porous limestone) and silicate (glass coverslips, porous sintered glass, and quartz sandstone) substrates following culturing in liquid medium (M-3P) inoculated with different types of bacteria (Myxococcus xanthus, Brevundimonas diminuta, and a carbonatogenic bacterial community isolated from porous calcarenite stone in a historical building) and direct application of sterile M-3P medium to limestone and sandstone with their own bacterial communities. Field emission scanning electron microscopy (FESEM), atomic force microscopy (AFM), powder X-ray diffraction (XRD), and 2-dimensional XRD (2D-XRD) analyses revealed that abundant highly oriented calcite crystals formed homoepitaxially on the calcitic substrates, irrespective of the bacterial type. Conversely, scattered spheroidal vaterite entombing bacterial cells formed on the silicate substrates. These results show that carbonate phase selection is not strain specific and that under equal culture conditions, the substrate type is the overruling factor for calcium carbonate polymorph selection. Furthermore, carbonate productivity is strongly dependent on the mineralogy of the substrate. Calcitic substrates offer a higher affinity for bacterial attachment than silicate substrates, thereby fostering bacterial growth and metabolic activity, resulting in higher production of calcium carbonate cement. Bacterial calcite grows coherently over the calcitic substrate and is therefore more chemically and mechanically stable than metastable vaterite, which formed incoherently on the silicate substrates. The implications of these results for technological applications of bacterial carbonatogenesis, including building stone conservation, are discussed.

Comparison between solid-state and powder-state alkali pretreatment on saccharification and fermentation for bioethanol production from rice straw.

PubMed

Yeasmin, Shabina; Kim, Chul-Hwan; Islam, Shah Md Asraful; Lee, Ji-Young

2016-01-01

The efficacy of different concentrations of NaOH (0.25%, 0.50%, 0.75%, and 1.00%) for the pretreatment of rice straw in solid and powder state in enzymatic saccharification and fermentation for the production of bioethanol was evaluated. A greater amount of biomass was recovered through solid-state pretreatment (3.74 g) from 5 g of rice straw. The highest increase in the volume of rice straw powder as a result of swelling was observed with 1.00% NaOH pretreatment (48.07%), which was statistically identical to 0.75% NaOH pretreatment (32.31%). The surface of rice straw was disrupted by the 0.75% NaOH and 1.00% NaOH pretreated samples as observed using field-emission scanning electron microscopy (FE-SEM) and atomic force microscopy (AFM). In Fourier-transform infrared (FT-IR) spectra, absorbance of hydroxyl groups at 1,050 cm(-1) due to the OH group of lignin was gradually decreased with the increase of NaOH concentration. The greatest amounts of glucose and ethanol were obtained in 1.00% NaOH solid-state pretreated and powder-state hydrolyzed samples (0.804 g g(-1) and 0.379 g g(-1), respectively), which was statistically similar to the use of 0.75% NaOH (0.763 g g(-1) and 0.358 g g(-1), respectively). Thus, solid-state pretreatment with 0.75% NaOH and powder-state hydrolysis appear to be suitable for fermentation and bioethanol production from rice straw.

Influence of Substrate Mineralogy on Bacterial Mineralization of Calcium Carbonate: Implications for Stone Conservation

PubMed Central

Jroundi, Fadwa; Schiro, Mara; Ruiz-Agudo, Encarnación; González-Muñoz, María Teresa

2012-01-01

The influence of mineral substrate composition and structure on bacterial calcium carbonate productivity and polymorph selection was studied. Bacterial calcium carbonate precipitation occurred on calcitic (Iceland spar single crystals, marble, and porous limestone) and silicate (glass coverslips, porous sintered glass, and quartz sandstone) substrates following culturing in liquid medium (M-3P) inoculated with different types of bacteria (Myxococcus xanthus, Brevundimonas diminuta, and a carbonatogenic bacterial community isolated from porous calcarenite stone in a historical building) and direct application of sterile M-3P medium to limestone and sandstone with their own bacterial communities. Field emission scanning electron microscopy (FESEM), atomic force microscopy (AFM), powder X-ray diffraction (XRD), and 2-dimensional XRD (2D-XRD) analyses revealed that abundant highly oriented calcite crystals formed homoepitaxially on the calcitic substrates, irrespective of the bacterial type. Conversely, scattered spheroidal vaterite entombing bacterial cells formed on the silicate substrates. These results show that carbonate phase selection is not strain specific and that under equal culture conditions, the substrate type is the overruling factor for calcium carbonate polymorph selection. Furthermore, carbonate productivity is strongly dependent on the mineralogy of the substrate. Calcitic substrates offer a higher affinity for bacterial attachment than silicate substrates, thereby fostering bacterial growth and metabolic activity, resulting in higher production of calcium carbonate cement. Bacterial calcite grows coherently over the calcitic substrate and is therefore more chemically and mechanically stable than metastable vaterite, which formed incoherently on the silicate substrates. The implications of these results for technological applications of bacterial carbonatogenesis, including building stone conservation, are discussed. PMID:22447589

Multi-walled carbon nanotubes/polymer composites in absence and presence of acrylic elastomer (ACM).

PubMed

Kumar, S; Rath, T; Mahaling, R N; Mukherjee, M; Khatua, B B; Das, C K

2009-05-01

Polyetherimide/Multiwall carbon nanotube (MWNTs) nanocomposites containing as-received and modified (COOH-MWNT) carbon nanotubes were prepared through melt process in extruder and then compression molded. Thermal properties of the composites were characterized by thermo-gravimetric analysis (TGA). Field emission scanning electron microscopy (FESEM) images showed that the MWNTs were well dispersed and formed an intimate contact with the polymer matrix without any agglomeration. However the incorporation of modified carbon nanotubes formed fascinating, highly crosslinked, and compact network structure throughout the polymer matrix. This showed the increased adhesion of PEI with modified MWNTs. Scanning electron microscopy (SEM) also showed high degree of dispersion of modified MWNTs along with broken ends. Dynamic mechanical analysis (DMA) results showed a marginal increase in storage modulus (E') and glass transition temperature (T(g)) with the addition of MWNTs. Increase in tensile strength and impact strength of composites confirmed the use the MWNTs as possible reinforcement agent. Both thermal and electrical conductivity of composites increased, but effect is more pronounced on modification due to formation of network of carbon nanotubes. Addition of acrylic elastomer to developed PEI/MWNTs (modified) nanocomposites resulted in the further increase in thermal and electrical properties due to the formation of additional bond between MWNTs and acrylic elastomers at the interface. All the results presented are well corroborated by SEM and FESEM studies.

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

PubMed Central

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

2016-01-01

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

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

PubMed

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

2016-01-11

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

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

PubMed

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

2012-04-01

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

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

NASA Astrophysics Data System (ADS)

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

2011-11-01

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

Chemical mapping and quantification at the atomic scale by scanning transmission electron microscopy.

PubMed

Chu, Ming-Wen; Chen, Cheng Hsuan

2013-06-25

With innovative modern material-growth methods, a broad spectrum of fascinating materials with reduced dimensions-ranging from single-atom catalysts, nanoplasmonic and nanophotonic materials to two-dimensional heterostructural interfaces-is continually emerging and extending the new frontiers of materials research. A persistent central challenge in this grand scientific context has been the detailed characterization of the individual objects in these materials with the highest spatial resolution, a problem prompting the need for experimental techniques that integrate both microscopic and spectroscopic capabilities. To date, several representative microscopy-spectroscopy combinations have become available, such as scanning tunneling microscopy, tip-enhanced scanning optical microscopy, atom probe tomography, scanning transmission X-ray microscopy, and scanning transmission electron microscopy (STEM). Among these tools, STEM boasts unique chemical and electronic sensitivity at unparalleled resolution. In this Perspective, we elucidate the advances in STEM and chemical mapping applications at the atomic scale by energy-dispersive X-ray spectroscopy and electron energy loss spectroscopy with a focus on the ultimate challenge of chemical quantification with atomic accuracy.

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

PubMed

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

2014-05-01

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

Tensile properties and water absorption assessment of linear low-Density Polyethylene/Poly (Vinyl Alcohol)/Kenaf composites: effect of eco-friendly coupling agent

NASA Astrophysics Data System (ADS)

Pang, A. L.; Ismail, H.; Abu Bakar, A.

2018-02-01

Linear low-density polyethylene (LLDPE)/poly (vinyl alcohol) (PVOH) filled with untreated kenaf (UT-KNF) and eco-friendly coupling agent (ECA)-treated kenaf (ECAT-KNF) were prepared using ThermoHaake internal mixer, respectively. Filler loadings of UT-KNF and ECAT-KNF used in this study are 10 and 40 parts per hundred parts of resin (phr). The effect of ECA on tensile properties and water absorption of LLDPE/PVOH/KNF composites were investigated. Field emission scanning electron microscopy (FESEM) analysis was applied to visualize filler-matrix adhesion. The results indicate LLDPE/PVOH/ECAT-KNF composites possess higher tensile strength and tensile modulus, but lower elongation at break compared to LLDPE/PVOH/UT-KNF composites. The morphological studies of tensile fractured surfaces using FESEM support the increment in tensile properties of LLDPE/PVOH/ECAT-KNF composites. Nevertheless, LLDPE/PVOH/UT-KNF composites reveal higher water absorption compared to LLDPE/PVOH/ECAT-KNF composites.

Strontium hexaferrite (SrFe12O19) based composites for hyperthermia applications

NASA Astrophysics Data System (ADS)

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

2013-10-01

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

Electrical properties of Mg doped ZnO nanostructure annealed at different temperature

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

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

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

Microstructure and mechanical properties of nickel coated multi walled carbon nanotube reinforced stainless steel 316L matrix composites by laser sintering process

NASA Astrophysics Data System (ADS)

Mahanthesha, P.; Mohankumar, G. C.

2018-04-01

Electroless Ni coated Multi-walled Carbon nanotubes reinforced with Stainless Steel 316L matrix composite was developed by Direct Metal Laser Sintering process (DMLS). Homogeneous mixture of Stainless Steel 316L powder and carbon nanotubes in different vol. % was obtained by using double cone blender machine. Characterization of electroless Ni coated carbon nanotubes was done by using X-ray diffraction, FESEM and EDS. Test samples were fabricated at different laser scan speeds. Effect of process parameters and CNT vol. % content on solidification microstructure and mechanical properties of test samples was investigated by using Optical microscopy, FESEM, and Hounsfield tensometer. Experimental results reveal DMLS process parameters affect the density and microstructure of sintered parts. Dense parts with minimum porosity when processed at low laser scan speeds and low CNT vol. %. Tensile fractured surface of test specimens evidences the survival of carbon nanotubes under high temperature processing condition.

Preparation and Mechanical Properties of Graphene Oxide: Cement Nanocomposites

PubMed Central

Babak, Fakhim; Abolfazl, Hassani; Alimorad, Rashidi; Parviz, Ghodousi

2014-01-01

We investigate the performance of graphene oxide (GO) in improving mechanical properties of cement composites. A polycarboxylate superplasticizer was used to improve the dispersion of GO flakes in the cement. The mechanical strength of graphene-cement nanocomposites containing 0.1–2 wt% GO and 0.5 wt% superplasticizer was measured and compared with that of cement prepared without GO. We found that the tensile strength of the cement mortar increased with GO content, reaching 1.5%, a 48% increase in tensile strength. Ultra high-resolution field emission scanning electron microscopy (FE-SEM) used to observe the fracture surface of samples containing 1.5 wt% GO indicated that the nano-GO flakes were well dispersed in the matrix, and no aggregates were observed. FE-SEM observation also revealed good bonding between the GO surfaces and the surrounding cement matrix. In addition, XRD diffraction data showed growth of the calcium silicate hydrates (C-S-H) gels in GO cement mortar compared with the normal cement mortar. PMID:24574878

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

NASA Astrophysics Data System (ADS)

Shariati, Mohsen

2015-07-01

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

Comparison study on biosynthesis of silver nanoparticles using fresh and hot air oven dried IMPERATA CYLINDRICA leaf

NASA Astrophysics Data System (ADS)

Najmi Bonnia, Noor; Fairuzi, Afiza Ahmad; Akhir, Rabiatuladawiyah Md.; Yahya, Sabrina M.; Rani, Mohd Azri Ab; Ratim, Suzana; Rahman, Norafifah A.; Akil, Hazizan Md

2018-01-01

The perennial rhizomatous grass; Imperata cylindrica (I. cylindrica) has been reported rich in various phytochemicals. In present study, silver nanoparticles were synthesized from aqueous leaf extract of I. cylindrica at two different leaf conditions; fresh leaves and hot-air oven dried leaves. Biosynthesized silver nanoparticles were characterized by UV-visible spectroscopy, field emission scanning electron microscopy (FESEM) and Fourier transform infrared spectroscopy (FTIR). Maximum absorption was recorded between 400 nm to 500 nm. FESEM analysis revealed that the silver nanoparticles predominantly form spherical shapes. The particles sizes were ranging from 22-37 nm. The elemental composition of the synthesized silver nanoparticles was confirmed by using energy dispersive X-ray spectroscopy (EDX) analysis. Fourier transform infrared spectroscopy (FTIR) confirmed the reducing and stabilizing actions came from biomolecules associated with I. cylindrica leaf extract. Thus in this investigation, an environmentally safe method to synthesized silver nanoparticles using local plant extract was successfully established.

Effects of post-annealing treatment on the structure and photoluminescence properties of CdS/PS nanocomposites prepared by sol-gel method

NASA Astrophysics Data System (ADS)

Zhang, Hong-yan

2016-03-01

CdS nanocrystals have been successfully grown on porous silicon (PS) by sol-gel method. The plan-view field emission scanning electron microscopy (FESEM) shows that the pore size of PS is smaller than 5 μm in diameter and the agglomerates of CdS are broadly distributed on the surface of PS substrate. With the increase of annealing time, the CdS nanoparticles grow in both length and diameter along the preferred orientation. The cross-sectional FESEM images of ZnO/PS show that CdS nanocrystals are uniformly penetrated into all PS layers and adhere to them very well. photoluminescence (PL) spectra demonstrate that the intensity of PL peak located at about 425 nm has almost no change after the annealing time increases. The range of emission wavelength of CdS/PS is from 425 nm to 455 nm and the PL intensity is decreasing with the annealing temperature increasing from 100 °C to 200 °C.

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

PubMed Central

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

2016-01-01

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

Facile synthesis of one dimensional ZnO nanostructures for DSSC applications

NASA Astrophysics Data System (ADS)

Marimuthu, T.; Anandhan, N.

2016-05-01

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

Observation of DNA Molecules Using Fluorescence Microscopy and Atomic Force Microscopy

ERIC Educational Resources Information Center

Ito, Takashi

2008-01-01

This article describes experiments for an undergraduate instrumental analysis laboratory that aim to observe individual double-stranded DNA (dsDNA) molecules using fluorescence microscopy and atomic force microscopy (AFM). dsDNA molecules are observed under several different conditions to discuss their chemical and physical properties. In…

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.

Preparation of silver nanoparticles loaded graphene oxide nanosheets for antibacterial activity

NASA Astrophysics Data System (ADS)

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

2016-11-01

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

Investigating the performance of nitrogen-doped graphene photoanode in dye-sensitized solar cells

NASA Astrophysics Data System (ADS)

Joseph, Easter; Singh, Balbir Singh Mahinder; Mohamed, Norani Muti; Kait, Chong Fai; Saheed, Mohamed Shuaib Mohamed; Khatani, Mehboob

2016-11-01

In this paper, the atmospheric pressure chemical vapor deposition (AP-CVD) is used to synthesize graphene on a copper substrate by utilizing methane as a precursor and N-doped graphene (NDG) in the presence of ammonia. The performance of pure titanium dioxide (TiO2), TiO2/graphene, and TiO2/NDG as photoanodes in dye-sensitized solar cell (DSSC) were compared. Field emission scanning electron microscopy (FESEM) and transmission electron microscopy (TEM) showed flakes of few layers with an interrupted layer in both graphene and NDG. DSSC consist of TiO2/NDG photoanode exhibits a better enhancement due to the high conductivity of donor N in graphene which enhances the electron transportation across nanoporous TiO2.

Microscopic evolution of dielectric nanoparticles at different calcination temperatures synthesized via sol-gel auto-combustion

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

Adil, Muhammad, E-mail: muhammadadil86@hotmail.com; Zaid, Hasnah Mohd, E-mail: hasnamz@petronas.com.my; Chuan, Lee Kean, E-mail: lee.kc@petronas.com.my

2015-07-22

Dielectric nano powder synthesis is carried by a simple and fast sol-gel auto-combustion method. The transformation of crystalline phases of as-synthesized nano powders is investigated through the detailed transmission electron microscopy (TEM), revealed the crystallographic alterations and morphological information even at lattice scale. From specific area electron diffraction (SAED) pattern, has specified the d-spacing and corresponding planes supported by the observed lattice fringes. The morphological characterization of nanoparticles is performed through field-emission scanning electron microscopy (FESEM), exhibiting the increment in particle size due to agglomeration with the increase in annealing temperature. Furthermore, EDX pattern has been used to verify themore » formation of nanoparticles by revealing the presence of required elements.« less

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

NASA Astrophysics Data System (ADS)

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

2017-11-01

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

Polyethylene glycol assisted growth of Sn-doped ZnO nanorod arrays prepared via sol-gel immersion method

NASA Astrophysics Data System (ADS)

Ismail, A. S.; Mamat, M. H.; Malek, M. F.; Saidi, S. A.; Yusoff, M. M.; Mohamed, R.; Sin, N. D. Md; Suriani, A. B.; Rusop, M.

2018-05-01

Tin-doped zinc oxide (SZO) nanorod films at different concentrations of polyethylene glycol (PEG) were successfully deposited on zinc oxide (ZnO) seeded layer catalyst using sol-gel immersion method. The morphology of the samples were characterized using field emission scanning electron microscopy (FESEM), optical properties using UV-Vis spectrophotometer and electrical properties using I-V measurement system. The current-voltage (I-V) characteristics displayed that 5 wt % sample produced the highest conductivity.

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

DTIC Science & Technology

2010-12-01

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

Photo-catalyzed and phyto-mediated rapid green synthesis of silver nanoparticles using herbal extract of Salvinia molesta and its antimicrobial efficacy.

PubMed

Verma, Devendra Kumar; Hasan, Syed Hadi; Banik, Rathindra Mohan

2016-02-01

Current study presents an economic, ecofriendly and simple photo-catalytic green route for the swift biosynthesis of silver nanoparticles (AgNPs) within 20s, devoid of any instrumental support or chemical reductant. Aqueous leaf-extract of an aquatic fern, Salvinia molesta (AES), was used as a bioreductant as well as a stabilizing agent. Rapid change in color of reaction mixture from yellowish green to reddish brown within 20s in direct sun light exposure was considered as the primary visual indication of AgNPs biosynthesis. The biosynthesis of AgNPs was confirmed by UV-visible spectroscopy through the presence of a characteristic surface plasmon resonance (SPR) band for AgNPs at λmax of 425 nm. The process parameters were optimized through one factor at a time approach. Optimal values of different process parameters for the current biosynthetic system were found as; 35 min of reaction time under sun light, 8.0mM AgNO3 concentration and 5.0% (v/v) AES inoculum dose. Field emission scanning electron microscopy (FESEM), energy dispersive X-Ray spectroscopy (EDX), high resolution transmission electron microscopy (HRTEM), atomic force microscopy (AFM) and X-ray diffraction (XRD) analysis showed that most of AgNPs were spherical in shape with average size distribution of 12.46 nm having face centered cubic (fcc) crystal lattice. IR analysis of AES and synthesized AgNPs indicated the involvement of both hydroxyl and amino groups in the biosynthesis and stabilization of AgNPs. The synthesized AgNPs were found to be an effective antibacterial agent against both Gram positive and Gram negative bacteria. On the basis of results and facts, a probable mechanism has also been proposed to explore the possible route of biosynthesis of AgNPs through AES. Copyright © 2015 Elsevier B.V. All rights reserved.

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

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

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

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

Urea-assisted low temperature green synthesis of graphene nanosheets for transparent conducting film

NASA Astrophysics Data System (ADS)

Chamoli, Pankaj; Das, Malay K.; Kar, Kamal K.

2018-02-01

Present work demonstrates the fabrication of graphene nanosheet (GN) based transparent conducting film (TCF) using spray coating. Green synthesis of GN is carried out by reduction of graphene oxide (GO) using urea as green reducing agent. The reductive ability of urea with varied concentration is studied for GO at low temperature (i.e., 90 °C). As synthesized graphene nanosheets (GNs) are characterized by Raman spectroscopy, Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), UV-visible spectroscopy, field emission scanning electron microscopy (FESEM), atomic force microscope (AFM), and X-ray Photon spectroscopy (XPS). Raman analysis confirms that the maximum reduction of oxygen species is noticed using 30 mg/ml urea concentration at 90 °C from GO, and found Raman D to G band ratio (ID/IG) of ∼1.30. XPS analysis validates the Raman signature of removal of oxygen functional groups from GO, and obtained C/O ratio of ∼5.28. Further, transparent conducting films (TCFs) are fabricated using synthesized GNs. Thermal graphitization is carried out to enhance the optical and electrical properties of TCFs. TCF shows best performance when it is annealed at 900 °C for 1 h in vacuum, and obtained sheet resistance is ∼1.89 kΩ/□ with transmittance of ∼62.53%.

Effect of applied voltage on surface properties of anodised titanium in mixture of β-glycerophosphate (β-GP) and calcium acetate (CA)

NASA Astrophysics Data System (ADS)

Chuan, Lee Te; Rathi, Muhammad Fareez Mohamad; Abidin, Muhamad Yusuf Zainal; Abdullah, Hasan Zuhudi; Idris, Maizlinda Izwana

2015-07-01

Anodic oxidation is a surface modification method which combines electric field driven metal and oxygen ion diffusion for formation of oxide layer on the anode surface. This method has been widely used to modify the surface morphology of biomaterial especially titanium. This study aimed to investigate the effect of applied voltage on titanium. Specifically, the titanium foil was anodised in mixture of β-glycerophosphate disodium salt pentahydrate (β-GP) and calcium acetate monohydrate (CA) with different applied voltage (50-350 V), electrolyte concentration (0.04 M β-GP + 0.4 M CA), anodising time (10minutes) and current density (50 and 70 mA.cm-2) at room temperature. Surface oxide properties of anodised titanium were characterised by digital single-lens reflex camera (DSLR camera), field emission scanning electron microscope (FESEM) and atomic force microscopy (AFM). At lower applied voltage (≤150 V), surface of titanium foils were relatively smooth. With increasing applied voltage (≥250 V), the oxide layer became more porous and donut-shaped pores were formed on the surface of titanium foils. The AFM results indicated that the surface roughness of anodised titanium increases with increasing of applied voltage. The porous and rough surface is able to promote the osseointegration and reduce the suffering time of patient.

Precisely detecting atomic position of atomic intensity images.

PubMed

Wang, Zhijun; Guo, Yaolin; Tang, Sai; Li, Junjie; Wang, Jincheng; Zhou, Yaohe

2015-03-01

We proposed a quantitative method to detect atomic position in atomic intensity images from experiments such as high-resolution transmission electron microscopy, atomic force microscopy, and simulation such as phase field crystal modeling. The evaluation of detection accuracy proves the excellent performance of the method. This method provides a chance to precisely determine atomic interactions based on the detected atomic positions from the atomic intensity image, and hence to investigate the related physical, chemical and electrical properties. Copyright © 2014 Elsevier B.V. All rights reserved.

Scanning ion-conductance and atomic force microscope with specialized sphere-shaped nanopippettes

NASA Astrophysics Data System (ADS)

Zhukov, M. V.; Sapozhnikov, I. D.; Golubok, A. O.; Chubinskiy-Nadezhdin, V. I.; Komissarenko, F. E.; Lukashenko, S. Y.

2017-11-01

A scanning ion-conductance microscope was designed on the basis of scanning probe microscope NanoTutor. The optimal parameters of nanopipettes fabrication were found according to scanning electron microscopy diagnostics, current-distance I (Z) and current-voltage characteristics. A comparison of images of test objects, including biological samples, was carried out in the modes of optical microscopy, atomic force microscopy and scanning ion-conductance microscopy. Sphere-shaped nanopippettes probes were developed and tested to increase the stability of pipettes, reduce invasiveness and improve image quality of atomic force microscopy in tapping mode. The efficiency of sphere-shaped nanopippettes is shown.

Preparation of CuO/NiO composite nanofibers by electrospinning and their application for electro-catalytic oxidation of hydrazine

NASA Astrophysics Data System (ADS)

Hosseini, Sayed Reza; Ghasemi, Shahram; Kamali-Rousta, Mina

2017-03-01

In present work, polyvinyl alcohol/copper acetate-nickel acetate composite nanofibers (PVA/Cu(OAc)2-Ni(OAc)2 NFs) with various weight percentages of Cu(OAc)2:Ni(OAc)2 such as 25:75, 50:50 and 75:25 are fabricated by electrospinning method. After this, the CuO/NiO composite NFs are produced after thermal treatment. A calcination temperature at about 600 °C is determined by thermal gravimetric analysis. Field-emission scanning electron microscopy (FE-SEM) for morphology characterization indicates that large quantities of the prepared PVA/Cu(OAc)2-Ni(OAc)2 composite fibers have smooth and bead-free surfaces. Fourier transform infrared spectroscopy, FE-SEM and energy dispersive X-ray spectroscopy are used to characterize the CuO/NiO composites. According to FE-SEM results, with increasing of Cu(OAc)2 content in polymeric solution, the fibers don't remain as continuous structures after calcination and accumulate in the form of nanoparticles. Also, a carbon paste electrode (CPE) bulky modified with CuO/NiO composites is used for investigation of the electro-catalytic oxidation of hydrazine hydrate in NaOH solution. The catalytic activities of the synthesized catalysts are studied through cyclic voltammetry, chronoamperometry and electrochemical impedance spectroscopy. The obtained results demonstrate that the most appropriate proportion of Cu(OAc)2:Ni(OAc)2 in electrospinning solution to enhance the electro-catalytic ability is 25:75.

In vitro degradation of a 3D porous Pennisetum purpureum/PLA biocomposite scaffold.

PubMed

Revati, R; Majid, M S Abdul; Ridzuan, M J M; Basaruddin, K S; Rahman Y, M N; Cheng, E M; Gibson, A G

2017-10-01

The in vitro degradation and mechanical properties of a 3D porous Pennisetum purpureum (PP)/polylactic acid (PLA)-based scaffold were investigated. In this study, composite scaffolds with PP to PLA ratios of 0%, 10%, 20%, and 30% were immersed in a PBS solution at 37°C for 40 days. Compression tests were conducted to evaluate the compressive strength and modulus of the scaffolds, according to ASTM F451-95. The compression strength of the scaffolds was found to increase from 1.94 to 9.32MPa, while the compressive modulus increased from 1.73 to 5.25MPa as the fillers' content increased from 0wt% to 30wt%. Moreover, field emission scanning electron microscopy (FESEM) and X-ray diffraction were employed to observe and analyse the microstructure and fibre-matrix interface. Interestingly, the degradation rate was reduced for the PLA/PP 20 scaffold, though insignificantly, this could be attributed to the improved mechanical properties and stronger fibre-matrix interface. Microstructure changes after degradation were observed using FESEM. The FESEM results indicated that a strong fibre-matrix interface was formed in the PLA/PP 20 scaffold, which reflected the addition of P. purpureum into PLA decreasing the degradation rate compared to in pure PLA scaffolds. The results suggest that the P. purpureum/PLA scaffold degradation rate can be altered and controlled to meet requirements imposed by a given tissue engineering application. Copyright © 2017 Elsevier Ltd. All rights reserved.

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

NASA Astrophysics Data System (ADS)

Bharathi, Devaraj; Vasantharaj, Seerangaraj; Bhuvaneshwari, V.

2018-05-01

The present study describes the antibacterial, anti-biofilm and photo catalytic activity of silver nanoparticles synthesized using Cordia dichotoma fruits (Cd-AgNPs) for the first time. The phyto-synthesized Cd-AgNPs were characterized by UV-Visible spectroscopy, Field emission-scanning electron microscopy (FE-SEM), Transmission electron microscopy (TEM), Energy dispersive x-ray spectrometer (EDX), Fourier transform infrared spectroscopy (FT-IR), and x-ray diffraction (XRD). FE-SEM and TEM observation showed that the average size of 2–60 nm with spherical shape of Cd-AgNPs and the presence of phyto-compounds which are responsible for capping and reduction were studied by FT-IR. XRD studies revealed the face-centered cubic structure of Cd-AgNPs. The synthesized Cd-AgNPs showed significant antibacterial activity against Gram-positive Staphylococcus aureus and Gram-negative Escherichia coli, assayed using agar well diffusion method. Phyto-synthesized Cd-AgNPs exhibited more than 90% inhibition of biofilm activity formed by S. aureus and E. coli. Furthermore, photocatalytic degradation of crystal violet (CV) under UV light irradiation using Cd-AgNPs was performed. Synthesized Cd-AgNPs exhibited ∼85% degradation activity for CV. Collectively, our findings suggest that C.dichotoma is a green source for the eco-friendly synthesis of Cd-AgNPs, which further can be used as a novel biocidal agent against bacterial pathogens and a potent photo catalytic agent.

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

NASA Astrophysics Data System (ADS)

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

2013-08-01

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

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

NASA Astrophysics Data System (ADS)

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

2018-04-01

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

Studies of silicon quantum dots prepared at different substrate temperatures

NASA Astrophysics Data System (ADS)

Al-Agel, Faisal A.; Suleiman, Jamal; Khan, Shamshad A.

2017-03-01

In this research work, we have synthesized silicon quantum dots at different substrate temperatures 193, 153 and 123 K at a fixed working pressure 5 Torr. of Argon gas. The structural studies of these silicon quantum dots have been undertaken using X-ray diffraction, Field Emission Scanning Electron Microscopy (FESEM) and High Resolution Transmission Electron Microscopy (HRTEM). The optical and electrical properties have been studied using UV-visible spectroscopy, Fourier transform infrared (FTIR) spectroscopy, Fluorescence spectroscopy and I-V measurement system. X-ray diffraction pattern of Si quantum dots prepared at different temperatures show the amorphous nature except for the quantum dots synthesized at 193 K which shows polycrystalline nature. FESEM images of samples suggest that the size of quantum dots varies from 2 to 8 nm. On the basis of UV-visible spectroscopy measurements, a direct band gap has been observed for Si quantum dots. FTIR spectra suggest that as-grown Si quantum dots are partially oxidized which is due exposure of as-prepared samples to air after taking out from the chamber. PL spectra of the synthesized silicon quantum dots show an intense peak at 444 nm, which may be attributed to the formation of Si quantum dots. Temperature dependence of dc conductivity suggests that the dc conductivity enhances exponentially by raising the temperature. On the basis above properties i.e. direct band gap, high absorption coefficient and high conductivity, these silicon quantum dots will be useful for the fabrication of solar cells.

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

NASA Astrophysics Data System (ADS)

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

2018-03-01

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

A convenient strategy to functionalize carbon nanotubes with ascorbic acid and its effect on the physical and thermomechanical properties of poly(amide–imide) composites

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

Mallakpour, Shadpour, E-mail: mallak@cc.iut.ac.ir; Nanotechnology and Advanced Materials Institute, Isfahan University of Technology, Isfahan 84156-83111, I.R. Iran; Zadehnazari, Amin

Multi-walled carbon nanotubes (MWCNTs) were functionalized by ascorbic acid by a fast strategy under microwave irradiation to improve interfacial interactions and dispersion of CNTs in a poly(amide–imide) (PAI) matrix. This technique provides a rapid and economically viable route to produce covalently functionalized CNTs. The as-prepared, new type of functionalized CNTs were analyzed by several techniques. The thermal stabilities and mechanical interfacial properties of CNT/PAI composites were investigated using several techniques. The dispersion state of CNTs in the PAI matrix was observed by field emission scanning electron microscopy (FE-SEM) and transmission electron microscopy (TEM). The mechanical interfacial property of the compositesmore » was significantly increased by the addition of ascorbic acid treated CNTs. The FE-SEM and TEM results showed that the separation and uniform dispersion of CNTs in the PAI matrix. The overview of these recent results is presented. -- Graphical abstract: Presentation of possible interactions of hydrogen bonding between the MWCNT-AS and the PAI chains. Highlights: • Surface functionalization of MWCNTs with ascorbic acid under microwave irradiation. • The MWCNT-AS/PAI composite films were fabricated by solution blending process. • Microstructure and MWCNT states in the composites were studied. • Thermal and mechanical properties of the composite films were evaluated. • Films of different contents of the MWCNTs-AS showed a superior tensile behavior.« less

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

NASA Astrophysics Data System (ADS)

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

2014-11-01

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

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

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

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

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

FS laser processing of bio-polymer thin films for studying cell-to-substrate specific response

NASA Astrophysics Data System (ADS)

Daskalova, A.; Nathala, Chandra S. R.; Kavatzikidou, P.; Ranella, A.; Szoszkiewicz, R.; Husinsky, W.; Fotakis, C.

2016-09-01

The use of ultra-short pulses for nanoengineering of biomaterials opens up possibilities for biological, medical and tissue engineering applications. Structuring the surface of a biomaterial into arrays with micro- and nanoscale features and architectures, defines new roadmaps to innovative engineering of materials. Thin films of novel collagen/elastin composite and gelatin were irradiated by Ti:sapphire fs laser in air at central wavelength 800 nm, with pulse durations in the range of 30 fs. The size and shape as well as morphological forms occurring in the resulted areas of interaction were analyzed as a function of irradiation fluence and number of pulses by atomic force microscopy (AFM). The fs interaction regime allows generation of well defined micro porous surface arrays. In this study we examined a novel composite consisting of collagen and elastin in order to create a biodegradable matrix to serve as a biomimetic surface for cell attachment. Confocal microscopy images of modified zones reveal formation of surface fringe patterns with orientation direction alongside the area of interaction. Outside the crater rim a wave-like topography pattern is observed. Structured, on a nanometer scale, surface array is employed for cell-culture experiments for testing cell's responses to substrate morphology. Mice fibroblasts migration was monitored after 3 days cultivation period using FESEM. We found that fibroblasts cells tend to migrate and adhere along the laser modified zones. The performed study proved that the immobilized collagen based biofilms suite as a template for successful fibroblasts cell guidance and orientation. Fs laser induced morphological modification of biomimetic materials exhibit direct control over fibroblasts behaviour due to induced change in their wettability state.

High-resolution structural and elemental analyses of calcium storage structures synthesized by the noble crayfish Astacus astacus.

PubMed

Luquet, Gilles; Salomé, Murielle; Ziegler, Andreas; Paris, Céline; Percot, Aline; Dauphin, Yannicke

2016-11-01

During premolt, crayfish develop deposits of calcium ions, called gastroliths, in their stomach wall. The stored calcium is used for the calcification of parts of the skeleton regularly renewed for allowing growth. Structural and molecular analyses of gastroliths have been primarily performed on three crayfish species, Orconectes virilis, Procambarus clarkii, and more recently, Cherax quadricarinatus. We have performed high-resolution analyses of gastroliths from the native noble crayfish, Astacus astacus, focusing on the microstructure, the mineralogical and elemental composition and distribution in a comparative perspective. Field emission scanning electron microscopy (FESEM) and atomic force microscopy (AFM) observations showed a classical layered microstructure composed of 200-nm diameter granules aligned along fibers. These granules are themselves composed of agglomerated nanogranules of 50nm-mean diameters. Denser regions of bigger fused granules are also present. Micro-Raman spectroscopy show that if A. astacus gastroliths, similarly to the other analyzed gastroliths, are mainly composed of amorphous calcium carbonate (ACC), they are also rich in amorphous calcium phosphate (ACP). The presence of a carotenoid pigment is also observed in A. astacus gastrolith contrary to C. quadricarinatus. Energy-dispersive X-ray spectroscopy (EDX) analyses demonstrate the presence of minor elements such as Mg, Sr, Si and P. The distribution of this last element is particularly heterogeneous. X-ray absorption near edge structure spectroscopy (XANES) reveals an alternation of layers more or less rich in phosphorus evidenced in the mineral phase as well as in the organic matrix in different molecular forms. Putative functions of the different P-comprising molecules are discussed. Copyright © 2016 Elsevier Inc. All rights reserved.

The controlled release of simvastatin from TiO2 nanotubes to promote osteoblast differentiation and inhibit osteoclast resorption

NASA Astrophysics Data System (ADS)

Lai, Min; Jin, Ziyang; Yang, Xinyi; Wang, Huaying; Xu, Kui

2017-02-01

The aim of this study was to fabricate a novel drug-releasing bioactive platform that has excellent potential for improving osteoblast differentiation and inhibiting osteoclast resorption. TiO2 nanotubes (TNTs) with an outer diameter of around 70 nm were prepared by an anodization method. TNTs were filled with simvastatin (SV) and then coated using chitosan/gelatin multilayers (TNT-SV-LBL). The successful fabrication of TNT-SV-LBL substrates was confirmed by field emission scanning electron microscopy (FE-SEM), atomic force microscopy (AFM), X-ray photoelectron spectroscopy (XPS) and contact angle measurement, respectively. The in vitro release behavior of simvastatin from TNT-SV-LBL substrates showed a sustained release as compared to the uncoated group. Osteoblasts adhering to TNT-SV-LBL substrates attached well and displayed significantly higher (p < 0.01) cell viability compared with the other substrates. More importantly, osteoblasts grown on TNT-SV-LBL substrates displayed a statistically significant (p < 0.01 or p < 0.05) increase in protein production levels of alkaline phosphatase (ALP), osteocalcin (OC) and mRNA expression of runt related transcription factor 2 (Runx2), ALP, collagen type I (Col I), osteopontin (OPN), OC and osteoprotegerin (OPG) compared to the other groups after 4, 7 and 14 days of culture, respectively. Additionally, multinuclear osteoclastic differentiation of RAW264.7 cells grown on TNT-SV-LBL substrates was inhibited as confirmed by tartrate-resistant acid phosphatase (TRAP) analysis. These results demonstrated that bio-functionalized substrates with SV and chitosan/gelatin multilayers have great potential for improving osteoblast differentiation, as well as inhibiting osteoclast formation. Therefore, these advanced surface and chemical capabilities make this substrate well suited for the development of a drug-releasing Ti implant for bone regeneration.

Leucine-rich amelogenin peptide (LRAP) as a surface primer for biomimetic remineralization of superficial enamel defects: An in vitro study.

PubMed

Shafiei, Farhad; Hossein, Bagheri G; Farajollahi, Mohammad M; Fathollah, Moztarzadeh; Marjan, Behroozibakhsh; Tahereh, Jafarzadeh Kashi

2015-01-01

This study was carried out to obtain more information about the assembly of hydroxyapatite bundles formed in the presence of Leucine-Rich Amelogenin Peptide (LRAP) and to evaluate its effect on the remineralization of enamel defects through a biomimetic approach. One or 2 mg/mL LRAP solutions containing 2.5 mM of Ca(+2) and 1.5 mM phosphate were prepared (pH = 7.2) and stored at 37 °C for 24 h. The products of the reaction were studied using atomic force microscopy (AFM), transmission electron microscopy (TEM), and selected area electron diffraction (SAED). Vickers surface microhardness recovery (SMR%) of acid-etched bovine enamel, with or without LRAP surface treatment, were calculated to evaluate the influence of peptide on the lesion remineralization. Distilled water and 1 or 2 mg/mL LRAP solution (pH = 7.2) were applied on the lesions and the specimens were incubated in mineralization solution (2.5mM Ca(+2) , 1.5mM PO4 (-3) , pH = 7.2) for 24 h. One-way ANOVA and Tukey's multi-comparison tests were used for statistical analysis. The pattern of enamel surface repair was studied using FE-SEM. AFM showed the formation of highly organized hierarchical structures, composed of hydroxyapatite (HA) crystals, similar to the dental enamel microstructure. ANOVA procedure showed significant effect of peptide treatment on the calculated SMR% (p < 0.001). Tukey's test revealed that peptide treated groups had significantly higher values of SMR%. In conclusion, LRAP is able to regulate the formation of HA and enhances the remineralization of acid-etched enamel as a surface treatment agent. © Wiley Periodicals, Inc.

Sonochemical assisted synthesis MnO2/RGO nanohybrid as effective electrode material for supercapacitor.

PubMed

Ghasemi, Shahram; Hosseini, Sayed Reza; Boore-Talari, Omid

2018-01-01

Manganese dioxide (MnO 2 ) needle-like nanostructures are successfully synthesized by a sonochemical method from an aqueous solution of potassium bromate and manganese sulfate. Also, hybride of MnO 2 nanoparticles wrapped with graphene oxide (GO) nanosheets are fabricated through an electrostatic coprecipitation procedure. With adjusting pH at 3.5, positive and negative charges are created on MnO 2 and on GO, respectively which can electrostatically attract to each other and coprecipitate. Then, MnO 2 /GO pasted on stainless steel mesh is electrochemically reduced by applying -1.1V to obtain MnO 2 /RGO nanohybrid. The structure and morphology of the MnO 2 and MnO 2 /RGO nanohybrid are examined by Raman spectroscopy, X-ray diffraction (XRD), atomic force microscopy (AFM), field emission-scanning electron microscopy (FE-SEM), energy dispersive spectroscopy (EDX), and thermal gravimetric analysis (TGA). The capacitive behaviors of MnO 2 and MnO 2 /RGO active materials on stainless steel meshes are investigated by cyclic voltammetry (CV), galvanostatic charge/discharge test and electrochemical impedance spectroscopy (EIS) by a three-electrode experimental setup in an aqueous solution of 0.5M sodium sulfate in the potential window of 0.0-1.0V. The electrochemical investigations reveal that MnO 2 /RGO exhibits high specific capacitance (C s ) of 375Fg -1 at current density of 1Ag -1 and good cycle stability (93% capacitance retention after 500 cycles at a scan rate of 200mVs -1 ). The obtained results give good prospect about the application of electrostatic coprecipitation method to prepare graphene/metal oxides nanohybrids as effective electrode materials for supercapacitors. Copyright © 2017 Elsevier B.V. All rights reserved.

Surface free energy of TiC layers deposited by electrophoretic deposition (EPD)

NASA Astrophysics Data System (ADS)

Gorji, Mohammad Reza; Sanjabi, Sohrab

2018-01-01

In this study porous structure coatings of bare TiC (i.e. 20 nm, 0.7 µm and 5/45 µm) and core-shell structures of TiC/NiP synthesized through electroless plating were deposited by EPD. Room temperature surface free energy (i.e. γs) of TiC and TiC/NiP coatings were determined via measuring contact angles of distilled water and diiodemethane liquids. The effect of Ni-P shell on spreading behavior of pure copper on porous EPD structures was also investigated by high temperature wetting experiments. According to the results existence of a Ni-P layer around the TiC particles has led to roughness (i.e. at least 0.1 µm), and porosity mean length (i.e. at least 1 µm) increase. This might be related to various sizes of TiC agglomerates formed during electroless plating. It has been observed that room temperature γs changed from 44.49 to 54.12 mJ.m-2 as a consequence of particle size enlargement for TiC. The highest and lowest (67.25 and 44.49 mJ.m-2) γs were measured for TiC nanoparticles which showed 1.5 times increase in surface free energy after being plated with Ni-P. It was also observed that plating Ni-P altered non-spreading (θs > 100 o) behavior of TiC to full-spreading ((θs 0o)) which can be useful for preparation of hard coatings by infiltration sintering phenomenon. Zeta potential of EPD suspensions, morphology, phase structure and topography of as-EPD layers were investigated through Zetasizer, field emission scanning electron microscopy (FESEM), X-ray diffraction (XRD) and atomic force microscopy (AFM) instruments respectively.

Surface modification of TiO2 nanotubes with osteogenic growth peptide to enhance osteoblast differentiation.

PubMed

Lai, Min; Jin, Ziyang; Su, Zhiguo

2017-04-01

To investigate the influence of surface-biofunctionalized substrates on osteoblast behavior, a layer of aligned TiO 2 nanotubes with a diameter of around 70nm was fabricated on titanium surface by anodization, and then osteogenic growth peptide (OGP) was conjugated onto TiO 2 nanotubes through the intermediate layer of polydopamine. The morphology, composition and wettability of different surfaces were characterized by field-emission scanning electron microscopy (FE-SEM), atomic force microscopy (AFM), X-ray photoelectron spectroscopy (XPS) and contact angle measurements, respectively. The effects of OGP-modified TiO 2 nanotube substrates on the morphology, proliferation and differentiation of osteoblasts were examined in vitro. Immunofluorescence staining revealed that the OGP-functionalized TiO 2 nanotubes were favorable for cell spreading. However, there was no significant difference in cell proliferation observed among the different groups. Cells grown onto OGP-functionalized TiO 2 nanotubes showed significantly higher (p<0.05 or p<0.01) levels of alkaline phosphatase (ALP) and mineralization after 4, 7 and 14days of culture, respectively. Cells grown on OGP-functionalized TiO 2 nanotubes had significantly higher (p<0.05 or p<0.01) expression of osteogenic-related genes including runt related transcription factor 2 (Runx2), ALP, collagen type I (Col I), osteopontin (OPN) and osteocalcin (OC) after 14days of culture. These data suggest that surface functionalization of TiO 2 nanotubes with OGP was beneficial for cell spreading and differentiation. This study provides a novel platform for the development and fabrication of titanium-based implants that enhance the propensity for osseointegration between the native tissue and implant interface. Copyright © 2016 Elsevier B.V. All rights reserved.

Photocatalyst based on TiO2 nanotube arrays co-decorated with CdS quantum dots and reduced graphene oxide irradiated by γ rays for effective degradation of ethylene

NASA Astrophysics Data System (ADS)

Zhang, Quan; Ye, Shengying; Song, Xianliang; Luo, Shucan

2018-06-01

We report herein a means of transforming TiO2 nanotube arrays (TNAs) from an amorphous state to an anatase crystal state (denoted as ∗TNAs), and present a single-step synthetic route for preparing CdS quantum dots (CdS QDs) as well as reduced graphene oxide (rGO) through gamma-ray irradiation. The as-prepared ∗TNAs, CdS QDs, and rGO, which had all been subjected to gamma-ray irradiation, were then assembled together to produce the desired heterojunction (denoted as CdS QDs/rGO-∗TNAs). X-ray diffraction (XRD), field-emission scanning electron microscopy (FESEM), ultraviolet/visible diffuse-reflectance spectroscopy (UV/Vis DRS), Fourier-transform infrared spectroscopy (FTIR), micro-Raman spectrometry (RS), atomic force microscopy (AFM), and X-ray photoelectron spectroscopy (XPS) have been applied to characterize the appearance and performance of this photocatalyst. The photocatalytic activity of CdS QDs/rGO-∗TNAs towards ethylene degradation has been measured by placing it in a simulated cold-storage environment, the temperature and humidity of which were set at about 3 ± 1 °C and 75-90%, respectively. The results showed that the rate constant (K) of ethylene degradation could reach up to 1.07 × 10-3 min-1 with CdS QDs/rGO-∗TNAs, as compared to 2.30 × 10-4 min-1 with ∗TNAs and 6.25 × 10-4 min-1 with CdS QDs-∗TNAs, indicating that the constructed CdS QDs/rGO-∗TNAs constitutes a promising photocatalyst for ethylene removal in a cold storage environment.

Optimized hydrogen sensing characteristic of Pd/ZnO nanoparticles based Schottky diode on glass substrate

NASA Astrophysics Data System (ADS)

Chandra, Lalit; Sahu, Praveen Kumar; Dwivedi, R.; Mishra, V. N.

2017-10-01

The present work deals with the development of the Pd/ZnO naoparticles based sensor for detection of hydrogen (H2) gas at relatively low temperature (75-110 °C). Pd/ZnO Schottky diode was fabricated by ZnO nanoparticles based thin film on glass substrate using sol-gel spin coating technique. These ZnO nanoparticles have been characterized by x-ray diffraction (XRD), atomic force microscopy (AFM), energy dispersive x-ray spectroscope (EDS), and field emission scanning electron microscope (FE-SEM) which reveals the ZnO film having particles size in the range of ~25 to ~110 nm with ~52.73 nm surface roughness. Gas dependent diode parameters such as barrier height and ideality factor have been evaluated upon exposure of H2 gas concentration in the range from 200-2000 ppm over the temperature range from 75 to 110 °C. The sensitivity of the Pd/ZnO sensor has been studied in terms of change in diode forward current upon exposure to H2 gas. Experimental result shows the optimized sensitivity ~246.22% for H2 concentration of 2000 ppm at temperature 90 °C. The hydrogen sensing mechanism has been explained by surface and subsurface adsorption of H2 molecules on Pd surface; subsequently, dissociation of H2 molecules into H  +  H atoms and diffusion to trap sites (oxygen ions) available on ZnO surface, resulting in formation of dipole moments at Pd/ZnO interface. The variation in the sensitivity, response and recovery time with temperature of Pd/ZnO sensor has also been studied.

Investigating the structure and biocompatibility of niobium and titanium oxides as coatings for orthopedic metallic implants.

PubMed

Pradhan, D; Wren, A W; Misture, S T; Mellott, N P

2016-01-01

Applying sol gel based coatings to orthopedic metallic implant materials can significantly improve their properties and lifespan in vivo. For this work, niobium (Nb2O5) and titanium (TiO2) oxides were prepared via solution processing in order to determine the effect of atomic arrangement (amorphous/crystalline) on bioactivity. Thermal evaluation on the synthesized materials identified an endotherm for Nb2O5 at 75 °C with 40% weight loss below 400 °C, and minimal weight loss between 400 and 850 °C. Regarding TiO2 an endotherm was present at 92 °C with 25% weight loss below 400 °C, and 4% between 400 and 850 °C. Phase evolution was determined using High Temperature X-ray Diffraction (HT-XRD) where amorphous-Nb2O5 (450 °C), hexagonal-Nb2O5 (525 °C), orthorhombic-Nb2O5 (650 °C), amorphous-TiO2 (275 °C) and tetragonal TiO2 (500 °C) structures were produced. Simulated body fluid (SBF) testing was conducted over 1, 7 and 30 days and resulted in positive chemical and morphological changes for crystalline Nb2O5 (525 °C) and TiO2 (500 °C) after 30 days of incubation. Rod-like CaP deposits were observed on the surfaces using Scanning Electron Microscopy (FE-SEM) and Grazing Incidence-X-ray Diffraction (GI-XRD) shows that the deposits were X-ray amorphous. Cell viability was higher with the TiO2 (122%) samples when compared to the growing cell population while Nb2O5 samples exhibited a range of viability (64-105%), partially dependent on materials atomic structure. Copyright © 2015 Elsevier B.V. All rights reserved.

Final Technical Report for Award DESC0011912, "Trimodal Tapping Mode Atomic Force Microscopy: Simultaneous 4D Mapping of Conservative and Dissipative Probe-Sample Interactions of Energy-Relevant Materials”

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

Solares, Santiago D.

The final project report covering the period 7/1/14-6/30/17 provides an overview of the technical accomplishments in the areas of (i) fundamental viscoelasticity, (ii) multifrequency atomic force microscopy, and (iii) characterization of energy-relevant materials with atomic force microscopy. A list of publications supported by the project is also provided.

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

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

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

Elemental Identification by Combining Atomic Force Microscopy and Kelvin Probe Force Microscopy.

PubMed

Schulz, Fabian; Ritala, Juha; Krejčí, Ondrej; Seitsonen, Ari Paavo; Foster, Adam S; Liljeroth, Peter

2018-06-01

There are currently no experimental techniques that combine atomic-resolution imaging with elemental sensitivity and chemical fingerprinting on single molecules. The advent of using molecular-modified tips in noncontact atomic force microscopy (nc-AFM) has made it possible to image (planar) molecules with atomic resolution. However, the mechanisms responsible for elemental contrast with passivated tips are not fully understood. Here, we investigate elemental contrast by carrying out both nc-AFM and Kelvin probe force microscopy (KPFM) experiments on epitaxial monolayer hexagonal boron nitride (hBN) on Ir(111). The hBN overlayer is inert, and the in-plane bonds connecting nearest-neighbor boron and nitrogen atoms possess strong covalent character and a bond length of only ∼1.45 Å. Nevertheless, constant-height maps of both the frequency shift Δ f and the local contact potential difference exhibit striking sublattice asymmetry. We match the different atomic sites with the observed contrast by comparison with nc-AFM image simulations based on the density functional theory optimized hBN/Ir(111) geometry, which yields detailed information on the origin of the atomic-scale contrast.

Optimization study of direct morphology observation by cold field emission SEM without gold coating.

PubMed

He, Dan; Fu, Cheng; Xue, Zhigang

2018-06-01

Gold coating is a general operation that is generally applied on non-conductive or low conductive materials, during which the morphology of the materials can be examined by scanning electron microscopy (SEM). However, fatal deficiencies in the materials can result in irreversible distortion and damage. The present study directly characterized different low conductive materials such as hydroxyapatite, modified poly(vinylidene fluoride) (PVDF) fiber, and zinc oxide nanopillar by cold field emission scanning electron microscopy (FE-SEM) without a gold coating. According to the characteristics of the low conductive materials, various test conditions, such as different working signal modes, accelerating voltages, electron beam spots, and working distances, were characterized to determine the best morphological observations of each sample. Copyright © 2018 Elsevier Ltd. All rights reserved.

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

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

NASA Astrophysics Data System (ADS)

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

2018-04-01

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

Surface Biology of DNA by Atomic Force Microscopy

NASA Astrophysics Data System (ADS)

Hansma, Helen G.

2001-10-01

The atomic force microscope operates on surfaces. Since surfaces occupy much of the space in living organisms, surface biology is a valid and valuable form of biology that has been difficult to investigate in the past owing to a lack of good technology. Atomic force microscopy (AFM) of DNA has been used to investigate DNA condensation for gene therapy, DNA mapping and sizing, and a few applications to cancer research and to nanotechnology. Some of the most exciting new applications for atomic force microscopy of DNA involve pulling on single DNA molecules to obtain measurements of single-molecule mechanics and thermodynamics.

Interplay between Switching Driven by the Tunneling Current and Atomic Force of a Bistable Four-Atom Si Quantum Dot.

PubMed

Yamazaki, Shiro; Maeda, Keisuke; Sugimoto, Yoshiaki; Abe, Masayuki; Zobač, Vladimír; Pou, Pablo; Rodrigo, Lucia; Mutombo, Pingo; Pérez, Ruben; Jelínek, Pavel; Morita, Seizo

2015-07-08

We assemble bistable silicon quantum dots consisting of four buckled atoms (Si4-QD) using atom manipulation. We demonstrate two competing atom switching mechanisms, downward switching induced by tunneling current of scanning tunneling microscopy (STM) and opposite upward switching induced by atomic force of atomic force microscopy (AFM). Simultaneous application of competing current and force allows us to tune switching direction continuously. Assembly of the few-atom Si-QDs and controlling their states using versatile combined AFM/STM will contribute to further miniaturization of nanodevices.

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

NASA Astrophysics Data System (ADS)

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

2016-08-01

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

ZnS nanostructured thin-films deposited by successive ionic layer adsorption and reaction

NASA Astrophysics Data System (ADS)

Deshmukh, S. G.; Jariwala, Akshay; Agarwal, Anubha; Patel, Chetna; Panchal, A. K.; Kheraj, Vipul

2016-04-01

ZnS thin films were grown on glass substrate using successive ionic layer adsorption and reaction (SILAR) technique at room temperature. Aqueous solutions of ZnCl2 and Na2S were used as precursors. The X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), Raman spectroscopy and optical absorption measurements were applied to study the structural, surface morphology and optical properties of as-deposited ZnS thin films. The X-ray diffraction profiles revealed that ZnS thin films consist of crystalline grains with cubic phase. Spherical nano grains of random size and well covered on the glass substrate were observed from FESEM. The average grain size were found to be 77 nm, 100 nm and 124 nm for 20 cycles, 40 cycles and 60 cycles samples respectively. For 60 cycle sample, Raman spectra show two prominent peaks at 554 cm-1 and 1094 cm-1. The optical band gap values were found to be 3.76 eV, 3.72 eV and 3.67 eV for 20 cycle, 40 cycle and 60 cycle samples respectively.

Highly Sensitive Detection of Target Biomolecules on Cell Surface Using Gold Nanoparticle Conjugated with Aptamer Probe

NASA Astrophysics Data System (ADS)

Kim, Hyonchol; Terazono, Hideyuki; Hayashi, Masahito; Takei, Hiroyuki; Yasuda, Kenji

2012-06-01

A method of gold nanoparticle (Au NP) labeling with backscattered electron (BE) imaging of field emission scanning electron microscopy (FE-SEM) was applied for specific detection of target biomolecules on a cell surface. A single-stranded DNA aptamer, which specifically binds to the target molecule on a human acute lymphoblastic leukemia cell, was conjugated with a 20 nm Au NP and used as a probe to label its target molecule on the cell. The Au NP probe was incubated with the cell, and the interaction was confirmed using BE imaging of FE-SEM through direct counting of the number of Au NPs attached on the target cell surface. Specific Au NP-aptamer probes were observed on a single cell surface and their spatial distributions including submicron-order localizations were also clearly visualized, whereas the nonspecific aptamer probes were not observed on it. The aptamer probe can be potentially dislodged from the cell surface with treatment of nucleases, indicating that Au NP-conjugated aptamer probes can be used as sensitive and reversible probes to label target biomolecules on cells.

Effect of mechanical vibrations on the wear behavior of AZ91 Mg alloy

NASA Astrophysics Data System (ADS)

Chaturvedi, V.; Pandel, U.; Sharma, A.

2018-02-01

AZ91 Mg alloy is the most promising alloy used for structural applications. The vibration induced methods are effective and economic viable in term of mechanical properties. Sliding wear tests were performed on AZ91 Mg alloy using a pin-on- disc configuration. Wear rates were measured at 5 N and 10N at a sliding velocity of 1m/s for varied frequency within the range of 5- 25Hz and a constant amplitude of 2mm. Microstructures of worn surfaces and wear debris were characterized by field emission scanning electron microscopy (FESEM). It is observed that wear resistance of vibrated AZ91 alloy at 15Hz frequency ad 2mm amplitude was superior than cast AZ91 Mg alloy. Finer grain size and equiaxed grain shape both are important parameters for better wear resistance in vibrated AZ91 Mg alloys. FESEM analysis revealed that wear is considerably affected due to frictional heat generated by the relative motion between AZ91 Mg alloy and EN31 steel surface. No single mechanism was responsible for material loss.

An evaluation of UO2-CNT composites made by SPS as an accident tolerant nuclear fuel pellet and the feasibility of SPS as an economical fabrication process for the nuclear fuel cycle

NASA Astrophysics Data System (ADS)

Cartas, Andrew R.

The innovative and advanced purpose of this study is to understand and establish proper sintering procedures for Spark Plasma Sintering process in order to fabricate high density, high thermal conductivity UO2 -CNT pellets. Mixing quality and chemical reactions have been investigated by field emission scanning electron microscopy (FESEM), wavelength dispersive spectroscopy (WDS), and X-ray diffraction (XRD). The effect of various types of CNTs on the mixing and sintering quality of UO2-CNT pellets with SPS processing have been examined. The Archimedes Immersion Method, laser flash method, and FE-SEM will be used to investigate the density, thermal conductivity, grain size, pinning effects, and CNT dispersion of fabricated UO2-CNT pellets. Pre-fabricated CNT's were added to UO 2 powder and dispersed via sonication and/or ball milling and then made into composite nuclear pellets. An investigation of the economic impact of SPS on the nuclear fuel cycle for producing pure and composite UO2 fuels was conducted.

Drug release characteristics of quercetin-loaded TiO2 nanotubes coated with chitosan.

PubMed

Mohan, L; Anandan, C; Rajendran, N

2016-12-01

TiO 2 nanotubes formed by anodic oxidation of Ti-6Al-7Nb were loaded with quercetin (TNTQ) and chitosan was coated on the top of the quercetin (TNTQC) to various thicknesses. Field emission scanning electron microscopy (FESEM), 3D and 2D analyses were used to characterize the samples. The drug release studies of TNTQ and TNTQC were studied in Hanks' solution for 192h. The studies showed that the native oxide on the sample is substituted by self assembled nanotube arrays by anodisation. FESEM images of chitosan-loaded TNT samples showed that filling of chitosan takes place in inter-tubular space and pores. Drug release studies revealed that the release of drug into the local environment during that duration was constant. The local concentration of the drug can be controlled and tuned by controlling the thickness of the chitosan (0.6, 1 and 3μm) to fit into an optimal therapeutic window in order to treat postoperative infections, inflammation and for quick healing with better osseointegration of the titanium implants. Copyright © 2016 Elsevier B.V. All rights reserved.

Synthesis and characterization of Eu{sup 3+}:Gd{sub 2}O{sub 3} hollow spheres for biomedical applications

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

Kumari, Manisha, E-mail: guptamanisha69@yahoo.co.in; Sharma, Prashant K., E-mail: prashantnac@gmail.com

Multifunctional magnetic Nanoparticles (MFMNPs) are potentially applicable in both drug delivery systems (DDS) and hyperthermia treatment. Structural, surface morphology and optical property were investigated by X-ray diffraction (XRD), Field emission scanning electron microscopy (FE-SEM) and photoluminescence (PL) measurement. Uniform Eu{sup 3+}:Gd{sub 2}O{sub 3} hollow microspheres of 1.8-2.0 μm diameters were synthesized by template based approach. We found that synthesized Hollow spheres are 100 nm in thickness. FE-SEM images revealed that the synthesized material are hollow in structure with good porous structure and these pores work as pathway for releasing drugs from the hollow particle inside. Luminescent properties of material were studiedmore » by room temperature photoluminescence emission spectra under the excitation of 275 nm. Material exhibit bright red emission corresponding to the {sup 5}D{sub 0}-{sup 7}F{sub 2} transition of the activator ions under ultraviolet light excitation, which might find potential applications in fields such as drug delivery or biological labeling because of their excellent luminescence properties.« less

A dipeptide-based superhydrogel: Removal of toxic dyes and heavy metal ions from waste water.

PubMed

Nandi, Nibedita; Baral, Abhishek; Basu, Kingshuk; Roy, Subhasish; Banerjee, Arindam

2017-01-01

A short peptide-based molecule has been found to form a strong hydrogel at phosphate buffer solution of pH 7.46. The hydrogel has been characterized thoroughly using various techniques including field emission scanning electron microscopy (FE-SEM), wide angle powder X-ray diffraction (PXRD), and rheological analysis. It has been observed from FE-SEM images that entangled nanofiber network is responsible for gelation. Rheological investigation demonstrates that the self-assembly of this synthetic dipeptide results in the formation of mechanically strong hydrogel with storage modulus (G') around 10 4 Pa. This gel has been used for removing both cationic and anionic toxic organic dyes (Brilliant Blue, Congo red, Malachite Green, Rhodamine B) and metal ions (Co 2+ and Ni 2+ ) from waste water. Moreover, only a small amount of the gelator is required (less than 1 mg/mL) for preparation of this superhydrogel and even this hydrogel can be reused three times for dye/metal ion absorption. This signifies the importance of the hydrogel towards waste water management. © 2016 Wiley Periodicals, Inc.

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

NASA Astrophysics Data System (ADS)

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

2018-05-01

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

Neurite outgrowth stimulatory effects of myco synthesized AuNPs from Hericium erinaceus (Bull.: Fr.) Pers. on pheochromocytoma (PC-12) cells

PubMed Central

Raman, Jegadeesh; Lakshmanan, Hariprasath; John, Priscilla A; Zhijian, Chan; Periasamy, Vengadesh; David, Pamela; Naidu, Murali; Sabaratnam, Vikineswary

2015-01-01

Background Hericium erinaceus has been reported to have a wide range of medicinal properties such as stimulation of neurite outgrowth, promotion of functional recovery of axonotmetic peroneal nerve injury, antioxidant, antihypertensive, and antidiabetic properties. In recent years, the green synthesis of gold nanoparticles (AuNPs) has attracted intense interest due to the potential use in biomedical applications. The aim of this study was to investigate the effects of AuNPs from aqueous extract of H. erinaceus on neurite outgrowth of rat pheochromocytoma (PC-12) cells. Methods The formation of AuNPs was characterized by UV–visible spectrum, energy dispersive X-ray (EDX), field-emission scanning electron microscope (FESEM), transmission electron microscopy (TEM), particle size distribution, and Fourier transform-infrared spectroscopy (FTIR). Furthermore, the neurite extension study of synthesized AuNPs was evaluated by in vitro assay. Results The AuNPs exhibited maximum absorbance between 510 and 600 nm in UV–visible spectrum. FESEM and TEM images showed the existence of nanoparticles with sizes of 20–40 nm. FTIR measurements were carried out to identify the possible biomolecules responsible for capping and efficient stabilization of the nanoparticles. The purity and the crystalline properties were confirmed by EDX diffraction analysis, which showed strong signals with energy peaks in the range of 2–2.4 keV, indicating the existence of gold atoms. The synthesized AuNPs showed significant neurite extension on PC-12 cells. Nerve growth factor 50 ng/mL was used as a positive control. Treatment with different concentrations (nanograms) of AuNPs resulted in neuronal differentiation and neuronal elongation. AuNPs induced maximum neurite outgrowth of 13% at 600 ng/mL concentration. Conclusion In this study, the AuNPs synthesis was achieved by a simple, low-cost, and rapid bioreduction approach. AuNPs were shown to have potential neuronal differentiation and stimulated neurite outgrowth. The water-soluble bioconstituents could be responsible for the neuroactivity. This is the first report for the biosynthesis of AuNPs using the hot aqueous extract of H. erinaceus. PMID:26425086

Neurite outgrowth stimulatory effects of myco synthesized AuNPs from Hericium erinaceus (Bull.: Fr.) Pers. on pheochromocytoma (PC-12) cells.

PubMed

Raman, Jegadeesh; Lakshmanan, Hariprasath; John, Priscilla A; Zhijian, Chan; Periasamy, Vengadesh; David, Pamela; Naidu, Murali; Sabaratnam, Vikineswary

2015-01-01

Hericium erinaceus has been reported to have a wide range of medicinal properties such as stimulation of neurite outgrowth, promotion of functional recovery of axonotmetic peroneal nerve injury, antioxidant, antihypertensive, and antidiabetic properties. In recent years, the green synthesis of gold nanoparticles (AuNPs) has attracted intense interest due to the potential use in biomedical applications. The aim of this study was to investigate the effects of AuNPs from aqueous extract of H. erinaceus on neurite outgrowth of rat pheochromocytoma (PC-12) cells. The formation of AuNPs was characterized by UV-visible spectrum, energy dispersive X-ray (EDX), field-emission scanning electron microscope (FESEM), transmission electron microscopy (TEM), particle size distribution, and Fourier transform-infrared spectroscopy (FTIR). Furthermore, the neurite extension study of synthesized AuNPs was evaluated by in vitro assay. The AuNPs exhibited maximum absorbance between 510 and 600 nm in UV-visible spectrum. FESEM and TEM images showed the existence of nanoparticles with sizes of 20-40 nm. FTIR measurements were carried out to identify the possible biomolecules responsible for capping and efficient stabilization of the nanoparticles. The purity and the crystalline properties were confirmed by EDX diffraction analysis, which showed strong signals with energy peaks in the range of 2-2.4 keV, indicating the existence of gold atoms. The synthesized AuNPs showed significant neurite extension on PC-12 cells. Nerve growth factor 50 ng/mL was used as a positive control. Treatment with different concentrations (nanograms) of AuNPs resulted in neuronal differentiation and neuronal elongation. AuNPs induced maximum neurite outgrowth of 13% at 600 ng/mL concentration. In this study, the AuNPs synthesis was achieved by a simple, low-cost, and rapid bioreduction approach. AuNPs were shown to have potential neuronal differentiation and stimulated neurite outgrowth. The water-soluble bioconstituents could be responsible for the neuroactivity. This is the first report for the biosynthesis of AuNPs using the hot aqueous extract of H. erinaceus.

Ultrasonic assisted synthesis of Bikitaite zeolite: A potential material for hydrogen storage application.

PubMed

Roy, Priyanka; Das, Nandini

2017-05-01

Li containing Bikitaite zeolite has been synthesized by an ultrasound-assisted method and used as a potential material for hydrogen storage application. The Sonication energy was varied from 150W to 250W and irradiation time from 3h to 6h. The Bikitaite nanoparticles were characterized by X-ray diffraction (XRD), infrared (IR) spectral analysis, and field-emission scanning electron microscopy (FESEM) thermo-gravimetrical analysis and differential thermal analysis (TGA, DTA). XRD and IR results showed that phase pure, nano crystalline Bikitaite zeolites were started forming after 3h irradiation and 72h of aging with a sonication energy of 150W and nano crystalline Bikitaite zeolite with prominent peaks were obtained after 6h irradiation of 250W sonic energy. The Brunauer-Emmett-Teller (BET) surface area of the powder by N 2 adsorption-desorption measurements was found to be 209m 2 /g. The TEM micrograph and elemental analysis showed that desired atomic ratio of the zeolite was obtained after 6h irradiation. For comparison, sonochemical method, followed by the hydrothermal method, with same initial sol composition was studied. The effect of ultrasonic energy and irradiation time showed that with increasing sonication energy, and sonication time phase formation was almost completed. The FESEM images revealed that 50nm zeolite crystals were formed at room temperature. However, agglomerated particles having woollen ball like structure was obtained by sonochemical method followed by hydrothermal treatment at 100°C for 24h. The hydrogen adsorption capacity of Bikitaite zeolite with different Li content, has been investigated. Experimental results indicated that the hydrogen adsorption capacities were dominantly related to their surface areas as well as total pore volume of the zeolite. The hydrogen adsorption capacity of 143.2c.c/g was obtained at 77K and ambient pressure of (0.11MPa) for the Bikitaite zeolite with 100% Li, which was higher than the reported values for other zeolites. To the best of our knowledge, there is no report on the synthesis of a Bikitaite zeolite by sonochemical method for H 2 storage. Copyright © 2016. Published by Elsevier B.V.

Progress on BN and Doped-BN Coatings on Woven Fabrics

NASA Technical Reports Server (NTRS)

Hurwitz, Frances I.; Scott, John M.; Chayka, Paul V.

2001-01-01

A novel, multistep process for applying interface coatings to woven structures using a pulsed CVD process is being evaluated. Borazine (B3N3H6), a neat liquid, and several Si precursors are used in the process to produce BN and SiBN coatings on Hi- Nicalon fabrics and preforms. A three variable, two level, full factorial matrix is proposed to define the influence of processing parameters. Coating morphology, uniformity and chemistry are characterized by field emission scanning electron microscopy (FESEM), energy dispersive (EDS) and Auger spectroscopies.

Solvothermal synthesis of fusiform hexagonal prism SrCO{sub 3} microrods via ethylene glycol solution

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

Shi Liange; Du Fanglin

2007-08-07

Fusiform hexagonal prism SrCO{sub 3} microrods were prepared by a simple solvothermal route at 120 deg. C, and characterized by X-ray powder diffraction (XRD), field-emission scanning electron microscopy (FE-SEM) and Fourier transform infrared (FT-IR) spectroscopy. By controlling the content of ethylene glycol (EG), it was found that ethylene glycol (EG) played an important role in the formation of such SrCO{sub 3} microrods. Finally, effects of other solvents on the products, including 1,2-propanediol and glycerin, were also investigated.

NiCo2S4 nanorod embedded rGO sheets as electrodes for supercapacitor

NASA Astrophysics Data System (ADS)

Sarkar, Aatreyee; Bera, Supriya; Chakraborty, Amit Kumar

2018-04-01

We report the synthesis of a hybrid nanostructure based on NiCo2S4 and reduced graphene oxide (rGO) following a facile hydrothermal method. X-ray diffraction (XRD), and electron microscopy (FESEM and HRTEM) analyses showed rod-like NiCo2S4 nanostructures embedded in rGO sheets. The electrochemical analysis of the synthesized nanohybrid using cyclic voltammetry (CV) and galvanostatic charge discharge (GCD) revealed specific capacitance of 410 F/gm indicating its suitability as a good electrode material for supercapacitor.

Synthesis and Raman scattering of GaN nanorings, nanoribbons and nanowires

NASA Astrophysics Data System (ADS)

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

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

Nanospheres Encapsulating Anti-Leishmanial Drugs for Their Specific Macrophage Targeting, Reduced Toxicity, and Deliberate Intracellular Release

PubMed Central

Shukla, Anil Kumar; Patra, Sanjukta

2012-01-01

Abstract The current work focuses on the study of polymeric, biodegradable nanoparticles (NPs) for the encapsulation of doxorubicin and mitomycin C (anti-leishmanial drugs), and their efficient delivery to macrophages, the parasite's home. The biodegradable polymer methoxypoly-(ethylene glycol)-b-poly (lactic acid) (MPEG-PLA) was used to prepare polymeric NPs encapsulating doxorubicin and mitomycin C. The morphology, mean diameter, and surface area of spherical NPs were determined by transmission electron microscopy (TEM), field emission scanning electron microscopy (FESEM), and BET surface area analysis. X-ray diffraction was performed to validate drug encapsulation. An in vitro release profile of the drugs suggested a fairly slow release. These polymeric NPs were efficiently capable of releasing drug inside macrophages at a slower pace than the free drug, which was monitored by epi-fluorescence microscopy. Encapsulation of doxorubicin and mitomycin C into NPs also decreases cellular toxicity in mouse macrophages (J774.1A). PMID:22925019

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.

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

NASA Astrophysics Data System (ADS)

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

2011-05-01

Bovine femur bone hydroxyapatite (HA) containing silver (Ag) nanoparticles was synthesized by thermal decomposition method and subsequent reduction of silver nitrate with N, N-dimethylformamide (DMF) in the presence of poly(vinylacetate) (PVAc). The structural, morphological, and chemical properties of the HA-Ag nanoparticles were characterized using X-ray diffraction (XRD), scanning electron microscopy (SEM), field-emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), and X-ray photoelectron spectroscopy (XPS). TEM images showed that the Ag nanoparticles with size ranging from 8 to 20 nm and were arranged at the periphery of HA crystals. Bactericidal activity of HA-Ag with different concentration of Ag nanoparticles immobilized on the surface of HA was investigated against gram-positive Staphylococcus aureus ( S. aureus, non-MRSA), Methicillin resistant S. aureus (MRSA) and gram-negative Escherichia coli ( E. coli) by the disc diffusion susceptibility test. The HA-Ag nanoparticles showed that broad spectrum activity against non-MRSA, MRSA, and E. coli bacterial strains.

A Fast Response Ammonia Sensor Based on Coaxial PPy-PAN Nanofiber Yarn.

PubMed

Liu, Penghong; Wu, Shaohua; Zhang, Yue; Zhang, Hongnan; Qin, Xiaohong

2016-06-23

Highly orientated polypyrrole (PPy)-coated polyacrylonitrile (PAN) (PPy-PAN) nanofiber yarn was prepared with an electrospinning technique and in-situ chemical polymerization. The morphology and chemical structure of PPy-PAN nanofiber yarn was characterized by scanning electron microscopy (SEM), field emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM), and fourier transform infrared spectroscopy (FTIR), which indicated that the PPy as the shell layer was homogeneously and uniformly polymerized on the surface of PAN nanofiber. The effects of different concentration of doping acid on the responses of PPy-PAN nanofiber yarn sensor were investigated. The electrical responses of the gas sensor based on the PPy-PAN nanofiber yarn to ammonia were investigated at room temperature. The nanoyarn sensor composed of uniaxially aligned PPy-PAN nanofibers with a one-dimensional structure exhibited a transient response, and the response time was less than 1 s. The excellent sensing properties mentioned above give rise to good potential application prospects in the field of ammonia sensor.

Isolating and moving single atoms using silicon nanocrystals

DOEpatents

Carroll, Malcolm S.

2010-09-07

A method is disclosed for isolating single atoms of an atomic species of interest by locating the atoms within silicon nanocrystals. This can be done by implanting, on the average, a single atom of the atomic species of interest into each nanocrystal, and then measuring an electrical charge distribution on the nanocrystals with scanning capacitance microscopy (SCM) or electrostatic force microscopy (EFM) to identify and select those nanocrystals having exactly one atom of the atomic species of interest therein. The nanocrystals with the single atom of the atomic species of interest therein can be sorted and moved using an atomic force microscope (AFM) tip. The method is useful for forming nanoscale electronic and optical devices including quantum computers and single-photon light sources.

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

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

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

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

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

NASA Astrophysics Data System (ADS)

Arulmozhi, K. T.; Mythili, N.

2013-12-01

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

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

NASA Astrophysics Data System (ADS)

Purty, B.; Choudhary, R. B.

2018-04-01

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

Synthesis, 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%.

Effect of annealing temperature on the properties of copper oxide films prepared by dip coating technique

NASA Astrophysics Data System (ADS)

Raship, N. A.; Sahdan, M. Z.; Adriyanto, F.; Nurfazliana, M. F.; Bakri, A. S.

2017-01-01

Copper oxide films were grown on silicon substrates by sol-gel dip coating method. In order to study the effects of annealing temperature on the properties of copper oxide films, the temperature was varied from 200 °C to 450 °C. In the process of dip coating, the substrate is withdrawn from the precursor solution with uniform velocity to obtain a uniform coating before undergoing an annealing process to make the copper oxide film polycrystalline. The physical properties of the copper oxide films were measured by an X-ray diffraction (XRD), a field emission scanning electron microscope (FESEM), an atomic force microscopy (AFM) and a four point probe instrument. From the XRD results, we found that pure cuprite (Cu2O) phase can be obtained by annealing the films annealed at 200 °C. Films annealed at 300 °C had a combination phase which consists of tenorite (CuO) and cuprite (Cu2O) phase while pure tenorite (CuO) phase can be obtained at 450 °C annealing temperature. The surface microstructure showed that the grains size is increased whereas the surface roughness is increased and then decreases by increasing in annealing temperature. The films showed that the resistivity decreased with increasing annealing temperature. Consequently, it was observed that annealing temperature has strong effects on the structural, morphological and electrical properties of copper oxide films.

Effect of applied voltage on surface properties of anodised titanium in mixture of β-glycerophosphate (β-GP) and calcium acetate (CA)

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

Chuan, Lee Te, E-mail: gd130079@siswa.uthm.edu.my; Rathi, Muhammad Fareez Mohamad, E-mail: cd110238@siswa.uthm.edu.my; Abidin, Muhamad Yusuf Zainal, E-mail: cd110221@siswa.uthm.edu.my

Anodic oxidation is a surface modification method which combines electric field driven metal and oxygen ion diffusion for formation of oxide layer on the anode surface. This method has been widely used to modify the surface morphology of biomaterial especially titanium. This study aimed to investigate the effect of applied voltage on titanium. Specifically, the titanium foil was anodised in mixture of β-glycerophosphate disodium salt pentahydrate (β-GP) and calcium acetate monohydrate (CA) with different applied voltage (50-350 V), electrolyte concentration (0.04 M β-GP + 0.4 M CA), anodising time (10minutes) and current density (50 and 70 mA.cm{sup −2}) at room temperature. Surfacemore » oxide properties of anodised titanium were characterised by digital single-lens reflex camera (DSLR camera), field emission scanning electron microscope (FESEM) and atomic force microscopy (AFM). At lower applied voltage (≤150 V), surface of titanium foils were relatively smooth. With increasing applied voltage (≥250 V), the oxide layer became more porous and donut-shaped pores were formed on the surface of titanium foils. The AFM results indicated that the surface roughness of anodised titanium increases with increasing of applied voltage. The porous and rough surface is able to promote the osseointegration and reduce the suffering time of patient.« less

Atom chip microscopy: A novel probe for strongly correlated materials

NASA Astrophysics Data System (ADS)

Kasch, Brian; Naides, Matthew; Turner, Richard; Ray, Ushnish; Lev, Benjamin

2010-03-01

Atom chip technology---substrates supporting micron-sized current-carrying wires that create magnetic microtraps near surfaces for thermal or degenerate gases of neutral atoms---will enable single-shot, large area detection of magnetic flux below the 10-7 flux quantum level. By harnessing the extreme sensitivity of Bose-Einstein condensates (BECs) to external perturbations, cryogenic atom chips could provide a magnetic flux detection capability that surpasses all other techniques by a factor of 10^2--10^3. We describe the merits of atom chip microscopy, our Rb BEC and atom chip apparatus, and prospects for imaging strongly correlated condensed matter materials.

Nanoscopic analysis of oxygen segregation at tilt boundaries in silicon ingots using atom probe tomography combined with TEM and ab initio calculations.

PubMed

Ohno, Y; Inoue, K; Fujiwara, K; Kutsukake, K; Deura, M; Yonenaga, I; Ebisawa, N; Shimizu, Y; Inoue, K; Nagai, Y; Yoshida, H; Takeda, S; Tanaka, S; Kohyama, M

2017-12-01

We have developed an analytical method to determine the segregation levels on the same tilt boundaries (TBs) at the same nanoscopic location by a joint use of atom probe tomography and scanning transmission electron microscopy, and discussed the mechanism of oxygen segregation at TBs in silicon ingots in terms of bond distortions around the TBs. The three-dimensional distribution of oxygen atoms was determined at the typical small- and large-angle TBs by atom probe tomography with a low impurity detection limit (0.01 at.% on a TB plane) simultaneously with high spatial resolution (about 0.4 nm). The three-dimensional distribution was correlated with the atomic stress around the TBs; the stress at large-angle TBs was estimated by ab initio calculations based on atomic resolution scanning transmission electron microscopy data and that at small-angle TBs were calculated with the elastic theory based on dark-field transmission electron microscopy data. Oxygen atoms would segregate at bond-centred sites under tensile stress above about 2 GPa, so as to attain a more stable bonding network by reducing the local stress. The number of oxygen atoms segregating in a unit TB area N GB (in atoms nm -2 ) was determined to be proportional to both the number of the atomic sites under tensile stress in a unit TB area n bc and the average concentration of oxygen atoms around the TB [O i ] (in at.%) with N GB ∼ 50 n bc [O i ]. © 2017 The Authors Journal of Microscopy © 2017 Royal Microscopical Society.

Atom-Dependent Edge-Enhanced Second-Harmonic Generation on MoS2 Monolayers.

PubMed

Lin, Kuang-I; Ho, Yen-Hung; Liu, Shu-Bai; Ciou, Jian-Jhih; Huang, Bo-Ting; Chen, Christopher; Chang, Han-Ching; Tu, Chien-Liang; Chen, Chang-Hsiao

2018-02-14

Edge morphology and lattice orientation of single-crystal molybdenum disulfide (MoS 2 ) monolayers, a transition metal dichalcogenide (TMD), possessing a triangular shape with different edges grown by chemical vapor deposition are characterized by atomic force microscopy and transmission electron microscopy. Multiphoton laser scanning microscopy is utilized to study one-dimensional atomic edges of MoS 2 monolayers with localized midgap electronic states, which result in greatly enhanced optical second-harmonic generation (SHG). Microscopic S-zigzag edge and S-Mo Klein edge (bare Mo atoms protruding from a S-zigzag edge) terminations and the edge-atom dependent resonance energies can therefore be deduced based on SHG images. Theoretical calculations based on density functional theory clearly explain the lower energy of the S-zigzag edge states compared to the corresponding S-Mo Klein edge states. Characterization of the atomic-scale variation of edge-enhanced SHG is a step forward in this full-optical and high-yield technique of atomic-layer TMDs.

Measuring Roughnesses Of Optical Surfaces

NASA Technical Reports Server (NTRS)

Coulter, Daniel R.; Al-Jumaily, Gahnim A.; Raouf, Nasrat A.; Anderson, Mark S.

1994-01-01

Report discusses use of scanning tunneling microscopy and atomic force microscopy to measure roughnesses of optical surfaces. These techniques offer greater spatial resolution than other techniques. Report notes scanning tunneling microscopes and atomic force microscopes resolve down to 1 nm.

Direct observation for atomically flat and ordered vertical {111} side-surfaces on three-dimensionally figured Si(110) substrate using scanning tunneling microscopy

NASA Astrophysics Data System (ADS)

Yang, Haoyu; Hattori, Azusa N.; Ohata, Akinori; Takemoto, Shohei; Hattori, Ken; Daimon, Hiroshi; Tanaka, Hidekazu

2017-11-01

A three-dimensional Si{111} vertical side-surface structure on a Si(110) wafer was fabricated by reactive ion etching (RIE) followed by wet-etching and flash-annealing treatments. The side-surface was studied with scanning tunneling microscopy (STM) in atomic scale for the first time, in addition to atomic force microscopy (AFM), scanning electron microscopy (SEM), and low-energy electron diffraction (LEED). AFM and SEM showed flat and smooth vertical side-surfaces without scallops, and STM proved the realization of an atomically-flat 7 × 7-reconstructed structure, under optimized RIE and wet-etching conditions. STM also showed that a step-bunching occurred on the produced {111} side-surface corresponding to a reversely taped side-surface with a tilt angle of a few degrees, but did not show disordered structures. Characteristic LEED patterns from both side- and top-reconstructed surfaces were also demonstrated.

Nano Electronics on Atomically Controlled van der Waals Quantum Heterostructures

DTIC Science & Technology

2015-03-30

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

Taking Nanomedicine Teaching into Practice with Atomic Force Microscopy and Force Spectroscopy

ERIC Educational Resources Information Center

Carvalho, Filomena A.; Freitas, Teresa; Santos, Nuno C.

2015-01-01

Atomic force microscopy (AFM) is a useful and powerful tool to study molecular interactions applied to nanomedicine. The aim of the present study was to implement a hands-on atomic AFM course for graduated biosciences and medical students. The course comprises two distinct practical sessions, where students get in touch with the use of an atomic…

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

NASA Astrophysics Data System (ADS)

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

2017-04-01

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

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.

Self-standing crystalline TiO2 nanotubes/CNTs heterojunction membrane: synthesis and characterization.

PubMed

Hesabi, Zohreh R; Allam, Nageh K; Dahmen, Klaus; Garmestani, Hamid; A El-Sayed, Mostafa

2011-04-01

In the present study, we report for the first time synthesis of TiO(2) nanotubes/CNTs heterojunction membrane. Chemical vapor deposition (CVD) of CNTs at 650 °C in a mixture of H(2)/He atmosphere led to in situ detachment of the anodically fabricated TiO(2) nanotube layers from the Ti substrate underneath. Morphological and structural evolution of TiO(2) nanotubes after CNTs deposition were investigated by field- emission scanning electron microscopy (FESEM), glancing angle X-ray diffraction (GAXRD), and X-ray photoelectron spectroscopy (XPS) analyses. © 2011 American Chemical Society

A low sludge generated anode by hybrid solar electrocoagulation for the removal of lead

NASA Astrophysics Data System (ADS)

Hussin, F.; Aroua, M. K.

2017-06-01

In this work, perforated zinc is proposed as a new anode for lead removal by hybrid solar electrocoagulation. The characteristics of the sludge were investigated to understand the behaviour of lead removal during electrocoagulation. Sludge products formed were characterised using X-ray diffraction (XRD), X-ray fluorescence (XRF) and Field Emission Scanning Electron Microscopy (FESEM). In addition, the pH variation during electrocoagulation and effects on the sludge products were examined. At optimum conditions showed that the perforated zinc electrode produced better performance with high removal efficiency, low sludge volume index and less energy consumption.

Development of Thin Films as Potential Structural Cathodes to Enable Multifunctional Energy-Storage Structural Composite Batteries for the U.S. Army’s Future Force

DTIC Science & Technology

2011-09-01

glancing angle X - ray diffraction (GAXRD), atomic force microscopy (AFM), scanning electron microscopy (SEM), and electrochemical...Emission SEM FWHM full width at half maximum GAXRD glancing angle X - ray diffraction H3COCH2CH2OH 2-methoxyethanol LiMn2O4 lithium manganese oxide...were characterized by scanning electron microscopy (SEM), X - ray diffraction (XRD), and atomic force microscopy (AFM). In addition,

Preparation and characterization of novel foamed porous glass-ceramics

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

Sasmal, Nibedita; Garai, Mrinmoy; Karmakar, Basudeb, E-mail: basudebk@cgcri.res.in

2015-05-15

Foamed glass-ceramics without using foaming agent have been synthesized in a novel glass system of SrO-CaO-Al{sub 2}O{sub 3}-TiO{sub 2}-B{sub 2}O{sub 3}-SiO{sub 2}-P{sub 2}O{sub 5}-M{sub x}O{sub y} (where M = Ba, Mg, La, Ce and Ni) by a simple process of powder sintering. The glass and glass-ceramics are characterized by dilatometry, differential scanning calorimetry (DSC), heating stage microscopy (HSM), X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), optical microscopy and Fourier transformed infrared spectroscopy (FTIR). All the glasses formed are amorphous and the glass transition temperature and dilatometric softening temperature of these glasses are found to be in the rangemore » 673–678 °C and 706–728 °C respectively. The glasses are highly stable as indicated by the DSC evaluated glass stability parameters of the range 195–240 °C. Quantitative sintering study of glass powder compacts revealed swelling in the samples with NiO and CeO{sub 2} corresponding to a geometry change of 75 and 108% around 900 °C respectively. With reference to this finding the glass powder compacts are heated to 900 °C and the foamed glass-ceramics are obtained. Characteristic crystalline silicate phases have been identified in the XRD studies and their microstructures are recorded by FESEM. Optical microscope study of the foamed samples revealed formation of bigger foamed cavity with residual pores in samples with NiO and CeO{sub 2} in comparison to samples with BaO, MgO and La{sub 2}O{sub 3}. The mean pore diameters of the samples with NiO and CeO{sub 2} are determined to be 43 and 32 μm, and their respective porosities are 2.34 and 1.82 cm{sup 3}/g respectively. Thus NiO and CeO{sub 2} are found to be very effective to obtain foamed glass-ceramics without using foaming agent by the viscous flow sintering of fine glass powder compacts along with the reduction of the respective polyvalent ions. - Highlights: • Synthesis of foamed porous glass-ceramics without foaming agent by sintering method • Only powder compact yielded foamed porous glass-ceramics but bulk glass did not. • Glasses containing NiO and CeO{sub 2} exhibited significant foaming efficiency. • Bloating of entrapped gas during viscous flow sintering is the origin of foaming. • Residual void created pores in the sintered glass-ceramics as evidenced in FESEM.« less

High-resolution imaging of silicene on an Ag(111) surface by atomic force microscopy

NASA Astrophysics Data System (ADS)

Onoda, Jo; Yabuoshi, Keisuke; Miyazaki, Hiroki; Sugimoto, Yoshiaki

2017-12-01

Silicene, a two-dimensional (2D) honeycomb arrangement of Si atoms, is expected to have better electronic properties than graphene and has been mostly synthesized on Ag surfaces. Although scanning tunneling microscopy (STM) has been used for visualizing its atomic structure in real space, the interpretation of STM contrast is not straightforward and only the topmost Si atoms were observed on the (4 ×4 ) silicene/Ag(111) surface. Here, we demonstrate that high-resolution atomic force microscopy (AFM) can resolve all constituent Si atoms in the buckled honeycomb arrangement of the (4 ×4 ) silicene. Site-specific force spectroscopy attributes the origin of the high-resolution AFM images to chemical bonds between the AFM probe apex and the individual Si atoms on the (4 ×4 ) silicene. A detailed analysis of the geometric parameters suggests that the pulling up of lower-buckled Si atoms by the AFM tip could be a key for high-resolution AFM, implying a weakening of the Si-Ag interactions at the interface. We expect that high-resolution AFM will also unveil atomic structures of edges and defects of silicene, or other emerging 2D materials.

Semi-in situ atomic force microscopy imaging of intracellular neurofilaments under physiological conditions through the 'sandwich' method.

PubMed

Sato, Fumiya; Asakawa, Hitoshi; Fukuma, Takeshi; Terada, Sumio

2016-08-01

Neurofilaments are intermediate filament proteins specific for neurons and characterized by formation of biochemically stable, obligate heteropolymers in vivo While purified or reassembled neurofilaments have been subjected to morphological analyses by electron microscopy and atomic force microscopy, there has been a need for direct imaging of cytoplasmic genuine intermediate filaments with minimal risk of artefactualization. In this study, we applied the modified 'cells on glass sandwich' method to exteriorize intracellular neurofilaments, reducing the risk of causing artefacts through sample preparation. SW13vim(-) cells were double transduced with neurofilament medium polypeptide (NF-M) and alpha-internexin (α-inx). Cultured cells were covered with a cationized coverslip after prestabilization with tannic acid to form a sandwich and then split into two. After confirming that neurofilaments could be deposited on ventral plasma membranes exposed via unroofing, we performed atomic force microscopy imaging semi-in situ in aqueous solution. The observed thin filaments, considered to retain native structures of the neurofilaments, exhibited an approximate periodicity of 50-60 nm along their length. Their structural property appeared to reflect the morphology formed by their constituents, i.e. NF-M and α-inx. The success of semi-in situ atomic force microscopy of exposed bona fide assembled neurofilaments through separating the sandwich suggests that it can be an effective and alternative method for investigating cytoplasmic intermediate filaments under physiological conditions by atomic force microscopy. © The Author 2016. Published by Oxford University Press on behalf of The Japanese Society of Microscopy. All rights reserved. For permissions, please e-mail: journals.permissions@oup.com.

Rational design of aromatic surfactants for graphene/natural rubber latex nanocomposites with enhanced electrical conductivity.

PubMed

Mohamed, Azmi; Ardyani, Tretya; Abu Bakar, Suriani; Sagisaka, Masanobu; Umetsu, Yasushi; Hamon, J J; Rahim, Bazura Abdul; Esa, Siti Rahmah; Abdul Khalil, H P S; Mamat, Mohamad Hafiz; King, Stephen; Eastoe, Julian

2018-04-15

Graphene nanoplatelets (GNPs) can be dispersed in natural rubber matrices using surfactants. The stability and properties of these composites can be optimized by the choice of surfactants employed as stabilizers. Surfactants can be designed and synthesized to have enhanced compatibility with GNPs as compared to commercially available common surfactants. Including aromatic groups in the hydrophobic chain termini improves graphene compatibility of surfactants, which is expected to increase with the number of aromatic moieties per surfactant molecule. Hence, it is of interest to study the relationship between molecular structure, dispersion stability and electrical conductivity enhancement for single-, double-, and triple-chain anionic graphene-compatible surfactants. Graphene-philic surfactants, bearing two and three chains phenylated at their chain termini, were synthesized and characterized by proton nuclear magnetic resonance ( 1 H NMR) spectroscopy. These were used to formulate and stabilize dispersion of GNPs in natural rubber latex matrices, and the properties of systems comprising the new phenyl-surfactants were compared with commercially available surfactants, sodium dodecylsulfate (SDS) and sodium dodecylbenzenesulfonate (SDBS). Raman spectroscopy, field emission scanning electron microscopy (FESEM), atomic force microscopy (AFM), and high-resolution transmission electron microscopy (HRTEM) were used to study structural properties of the materials. Electrical conductivity measurements and Zeta potential measurements were used to assess the relationships between surfactant architecture and nanocomposite properties. Small-angle neutron scattering (SANS) was used to study self-assembly structure of surfactants. Of these different surfactants, the tri-chain aromatic surfactant TC3Ph3 (sodium 1,5-dioxo-1,5-bis(3-phenylpropoxy)-3-((3phenylpropoxy)carbonyl) pentane-2-sulfonate) was shown to be highly graphene-compatible (nanocomposite electrical conductivity = 2.22 × 10 -5  S cm -1 ), demonstrating enhanced electrical conductivity over nine orders of magnitude higher than neat natural rubber-latex matrix (1.51 × 10 -14  S cm -1 ). Varying the number of aromatic moieties in the surfactants appears to cause significant differences to the final properties of the nanocomposites. Copyright © 2018 Elsevier Inc. All rights reserved.

Direct Writing of Graphene-based Nanoelectronics via Atomic Force Microscopy

DTIC Science & Technology

2012-05-07

To) 07-05-2012 4. TITLE AND SUBTITLE 5a. CONTRACT NUMBER Direct Writing of Graphene -based Nanoelectronics via Atomic Force Microscopy 5b. GRANT...ABSTRACT This project employs direct writing with an atomic force microscope (AFM) to fabricate simple graphene -based electronic components like resistors...and transistors at nanometer-length scales. The goal is to explore their electrical properties for graphene -based electronics. Conducting

Incident-response monitoring technologies for aircraft cabin air quality

NASA Astrophysics Data System (ADS)

Magoha, Paul W.

Poor air quality in commercial aircraft cabins can be caused by volatile organophosphorus (OP) compounds emitted from the jet engine bleed air system during smoke/fume incidents. Tri-cresyl phosphate (TCP), a common anti-wear additive in turbine engine oils, is an important component in today's global aircraft operations. However, exposure to TCP increases risks of certain adverse health effects. This research analyzed used aircraft cabin air filters for jet engine oil contaminants and designed a jet engine bleed air simulator (BAS) to replicate smoke/fume incidents caused by pyrolysis of jet engine oil. Field emission scanning electron microscopy (FESEM) with X-ray energy dispersive spectroscopy (EDS) and neutron activation analysis (NAA) were used for elemental analysis of filters, and gas chromatography interfaced with mass spectrometry (GC/MS) was used to analyze used filters to determine TCP isomers. The filter analysis study involved 110 used and 90 incident filters. Clean air filter samples exposed to different bleed air conditions simulating cabin air contamination incidents were also analyzed by FESEM/EDS, NAA, and GC/MS. Experiments were conducted on a BAS at various bleed air conditions typical of an operating jet engine so that the effects of temperature and pressure variations on jet engine oil aerosol formation could be determined. The GC/MS analysis of both used and incident filters characterized tri- m-cresyl phosphate (TmCP) and tri-p-cresyl phosphate (TpCP) by a base peak of an m/z = 368, with corresponding retention times of 21.9 and 23.4 minutes. The hydrocarbons in jet oil were characterized in the filters by a base peak pattern of an m/z = 85, 113. Using retention times and hydrocarbon thermal conductivity peak (TCP) pattern obtained from jet engine oil standards, five out of 110 used filters tested had oil markers. Meanwhile 22 out of 77 incident filters tested positive for oil fingerprints. Probit analysis of jet engine oil aerosols obtained from BAS tests by optical particle counter (OPC) revealed lognormal distributions with the mean (range) of geometric mass mean diameter (GMMD) = 0.41 (0.39, 0.45) microm and geometric standard deviation (GSD), sigma g = 1.92 (1.87, 1.98). FESEM/EDS and NAA techniques found a wide range of elements on filters, and further investigations of used filters are recommended using these techniques. The protocols for air and filter sampling and GC/MS analysis used in this study will increase the options available for detecting jet engine oil on cabin air filters. Such criteria could support policy development for compliance with cabin air quality standards during incidents.

Antibacterial silver nanocluster/silica composite coatings on stainless steel

NASA Astrophysics Data System (ADS)

Ferraris, M.; Perero, S.; Ferraris, S.; Miola, M.; Vernè, E.; Skoglund, S.; Blomberg, E.; Odnevall Wallinder, I.

2017-02-01

A coating made of silver nanocluster/silica composites has been deposited, via a radio frequency (RF) co-sputtering technique, for the first time onto stainless steel (AISI 304L) with the aim to improve its antibacterial properties. Different thermal treatments after coating deposition have been applied in order to optimize the coating adhesion, cohesion and its antibacterial properties. Its applicability has been investigated at realistic conditions in a cheese production plant. The physico-chemical characteristics of the coatings have been analyzed by means of different bulk and surface analytical techniques. Field emission scanning electron microscopy (FESEM), X-ray Photoelectron Spectroscopy (XPS), contact angle measurements and atomic force microscopy (AFM) were employed to assess coating morphology, composition, surface roughness, wetting properties, size and local distribution of the nanoparticles within the coating. Tape tests were used to determine the adhesion/cohesion properties of the coating. The amount and time-dependence of released silver in solutions of acetic acid, artificial water, artificial tap water and artificial milk were determined by means of Atomic Absorption Spectroscopy (AAS). The antibacterial effect of the coating was evaluated at different experimental conditions using a standard bacterial strain of Staphylococcus aureus in compliance with National Committee for Clinical Laboratory Standards (NCCLS) and AATCC 147 standards. The Ahearn test was performed to measure the adhesion of bacteria to the coated stainless steel surface compared with a control surface. The antibacterial coating retained its antibacterial activity after thermal treatment up to 450 °C and after soaking in common cleaning products for stainless steel surfaces used for e.g. food applications. The antibacterial capacity of the coating remained at high levels for 1-5 days, and showed a good capacity to reduce the adhesion of bacteria up to 30 days. Only a few percent of silver in the coating was released into acetic acid, even after 10 days of exposure at 40 °C. Most silver (> 90%) remained also in the coating even after 240 h of continuous exposure. Similar observations were made after repeated exposure at 100 °C. Very low levels of released silver in solution were observed in artificial milk. No release of silver nanoparticles was observed either in synthetic tap water or in artificial milk at given conditions. The coating further displayed good antibacterial properties also when tested during working conditions in a cheese production plant.

NSTAR Extended Life Test Discharge Chamber Flake Analysis

NASA Technical Reports Server (NTRS)

deGroh, Kim K.; Banks, Bruce A.; Karniotis, Christina A.

2005-01-01

The Extended Life Test (ELT) of the NASA Solar Electric Propulsion Technology Readiness (NSTAR) ion thruster was concluded after 30,352 hours of operation. The ELT was conducted using the Deep Space 1 (DS1) back-up flight engine, a 30 cm diameter xenon ion thruster. Post-test inspection of the ELT engine revealed numerous contaminant flakes distributed over the bottom of the cylindrical section of the anode within the discharge chamber (DC). Extensive analyses were conducted to determine the source of the particles, which is critical to the understanding of degradation mechanisms of long life ion thruster operation. Analyses included: optical microscopy (OM) and particle length histograms, field emission scanning electron microscopy (FESEM) combined with energy dispersive spectroscopy (EDS), and atomic oxygen plasma exposure tests. Analyses of the particles indicate that the majority of the DC flakes consist of a layered structure, typically with either two or three layers. The flakes comprising two layers were typically found to have a molybdenum-rich (Mo-rich) layer on one side and a carbon-rich (C-rich) layer on the other side. The flakes comprising three layers were found to be sandwich-like structures with Mo-rich exterior layers and a C-rich interior layer. The presence of the C-rich layers indicates that these particles were produced by sputter deposition build-up on a surface external to the discharge chamber from ion sputter erosion of the graphite target in the test chamber. This contaminant layer became thick enough that particles spalled off, and then were electro-statically attracted into the ion thruster interior, where they were coated with Mo from internal sputter erosion of the screen grid and cathode components. Atomic oxygen tests provided evidence that the DC chamber flakes are composed of a significant fraction of carbon. Particle size histograms further indicated that the source of the particles was spalling of carbon flakes from downstream surfaces. Analyses of flakes taken from the downstream surface of the accelerator grid provided additional supportive information. The production of the downstream carbon flakes, and hence the potential problems associated with the flake particles in the ELT ion thruster engine is a facility induced effect and would not occur in the space environment.

Zr doping dependence of structural and magnetic properties of cobalt ferrite synthesized by sol-gel based Pechini method

NASA Astrophysics Data System (ADS)

Motavallian, Pourya; Abasht, Behzad; Abdollah-Pour, Hassan

2018-04-01

Nanocrystalline CoZrxFe2-xO4 (0 ≤ x ≤ 0.3 in a step of 0.05) powders were synthesized by Pechini sol-gel method. The dry gel was grinded and calcined at 700 °C in a static air atmosphere for 1 h. Some tests such as thermo gravimetric analysis (TGA) combined with differential analysis (DTA), fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM) and vibrating sample magnetometer (VSM) were carried out to investigate the thermal behaviour, structural bonds identification, crystallographic properties, morphology and magnetic properties of the obtained powders. X-ray diffraction revealed a single-phase cubic spinel structure for all samples, where the crystallite size decreases; the lattice parameter simultaneously increases with substitution of Zr. The results of FE-SEM showed that the particle size is in the 20-70 nm range. The magnetic properties such as saturation magnetization (Ms), remanent magnetization (Mr) and coercivity (Hc) were measured from the hysteresis loops. The greatest amount of saturation magnetization for CoZr0.05Fe1.95O4 sample was 67.9 emu·g-1.

Tartaric Acid as a Non-toxic and Environmentally-Friendly Anti-scaling Material for Using in Cooling Water Systems: Electrochemical and Surface Studies

NASA Astrophysics Data System (ADS)

Asghari, Elnaz; Gholizadeh-Khajeh, Maryam; Ashassi-Sorkhabi, Habib

2016-10-01

Because of the major limitations in drinking water resources, the industries need to use unprocessed water sources for their cooling systems; these water resources contain major amount of hardening cations. So, mineral scales are formed in cooling water systems during the time and cause major problems. The use of green anti-scaling materials such as carboxylic acids is considered due to their low risks of environmental pollution. In the present work, the scale inhibition performance of tartaric acid as a green organic material was evaluated. Chemical screening tests, cathodic and anodic voltammetry measurements and electrochemical impedance spectroscopy (EIS), field emission scanning electron microscopy (FESEM), energy-dispersive x-ray and x-ray diffraction, were used for the evaluation of the scale inhibition performance. The results showed that tartaric acid can prevent calcium carbonate precipitation significantly. The hard water solution with 2.0 mM of tartaric acid indicated the highest scale inhibition efficiency (ca. 68%). The voltammetry, EIS and FESEM results verified that tartaric acid can form smooth and homogeneous film on steel surface through formation of Fe(III)-tartrate complexes and retard the local precipitation of calcium carbonate deposits.

A study on the structural and mechanical properties of nanocrystalline CuS thin films grown by chemical bath deposition technique

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

Mukherjee, Nillohit; Sinha, Arijit; Khan, Gobinda Gopal

2011-01-15

We report a chemical route for the deposition of nanocrystalline thin films of CuS, using aqueous solutions of Cu(CH{sub 3}COO){sub 2}, SC(NH{sub 2}){sub 2} and N(CH{sub 2}CH{sub 2}OH){sub 3} [triethanolamine, i.e. TEA] in proper concentrations and ratios. The films were structurally characterized using X-ray diffraction technique (XRD), field emission scanning electron microscopy (FESEM) and optical analysis [both photo luminescence (PL) and ultraviolet-visible (UV-vis)]. Optical studies showed a large blue shift in the band gap energy of the films due to quantum confinement effect exerted by the nanocrystals. From both XRD and FESEM analyses, formation of CuS nanocrystals with sizes withinmore » 10-15 nm was evident. A study on the mechanical properties was carried out using nanoindentation and nanoscratch techniques, which showed good mechanical stability and high adherence of the films with the bottom substrate. Such study on the mechanical properties of the CuS thin films is being reported here for the first time. Current-voltage (I-V) measurements were also carried out for the films, which showed p-type conductivity.« less

ZnS nanostructured thin-films deposited by successive ionic layer adsorption and reaction

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

Deshmukh, S. G., E-mail: deshmukhpradyumn@gmail.com; Jariwala, Akshay; Agarwal, Anubha

ZnS thin films were grown on glass substrate using successive ionic layer adsorption and reaction (SILAR) technique at room temperature. Aqueous solutions of ZnCl{sub 2} and Na{sub 2}S were used as precursors. The X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), Raman spectroscopy and optical absorption measurements were applied to study the structural, surface morphology and optical properties of as-deposited ZnS thin films. The X-ray diffraction profiles revealed that ZnS thin films consist of crystalline grains with cubic phase. Spherical nano grains of random size and well covered on the glass substrate were observed from FESEM. The average grainmore » size were found to be 77 nm, 100 nm and 124 nm for 20 cycles, 40 cycles and 60 cycles samples respectively. For 60 cycle sample, Raman spectra show two prominent peaks at 554 cm{sup −1} and 1094 cm{sup −1}. The optical band gap values were found to be 3.76 eV, 3.72 eV and 3.67 eV for 20 cycle, 40 cycle and 60 cycle samples respectively.« less

The anti-biofouling behavior of high voltage pulse electric field (HPEF) mediated by carbon fiber composite coating in seawater.

PubMed

Feng, Tiantian; Wu, Jinyi; Chai, Ke; Yang, Pengpeng

2018-04-25

One of the most important research areas in the marine industry is to investigate new and effective anti-biofouling technologies. In this study, high voltage pulse electric field (HPEF) mediated by carbon fiber (CF) composite coating was utilized to prevent the fouling of bacteria, microalgae and barnacle larvae in seawater. The plate count, 2, 3, 5-triphenyl-tetrazolium chloride (TTC) reduction assay and neutral red (NR) staining and larval motility detection showed that the inactivation rates were at the highest levels, which reached 99.1%, 99.9%, 99.7%, 98.7% and 85% respectively for Pseudomonas sp., Vibrio sp., iron bacteria, Navicula sp. and the second stage nauplii of Balanus reticulatus, under the HPEF with 19 kV pulse amplitude, 23.15 kHz frequency and 0.5 duty cycle. The field-emission scanning electron microscopy (FE-SEM) of Navicula sp. revealed that the HPEF brought about the cell lysis and the cell organic matter release on the coating, which could be the mechanism of the inactivation by the HPEF. Additionally, the FE-SEM and Raman spectroscopy indicated that the HPEF hardly damaged the coating. Copyright © 2018 Elsevier B.V. All rights reserved.

Controlled synthesis, characterization and photoluminescence property of olive-like tetragonal α-Nd{sub 2}(MoO{sub 4}){sub 3}

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

Zhang, Youjin, E-mail: zyj@ustc.edu.cn; Zheng, Ao; Yang, Xiaozhi

2012-09-15

Highlights: ► The olive-like tetragonal α-Nd{sub 2}(MoO{sub 4}){sub 3} was gained with EDTA assisted hydrothermal method. ► The product was characterized by XRD, XPS, FTIR, FESEM, and PL. ► The possible formation mechanism for olive-like α-Nd{sub 2}(MoO{sub 4}){sub 3} was proposed. ► The PL in visible region of the olive-like α-Nd{sub 2}(MoO{sub 4}){sub 3} was studied. -- Abstract: The olive-like tetragonal α-Nd{sub 2}(MoO{sub 4}){sub 3} was obtained by a convenient and facile complex agent assisted hydrothermal method. The product was characterized by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), Fourier transform infrared (FTIR) spectroscopy, field-emission scanning electron microscopy (FESEM) andmore » photoluminescence (PL). The possible formation mechanism of the olive-like α-Nd{sub 2}(MoO{sub 4}){sub 3} was proposed. The photoluminescence property in visible region of the olive-like tetragonal α-Nd{sub 2}(MoO{sub 4}){sub 3} was studied.« less

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

NASA Astrophysics Data System (ADS)

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

2018-04-01

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

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

NASA Astrophysics Data System (ADS)

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

2018-03-01

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

Polyamidoamine dendrimers-assisted electrodeposition of gold-platinum bimetallic nanoflowers.

PubMed

Qian, Lei; Yang, Xiurong

2006-08-24

Novel Au-Pt bimetallic flower nanostructures fabricated on a polyamidoamine dendrimers-modified surface by electrodeposition are reported. These polyamidoamine dendrimers were stable, and they assisted the formation of Au-Pt bimetallic nanoflowers during the electrodeposition process. These nanoflowers were characterized by field-emitted scanning electron microscopy (FE-SEM), energy-dispersive spectroscopy (EDS), X-ray photoelectron spectroscopy (XPS), X-ray diffraction, and electrochemical methods. FE-SEM images showed that the bimetallic nanoflower included two parts: the "light" and the "pale" part. The two parts consisted of many small bimetallic nanoparticles, which was attributed to the progressive nucleation process. Moreover, the "light" part contained more bimetallic nanoparticles. The morphologies of bimetallic nanoflowers depended on the electrodeposition time and potential and the layer number of assembled dendrimers. The average size of nanoflowers increased with the increase in electrodeposition time. The layer number of assembled dendrimers obviously affected the size and morphologies of the "pale" parts of deposited nanoflowers. EDS and XPS indicated that the content of Au element was higher than that of Pt element in the nanoflowers. The bimetallic nanoflowers-modified electrode had electrochemical properties similar to those of bare gold and platinum electrodes. It also exhibited significant electrocatalytic activities toward oxygen reduction.

Copper diffusion in Ti Si N layers formed by inductively coupled plasma implantation

NASA Astrophysics Data System (ADS)

Ee, Y. C.; Chen, Z.; Law, S. B.; Xu, S.; Yakovlev, N. L.; Lai, M. Y.

2006-11-01

Ternary Ti-Si-N refractory barrier films of 15 nm thick was prepared by low frequency, high density, inductively coupled plasma implantation of N into TixSiy substrate. This leads to the formation of Ti-N and Si-N compounds in the ternary film. Diffusion of copper in the barrier layer after annealing treatment at various temperatures was investigated using time-of-flight secondary ion mass spectrometer (ToF-SIMS) depth profiling, X-ray diffractometer (XRD), field emission scanning electron microscopy (FESEM), energy dispersive X-ray (EDX) and sheet resistance measurement. The current study found that barrier failure did not occur until 650 °C annealing for 30 min. The failure occurs by the diffusion of copper into the Ti-Si-N film to form Cu-Ti and Cu-N compounds. FESEM surface morphology and EDX show that copper compounds were formed on the ridge areas of the Ti-Si-N film. The sheet resistance verifies the diffusion of Cu into the Ti-Si-N film; there is a sudden drop in the resistance with Cu compound formation. This finding provides a simple and effective method of monitoring Cu diffusion in TiN-based diffusion barriers.

Effects of argon addition on a-CNx film deposition by hot carbon filament chemical vapor deposition

NASA Astrophysics Data System (ADS)

Watanabe, Yoshihisa; Aono, Masami; Yamazaki, Ayumi; Kitazawa, Nobuaki; Nakamura, Yoshikazu

2002-07-01

Using a carbon filament which supplies carbon and heat, amorphous carbon nitride (a-CNx) films were prepared on Si (100) substrates by hot filament chemical vapor deposition. Deposition was performed in a low-pressure atmosphere of pure nitrogen and a gas mixture of nitrogen and argon. Effects of argon additions to the nitrogen atmosphere on the film microstructure and interface composition between the film and substrate were studied by field-emission scanning electron microscopy (FESEM) and x-ray photoelectron spectroscopy (XPS). FESEM observations reveal that the film prepared in a pure nitrogen atmosphere has uniform nucleation and a densely packed columnar pieces structure. The film prepared in the nitrogen and argon gas mixture exhibits preferential nucleation and a tapered structure with macroscopic voids. Depth analyses using XPS reveal that the film prepared in pure nitrogen possesses a broad interface, which includes silicon carbide as well as a-CNx, whereas a sharp interface is discerned in the film prepared in the mixed nitrogen and argon gas. We observed that silicon carbide formation is suppressed by an argon addition to the nitrogen atmosphere during deposition. copyright 2002 American Vacuum Society.

Effect of particle morphology of Ni on the mechanical behavior of AZ91E-Ni coated nano Al2O3 composites

NASA Astrophysics Data System (ADS)

Sameer Kumar, D.; Suman, K. N. S.; Poddar, Palash

2017-06-01

The properties of any composite always depend on the bonding between the matrix and reinforcement phases. One way of improving the wettability of reinforcement in a matrix is to apply a layer of coating on reinforcing particles. The present study aims at developing Ni coating on nano Al2O3 ceramic particles and dispersing them in AZ91E magnesium matrix material. The electroless plating method has been employed to coat the particles and semi solid stir casting technique was adopted to prepare the composites. Several weight fractions of dispersed phase are considered to analyze the behavior of the fabricated composites. Field emission scanning electron microscopy (FESEM) and x-ray diffraction analysis has been carried out to investigate the distribution of particles and phase characteristics of the proposed material. The physical and mechanical behavior of the material was examined through density measurements, hardness, elastic modulus, ductility and tensile strength calculations. The metal coating on reinforcement aids to promote metal-metal bonding interface reactions which result in improved properties of the composite. Tensile fractography was carried out under FESEM and presented.

Mechanical Properties and Durability of Ultra High Strength Concrete Incorporating Multi-Walled Carbon Nanotubes

PubMed Central

Lu, Liulei; Ouyang, Dong; Xu, Weiting

2016-01-01

In this work, the effect of the addition of multi-walled carbon nanotubes (MWCNTs) on the mechanical properties and durability of ultra high strength concrete (UHSC) is reported. First, the MWCNTs were dispersed by a nano sand-mill in the presence of a surfactant in water. The UHSC specimens were prepared with various amounts of MWCNTs, ranging from 0% to 0.15% by weight of cement (bwoc). Results indicated that use of an optimal percentage of MWCNTs (0.05% bwoc) caused a 4.63% increase in compressive strength and a 24.0% decrease in chloride diffusion coefficient of UHSC at 28 days curing. Moreover, the addition of MWCNTs also improved the flexural strength and deformation ability. Furthermore, a field-emission scanning electron microscopy (FE-SEM) was used to observe the dispersion of MWCNTs in the cement matrix and morphology of the hardened cement paste containing MWCNTs. FE-SEM observation revealed that MWCNTs were well dispersed in the matrix and no agglomerate was found and the reinforcing effect of MWCNTs on UHSC was thought to be pulling out and microcrack bridging of MWCNTs, which transferred the load in tension. PMID:28773541

Mechanical Properties and Durability of Ultra High Strength Concrete Incorporating Multi-Walled Carbon Nanotubes.

PubMed

Lu, Liulei; Ouyang, Dong; Xu, Weiting

2016-05-27

In this work, the effect of the addition of multi-walled carbon nanotubes (MWCNTs) on the mechanical properties and durability of ultra high strength concrete (UHSC) is reported. First, the MWCNTs were dispersed by a nano sand-mill in the presence of a surfactant in water. The UHSC specimens were prepared with various amounts of MWCNTs, ranging from 0% to 0.15% by weight of cement (bwoc). Results indicated that use of an optimal percentage of MWCNTs (0.05% bwoc) caused a 4.63% increase in compressive strength and a 24.0% decrease in chloride diffusion coefficient of UHSC at 28 days curing. Moreover, the addition of MWCNTs also improved the flexural strength and deformation ability. Furthermore, a field-emission scanning electron microscopy (FE-SEM) was used to observe the dispersion of MWCNTs in the cement matrix and morphology of the hardened cement paste containing MWCNTs. FE-SEM observation revealed that MWCNTs were well dispersed in the matrix and no agglomerate was found and the reinforcing effect of MWCNTs on UHSC was thought to be pulling out and microcrack bridging of MWCNTs, which transferred the load in tension.

Effect of Cr doping on the structural, morphological, optical and electrical properties of indium tin oxide films

NASA Astrophysics Data System (ADS)

Mirzaee, Majid; Dolati, Abolghasem

2015-03-01

We report on the preparation and characterization of high-purity chromium (0.5-2.5 at.%)-doped indium tin oxide (ITO, In:Sn = 90:10) films deposited by sol-gel-mediated dip coating. The effects of different Cr-doping contents on structural, morphological, optical and electrical properties of the films were characterized by means of X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), field emission scanning electron microscopy (FESEM), UV-Vis spectroscopy and four-point probe methods. XRD showed high phase purity cubic In2O3 and indicated a contraction of the lattice with Cr doping. FESEM micrographs show that grain size decreased with increasing the Cr-doping content. A method to determine chromium species in the sample was developed through the decomposition of the Cr 2 p XPS spectrum in Cr6+ and Cr3+ standard spectra. Optical and electrical studies revealed that optimum opto-electronic properties, including minimum sheet resistance of 4,300 Ω/Sq and an average optical transmittance of 85 % in the visible region with a band gap of 3.421 eV, were achieved for the films doped with Cr-doping content of 2 at.%.

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

Hlaing, Nwe Ni, E-mail: nwenihlaing76@gmail.com; Department of International Development Engineering, Tokyo Institute of Technology, 2-12-1 Ookayama, Meguro-ku, Tokyo; Department of Physics, University of Yangon, 11041 Kamayut, Yangon

Recent years, CaO-based synthetic materials have been attracted attention as potential adsorbents for CO{sub 2} capture mainly due to their high CO{sub 2} adsorption capacity. In this study, micro/nanostructured aragonite CaCO{sub 3} was synthesized by a simple hydrothermal method with using polyacrylamide (PAM). The structural, morphological and thermal properties of the synthesized sample were investigated by X-ray diffraction (XRD), field-emission scanning electron microscopy (FESEM) and thermogravimetry analysis (TG-DTA). The XRD and FESEM results showed that the obtained sample was aragonite CaCO{sub 3} with aggregated nanorods and microspheres composed of nanorods. A TG-DTA apparatus with Thermoplus 2 software was used tomore » investigate the effect of carbonation temperature on the CO{sub 2} adsorption capacity of CaO derived from aragonite CaCO{sub 3} sample. At 300 °C, the sample reached the CO{sub 2} adsorption capacity of 0.098 g-CO{sub 2}/g-adsorbent, whereas the sample achieved the highest capacity of 0.682 g-CO{sub 2}/g-adsorbent at 700 °C. The results showed that the carbonation temperature significantly influenced on the CO{sub 2} adsorption capacity of the CaO derived from aragonite CaCO{sub 3}.« less

Performance assessment of MCM-48 ceramic composite membrane by separation of AlCl3 from aqueous solution.

PubMed

Kumar Basumatary, Ashim; Kumar Ghoshal, Aloke; Pugazhenthi, G

2016-12-01

Three dimensional ordered mesoporous MCM-48 membrane was fabricated on a circular shaped ceramic support by in-situ hydrothermal method. The synthesized MCM-48 powder and MCM-48 ceramic composite membrane were characterized by X-ray diffraction (XRD), thermogravimetric analysis (TGA) and field emission scanning electron microscopy (FESEM). The porosity and pore size of the composite membrane are reduced considerably by the deposition of MCM-48 on the support. The formation of MCM-48 is verified by the XRD analysis. Three stepwise mechanisms for surfactant removal are observed by TGA analysis. FESEM images clearly signify the deposition of MCM-48 on the ceramic support. The pure water flux of the support and MCM-48 composite membrane is found to be 3.63×10 -6 and 4.18×10 -8 m 3 /m 2 skPa, respectively. The above prepared MCM-48 ceramic composite membrane is employed for the removal of AlCl 3 from aqueous solution and the highest rejection of 81% is obtained at an applied pressure of 276kPa with salt concentration of 250ppm. Copyright © 2015 Elsevier Inc. All rights reserved.

Probing Membrane Order and Topography in Supported Lipid Bilayers by Combined Polarized Total Internal Reflection Fluorescence-Atomic Force Microscopy

PubMed Central

Oreopoulos, John; Yip, Christopher M.

2009-01-01

Determining the local structure, dynamics, and conformational requirements for protein-protein and protein-lipid interactions in membranes is critical to understanding biological processes ranging from signaling to the translocating and membranolytic action of antimicrobial peptides. We report here the application of a combined polarized total internal reflection fluorescence microscopy-in situ atomic force microscopy platform. This platform's ability to image membrane orientational order was demonstrated on DOPC/DSPC/cholesterol model membranes containing the fluorescent membrane probe, DiI-C20 or BODIPY-PC. Spatially resolved order parameters and fluorophore tilt angles extracted from the polarized total internal reflection fluorescence microscopy images were in good agreement with the topographical details resolved by in situ atomic force microscopy, portending use of this technique for high-resolution characterization of membrane domain structures and peptide-membrane interactions. PMID:19254557

Atomic species identification at the (101) anatase surface by simultaneous scanning tunnelling and atomic force microscopy

PubMed Central

Stetsovych, Oleksandr; Todorović, Milica; Shimizu, Tomoko K.; Moreno, César; Ryan, James William; León, Carmen Pérez; Sagisaka, Keisuke; Palomares, Emilio; Matolín, Vladimír; Fujita, Daisuke; Perez, Ruben; Custance, Oscar

2015-01-01

Anatase is a pivotal material in devices for energy-harvesting applications and catalysis. Methods for the accurate characterization of this reducible oxide at the atomic scale are critical in the exploration of outstanding properties for technological developments. Here we combine atomic force microscopy (AFM) and scanning tunnelling microscopy (STM), supported by first-principles calculations, for the simultaneous imaging and unambiguous identification of atomic species at the (101) anatase surface. We demonstrate that dynamic AFM-STM operation allows atomic resolution imaging within the material's band gap. Based on key distinguishing features extracted from calculations and experiments, we identify candidates for the most common surface defects. Our results pave the way for the understanding of surface processes, like adsorption of metal dopants and photoactive molecules, that are fundamental for the catalytic and photovoltaic applications of anatase, and demonstrate the potential of dynamic AFM-STM for the characterization of wide band gap materials. PMID:26118408

Quantification of surface displacements and electromechanical phenomena via dynamic atomic force microscopy

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

Balke, Nina; Jesse, Stephen; Yu, Pu

Detection of dynamic surface displacements associated with local changes in material strain provides access to a number of phenomena and material properties. Contact resonance-enhanced methods of atomic force microscopy (AFM) have been shown capable of detecting ~1–3 pm-level surface displacements, an approach used in techniques such as piezoresponse force microscopy, atomic force acoustic microscopy, and ultrasonic force microscopy. Here, based on an analytical model of AFM cantilever vibrations, we demonstrate a guideline to quantify surface displacements with high accuracy by taking into account the cantilever shape at the first resonant contact mode, depending on the tip–sample contact stiffness. The approachmore » has been experimentally verified and further developed for piezoresponse force microscopy (PFM) using well-defined ferroelectric materials. These results open up a way to accurate and precise measurements of surface displacement as well as piezoelectric constants at the pm-scale with nanometer spatial resolution and will allow avoiding erroneous data interpretations and measurement artifacts. Furthermore, this analysis is directly applicable to all cantilever-resonance-based scanning probe microscopy (SPM) techniques.« less

Quantification of surface displacements and electromechanical phenomena via dynamic atomic force microscopy

DOE PAGES

Balke, Nina; Jesse, Stephen; Yu, Pu; ...

2016-09-15

Detection of dynamic surface displacements associated with local changes in material strain provides access to a number of phenomena and material properties. Contact resonance-enhanced methods of atomic force microscopy (AFM) have been shown capable of detecting ~1–3 pm-level surface displacements, an approach used in techniques such as piezoresponse force microscopy, atomic force acoustic microscopy, and ultrasonic force microscopy. Here, based on an analytical model of AFM cantilever vibrations, we demonstrate a guideline to quantify surface displacements with high accuracy by taking into account the cantilever shape at the first resonant contact mode, depending on the tip–sample contact stiffness. The approachmore » has been experimentally verified and further developed for piezoresponse force microscopy (PFM) using well-defined ferroelectric materials. These results open up a way to accurate and precise measurements of surface displacement as well as piezoelectric constants at the pm-scale with nanometer spatial resolution and will allow avoiding erroneous data interpretations and measurement artifacts. Furthermore, this analysis is directly applicable to all cantilever-resonance-based scanning probe microscopy (SPM) techniques.« less

Preparation of boron doped diamond modified by iridium for electroreduction of carbon dioxide (CO2)

NASA Astrophysics Data System (ADS)

Ichzan, A. M.; Gunlazuardi, J.; Ivandini, T. A.

2017-04-01

Electroreduction of carbon dioxide (CO2) at iridium oxide-modified boron-doped diamond (IrOx-BDD) electrodes in aqueous electrolytes was studied by voltammetric method. The aim of this study was to find out the catalytic effect of IrOx to produce fine chemicals contained of two or more carbon atoms (for example acetic acid) in high percentage. Characterization using FE-SEM and XPS indicated that IrO2 can be deposited at BDD electrode, whereas characterization using cyclic voltammetry indicated that the electrode was applicable to be used as working electrode for CO2 electroreduction.

Analytical Model of the Nonlinear Dynamics of Cantilever Tip-Sample Surface Interactions for Various Acoustic-Atomic Force Microscopies

NASA Technical Reports Server (NTRS)

Cantrell, John H., Jr.; Cantrell, Sean A.

2008-01-01

A comprehensive analytical model of the interaction of the cantilever tip of the atomic force microscope (AFM) with the sample surface is developed that accounts for the nonlinearity of the tip-surface interaction force. The interaction is modeled as a nonlinear spring coupled at opposite ends to linear springs representing cantilever and sample surface oscillators. The model leads to a pair of coupled nonlinear differential equations that are solved analytically using a standard iteration procedure. Solutions are obtained for the phase and amplitude signals generated by various acoustic-atomic force microscope (A-AFM) techniques including force modulation microscopy, atomic force acoustic microscopy, ultrasonic force microscopy, heterodyne force microscopy, resonant difference-frequency atomic force ultrasonic microscopy (RDF-AFUM), and the commonly used intermittent contact mode (TappingMode) generally available on AFMs. The solutions are used to obtain a quantitative measure of image contrast resulting from variations in the Young modulus of the sample for the amplitude and phase images generated by the A-AFM techniques. Application of the model to RDF-AFUM and intermittent soft contact phase images of LaRC-cp2 polyimide polymer is discussed. The model predicts variations in the Young modulus of the material of 24 percent from the RDF-AFUM image and 18 percent from the intermittent soft contact image. Both predictions are in good agreement with the literature value of 21 percent obtained from independent, macroscopic measurements of sheet polymer material.

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

PubMed

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

2018-08-01

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

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

NASA Astrophysics Data System (ADS)

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

2018-05-01

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

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

PubMed

Wang, Jun; Zhang, Kai; Zhu, Yuejin

2005-05-01

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

Self-Assembly of a Tripodal Triszwitterion Forms a pH-Switchable Hydrogel that Can Reversibly Encapsulate Hydrophobic Guests in Water.

PubMed

Jana, Poulami; Schmuck, Carsten

2017-01-05

The development of supramolecular smart materials, which exhibit physicochemical structural changes in response to external stimuli is of current interest for various applications. Herein, we have developed the novel tripodal triszwitterion 1, derived from a C 3 -symmetric benzene-1,3,5-tricarboxamide (BTA) core, which forms a thermo-reversible and pH-switchable transparent hydrogel through intermolecular self-complementary zwitterionic interactions at a neutral pH value. The hierarchical supramolecular self-aggregation was fully analyzed by microscopy (AFM, field emission scanning electron microscopy (FESEM)), viscosity, dynamic light scattering (DLS), and rheology studies. Moreover, compound 1 enables to encapsulate hydrophobic guests, such as the dye Nile red in aqueous medium at pH 6, which makes it an interesting candidate for drug delivery and controlled release. © 2017 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

A facile hydrothermal approach to synthesize rGO/BiVO4 photocatalysts for visible light induced degradation of RhB dye

NASA Astrophysics Data System (ADS)

Pal, Shreyasi; Dutta, Shibsankar; De, Sukanta

2018-05-01

RGO/BiVO4 composites were synthesized by a simple hydrothermal method. The samples were characterized by X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM) and high-resolution transmission electron microscopy (HRTEM) and surface analysis (BET). The photocatalytic activity of the as-prepared samples was evaluated by studying the degradation of model dyes rhodamine B (RhB) under visible light. The prepared rGO/BiVO4 composites exhibited higher photocatalytic activity for the degradation of RhB with a maximum removal rate of 86% under visible light irradiation under visible-light irradiation than pure BiVO4 nanoparticles (63%). This behavior could be associated to their higher specific surface area (BET), increased light absorption intensity and the degradation of electron-hole pair recombination in BiVO4 with the introduction of the rGO.

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

NASA Astrophysics Data System (ADS)

Saberi, Maliheh; Ashkarran, Ali Akbar

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

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

NASA Astrophysics Data System (ADS)

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

2018-05-01

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

A trimodal porous carbon as an effective catalyst for hydrogen production by methane decomposition.

PubMed

Shen, Yi; Lua, Aik Chong

2016-01-15

A new type of porous carbon with an interconnected trimodal pore system is synthesized by a nanocasting method using nanoparticulated bimodal micro-mesoporous silica particles as the template. The synthesized template and carbon material are characterized using transmission electron microscopy (TEM), field emission electron scanning microscopy (FESEM) and nitrogen adsorption-desorption test. The synthesized carbon material has an extremely high surface area, a large pore volume and an interconnected pore structure, which could provide abundant active sites and space for chemical reactions and minimize the diffusion resistance of the reactants. The resulting carbon is used as the catalyst for hydrogen production by the thermal decomposition of methane. The catalytic results show that the as-synthesized carbon in this study produces much higher methane conversion and hydrogen yield than the commercial carbon materials. Copyright © 2015 Elsevier Inc. All rights reserved.

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

NASA Astrophysics Data System (ADS)

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

2008-12-01

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

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

NASA Astrophysics Data System (ADS)

Tan, De-Xin; Wang, Yan-Li

2018-03-01

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

Facile Preparation of Carbon Microcapsules Containing Phase-Change Material with Enhanced Thermal Properties

PubMed Central

Tahan Latibari, Sara; Mehrali, Mohammad; Mehrali, Mehdi; Mahlia, Teuku Meurah Indra; Metselaar, Hendrik Simon Cornelis

2014-01-01

This study describes the hydrothermal synthesis of a novel carbon/palmitic acid (PA) microencapsulated phase change material (MEPCM). The field emission scanning electron microscopy (FESEM) and high resolution transmission electron microscopy (HRTEM) images confirm that spherical capsules of uniform size were formed with a mean diameter of 6.42 μm. The melting and freezing temperature were found to be slightly lower than those of pure PA with little undercooling. The composite retained 75% of the latent heat of pure PA. Thermal stability of the MEPCM was found to be better than that of pure PA. The thermal conductivity of MEPCM was increased by as much as 41% at 30°C. Due to its good thermal properties and chemical and mechanical stability, the carbon/PA MEPCM displays a good potential for thermal energy storage systems. PMID:25054179

Formation of helical organic-inorganic hybrid silica nanotubes using a chiral anionic gelator.

PubMed

Wang, Liwen; Wang, Hairui; Li, Yi; Zhuang, Wei; Zhu, Zhaoyong; Chen, Yuanli; Li, Baozong; Yang, Yonggang

2011-03-01

Right-handed helical organic-inorganic hybrid silica nanotubes were prepared using a chiral anionic gelator with 3-aminopropyltrimethoxysilane as a co-structure-directing agent and 1,4-bis(triethoxysilyl)benzene, 4,4'-bis(triethoxysilyl)-1,1'-biphenyl, bis(triethoxysilyl)methane, 1,2-bis(triethoxysilyl)ethane, and 1,2-bis(triethoxysilyl)ethene as the precursors. The sol-gel reactions were carried out in a mixture of water and ethanol at the volume ratio of 2.2:1.8. The nanostructures were studied using field emission scanning electron microscopy (FESEM) and transmission electron microscopy (TEM). For 4,4'-biphenylene-silica nanotube, the circular dichroism spectrum indicates at least some of the biphenyl rings within the walls stack in chiral form. The TEM images taken after different reaction time reveal a cooperative mechanism. The growth of the organic self-assemblies and the adsorption of the hybrid silica oligomers occurred at the same time.

Synthesis, magnetic and ethanol gas sensing properties of semiconducting magnetite nanoparticles

NASA Astrophysics Data System (ADS)

Al-Ghamdi, Ahmed A.; Al-Hazmi, Faten; Al-Tuwirqi, R. M.; Alnowaiser, F.; Al-Hartomy, Omar A.; El-Tantawy, Farid; Yakuphanoglu, F.

2013-05-01

The superparamagnetic magnetite (Fe3O4) nanoparticles with an average size of 7 nm were synthesized using a rapid and facile microwave hydrothermal technique. The structure of the magnetite nanoparticles was characterized by X-ray diffraction (X-ray), field effect scanning electron microscopy (FESEM), energy dispersive X-ray spectroscopy (EDS), and transmission electron microscopy (TEM). The prepared Fe3O4 was shown to have a cubic phase of pure magnetite. Magnetization hysteresis loop shows that the synthesized magnetite exhibits no hysteretic features with a superparamagnetic behavior. The ethanol gas sensing properties of the synthesized magnetite were investigated, and it was found that the responsibility time is less than 10 s with good reproducibility for ethanol sensor. Accordingly, it is evaluated that the magnetite nanoparticles can be effectively used as a solid state ethanol sensor in industrial commercial product applications.

Elemental, morphological, structural, optical, and magnetic properties of erbium doped ZnO nanoparticles

NASA Astrophysics Data System (ADS)

Poornaprakash, B.; Chalapathi, U.; Purusottam Reddy, B.; Prabhakar Vattikuti, S. V.; Siva Pratap Reddy, M.; Park, Si-Hyun

2018-03-01

The sensible tuning of the structural, optical, and magnetic properties of ZnO nanoparticles (NPs) with suitable doping can enhance their applicability in diverse fields. In this study, we synthesized ZnO NPs with Er (0-4 at%) doping and their elemental, structural, optical, and magnetic properties were studied. Both field emission scanning electron microscopy (FESEM) and high resolution transmission electron microscopy (HRTEM) studies of the suspensions consist of hexagonal shaped NPs. All the prepared NPs exhibited hexagonal phase as demonstrated by powder x-ray diffraction studies. A blue shift was observed in the Er doped ZnO NPs compared to pure ZnO, indicating the increased optical bandgap. Vibrating sample magnetometer studies exhibited the pure ZnO NPs was typical diamagnetic feature whereas all the Er doped ZnO NPs were paramagnetic feature at 300 K. This is the first paramagnetic report on Er doped ZnO NPs.

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.

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

NASA Astrophysics Data System (ADS)

Hajian, Robabeh; Ehsanikhah, Amin

2018-01-01

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

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

Wu Changle; Qiao Xueliang; Luo Langli

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

Topological Structures and Membrane Nanostructures of Erythrocytes after Splenectomy in Hereditary Spherocytosis Patients via Atomic Force Microscopy.

PubMed

Li, Ying; Lu, Liyuan; Li, Juan

2016-09-01

Hereditary spherocytosis is an inherited red blood cell membrane disorder resulting from mutations of genes encoding erythrocyte membrane and cytoskeletal proteins. Few equipments can observe the structural characteristics of hereditary spherocytosis directly expect for atomic force microscopy In our study, we proved atomic force microscopy is a powerful and sensitive instrument to describe the characteristics of hereditary spherocytosis. Erythrocytes from hereditary spherocytosis patients were small spheroidal, lacking a well-organized lattice on the cell membrane, with smaller cell surface particles and had reduced valley to peak distance and average cell membrane roughness vs. those from healthy individuals. These observations indicated defects in the certain cell membrane structural proteins such as α- and β-spectrin, ankyrin, etc. Until now, splenectomy is still the most effective treatment for symptoms relief for hereditary spherocytosis. In this study, we further solved the mysteries of membrane nanostructure changes of erythrocytes before and after splenectomy in hereditary spherocytosis by atomic force microscopy. After splenectomy, the cells were larger, but still spheroidal-shaped. The membrane ultrastructure was disorganized and characterized by a reduced surface particle size and lower than normal Ra values. These observations indicated that although splenectomy can effectively relieve the symptoms of hereditary spherocytosis, it has little effect on correction of cytoskeletal membrane defects of hereditary spherocytosis. We concluded that atomic force microscopy is a powerful tool to investigate the pathophysiological mechanisms of hereditary spherocytosis and to monitor treatment efficacy in clinical practices. To the best of our knowledge, this is the first report to study hereditary spherocytosis with atomic force microscopy and offers important mechanistic insight into the underlying role of splenectomy.

Atomic force microscopy as a tool for the investigation of living cells.

PubMed

Morkvėnaitė-Vilkončienė, Inga; Ramanavičienė, Almira; Ramanavičius, Arūnas

2013-01-01

Atomic force microscopy is a valuable and useful tool for the imaging and investigation of living cells in their natural environment at high resolution. Procedures applied to living cell preparation before measurements should be adapted individually for different kinds of cells and for the desired measurement technique. Different ways of cell immobilization, such as chemical fixation on the surface, entrapment in the pores of a membrane, or growing them directly on glass cover slips or on plastic substrates, result in the distortion or appearance of artifacts in atomic force microscopy images. Cell fixation allows the multiple use of samples and storage for a prolonged period; it also increases the resolution of imaging. Different atomic force microscopy modes are used for the imaging and analysis of living cells. The contact mode is the best for cell imaging because of high resolution, but it is usually based on the following: (i) image formation at low interaction force, (ii) low scanning speed, and (iii) usage of "soft," low resolution cantilevers. The tapping mode allows a cell to behave like a very solid material, and destructive shear forces are minimized, but imaging in liquid is difficult. The force spectroscopy mode is used for measuring the mechanical properties of cells; however, obtained results strongly depend on the cell fixation method. In this paper, the application of 3 atomic force microscopy modes including (i) contact, (ii) tapping, and (iii) force spectroscopy for the investigation of cells is described. The possibilities of cell preparation for the measurements, imaging, and determination of mechanical properties of cells are provided. The applicability of atomic force microscopy to diagnostics and other biomedical purposes is discussed.

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

PubMed

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

2016-02-01

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

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

PubMed

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

2010-07-01

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

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

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

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

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

Electronegativity determination of individual surface atoms by atomic force microscopy.

PubMed

Onoda, Jo; Ondráček, Martin; Jelínek, Pavel; Sugimoto, Yoshiaki

2017-04-26

Electronegativity is a fundamental concept in chemistry. Despite its importance, the experimental determination has been limited only to ensemble-averaged techniques. Here, we report a methodology to evaluate the electronegativity of individual surface atoms by atomic force microscopy. By measuring bond energies on the surface atoms using different tips, we find characteristic linear relations between the bond energies of different chemical species. We show that the linear relation can be rationalized by Pauling's equation for polar covalent bonds. This opens the possibility to characterize the electronegativity of individual surface atoms. Moreover, we demonstrate that the method is sensitive to variation of the electronegativity of given atomic species on a surface due to different chemical environments. Our findings open up ways of analysing surface chemical reactivity at the atomic scale.

Electronegativity determination of individual surface atoms by atomic force microscopy

PubMed Central

Onoda, Jo; Ondráček, Martin; Jelínek, Pavel; Sugimoto, Yoshiaki

2017-01-01

Electronegativity is a fundamental concept in chemistry. Despite its importance, the experimental determination has been limited only to ensemble-averaged techniques. Here, we report a methodology to evaluate the electronegativity of individual surface atoms by atomic force microscopy. By measuring bond energies on the surface atoms using different tips, we find characteristic linear relations between the bond energies of different chemical species. We show that the linear relation can be rationalized by Pauling's equation for polar covalent bonds. This opens the possibility to characterize the electronegativity of individual surface atoms. Moreover, we demonstrate that the method is sensitive to variation of the electronegativity of given atomic species on a surface due to different chemical environments. Our findings open up ways of analysing surface chemical reactivity at the atomic scale. PMID:28443645

Attractive interaction between Mn atoms on the GaAs(110) surface observed by scanning tunneling microscopy.

PubMed

Taninaka, Atsushi; Yoshida, Shoji; Kanazawa, Ken; Hayaki, Eiko; Takeuchi, Osamu; Shigekawa, Hidemi

2016-06-16

Scanning tunneling microscopy/spectroscopy (STM/STS) was carried out to investigate the structures of Mn atoms deposited on a GaAs(110) surface at room temperature to directly observe the characteristics of interactions between Mn atoms in GaAs. Mn atoms were paired with a probability higher than the random distribution, indicating an attractive interaction between them. In fact, re-pairing of unpaired Mn atoms was observed during STS measurement. The pair initially had a new structure, which was transformed during STS measurement into one of those formed by atom manipulation at 4 K. Mn atoms in pairs and trimers were aligned in the <110> direction, which is theoretically predicted to produce a high Curie temperature.

Synthesis and characterization of polyaniline coated gold nanocomposites

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

Zuber, Siti Nurzulaiha Mohd; Kamarun, Dzaraini; Zaki, Hamizah

2015-08-28

Considerable attention has been drawn during the last two decades to prepare nanocomposites consists of conducting polymer and noble metal due to their potential ability to generate a new class of material with novel optical, chemical, electronic or mechanical properties for various applications. In this work, an attempt has been made to synthesize nanocomposite of polyaniline (PANI) coated with gold nanoparticles (AuNPs) chemically with various types of surfactants such as polyvinylpyrrolidone (PVP), and sodium dodecyl sulphate (SDS) which act as stabilizing agents to help in stabilization of the PANI/Gold nanocomposites system. The synthesized nanocomposites were characterized by UV-Visible, field emissionmore » scanning electron microscope (FESEM) and particle size analyzer (PSA). The formation of finger like structure can be seen in the FESEM images when the AuNPs were incorporated into the polymer matrix. The EDX data showed that 18.66% and 12.67% of AuNPs atoms were present in the composite system thus proved the incorporation of AuNPs into the polymer matrix. A small red shift of the absorption peak in the UV-Vis of both PANI/AuNPs composites system may be due to the incorporation of AuNPs in the PANI matrix.« less

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

PubMed

Kim, Myoung-Hee; Lee, Jun; Mo, Soo-Yong; Woo, Hee-Gweon; Yang, Kap Seung; Kim, Bo-Hye; Lee, Byeong-Gweon; Sohn, Honglae

2012-05-01

The one-pot synthesis and characterization of silver nanoparticle-poly(p-Br-phenylsilane) composites have been carried out. The conversion of silver(+1) salt to stable silver(0) nanoparticles is promoted by poly(p-Br-phenylsilane), Br-PPS possessing both possible reactive Si-H bonds in the polymer backbone and C-Br bonds in the substituents. The composites were characterized using XRD, TEM, FE-SEM, and solid-state UV-vis analytical techniques. TEM and FE-SEM data show the formation of the composites where large number of silver nanoparticles (less than 30 nm of size) are well dispersed throughout the Br-PPS matrix. XRD patterns are consistent with that for fcc-typed silver. The elemental analysis for Br atom and the polymer solubility confirm that the cleavage of C-Br bond and the Si-Br dative bonding were not occurred appreciably at ambient temperature. Nonetheless, TGA data suggest that some sort of cross-linking was occurred at high temperature. The size and processability of such nanoparticles depend on the ratio of metal to Br-PPS. In the absence of Br-PPS, most of the silver particles undergo macroscopic aggregation, which indicates that the polysilane is necessary for stabilizing the silver nanoparticles.

Electrical characterization of grain boundaries of CZTS thin films using conductive atomic force microscopy techniques

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

Muhunthan, N.; Singh, Om Pal; Toutam, Vijaykumar, E-mail: toutamvk@nplindia.org

2015-10-15

Graphical abstract: Experimental setup for conducting AFM (C-AFM). - Highlights: • Cu{sub 2}ZnSnS{sub 4} (CZTS) thin film was grown by reactive co-sputtering. • The electronic properties were probed using conducting atomic force microscope, scanning Kelvin probe microscopy and scanning capacitance microscopy. • C-AFM current flow mainly through grain boundaries rather than grain interiors. • SKPM indicated higher potential along the GBs compared to grain interiors. • The SCM explains that charge separation takes place at the interface of grain and grain boundary. - Abstract: Electrical characterization of grain boundaries (GB) of Cu-deficient CZTS (Copper Zinc Tin Sulfide) thin films wasmore » done using atomic force microscopic (AFM) techniques like Conductive atomic force microscopy (CAFM), Kelvin probe force microscopy (KPFM) and scanning capacitance microscopy (SCM). Absorbance spectroscopy was done for optical band gap calculations and Raman, XRD and EDS for structural and compositional characterization. Hall measurements were done for estimation of carrier mobility. CAFM and KPFM measurements showed that the currents flow mainly through grain boundaries (GB) rather than grain interiors. SCM results showed that charge separation mainly occurs at the interface of grain and grain boundaries and not all along the grain boundaries.« less

The Use of Contact Mode Atomic Force Microscopy in Aqueous Medium for Structural Analysis of Spinach Photosynthetic Complexes

DOE PAGES

Phuthong, Witchukorn; Huang, Zubin; Wittkopp, Tyler M.; ...

2015-07-28

To investigate the dynamics of photosynthetic pigment-protein complexes in vascular plants at high resolution in an aqueous environment, membrane-protruding oxygen-evolving complexes (OECs) associated with photosystem II (PSII) on spinach ( Spinacia oleracea) grana membranes were examined using contact mode atomic force microscopy. This study represents, to our knowledge, the first use of atomic force microscopy to distinguish the putative large extrinsic loop of Photosystem II CP47 reaction center protein (CP47) from the putative oxygen-evolving enhancer proteins 1, 2, and 3 (PsbO, PsbP, and PsbQ) and large extrinsic loop of Photosystem II CP43 reaction center protein (CP43) in the PSII-OEC extrinsicmore » domains of grana membranes under conditions resulting in the disordered arrangement of PSII-OEC particles. Moreover, we observed uncharacterized membrane particles that, based on their physical characteristics and electrophoretic analysis of the polypeptides associated with the grana samples, are hypothesized to be a domain of photosystem I that protrudes from the stromal face of single thylakoid bilayers. Furthermore, our results are interpreted in the context of the results of others that were obtained using cryo-electron microscopy (and single particle analysis), negative staining and freeze-fracture electron microscopy, as well as previous atomic force microscopy studies.« less

HAADF-STEM atom counting in atom probe tomography specimens: Towards quantitative correlative microscopy.

PubMed

Lefebvre, W; Hernandez-Maldonado, D; Moyon, F; Cuvilly, F; Vaudolon, C; Shinde, D; Vurpillot, F

2015-12-01

The geometry of atom probe tomography tips strongly differs from standard scanning transmission electron microscopy foils. Whereas the later are rather flat and thin (<20 nm), tips display a curved surface and a significantly larger thickness. As far as a correlative approach aims at analysing the same specimen by both techniques, it is mandatory to explore the limits and advantages imposed by the particular geometry of atom probe tomography specimens. Based on simulations (electron probe propagation and image simulations), the possibility to apply quantitative high angle annular dark field scanning transmission electron microscopy to of atom probe tomography specimens has been tested. The influence of electron probe convergence and the benefice of deconvolution of electron probe point spread function electron have been established. Atom counting in atom probe tomography specimens is for the first time reported in this present work. It is demonstrated that, based on single projections of high angle annular dark field imaging, significant quantitative information can be used as additional input for refining the data obtained by correlative analysis of the specimen in APT, therefore opening new perspectives in the field of atomic scale tomography. Copyright © 2015 Elsevier B.V. All rights reserved.

The use of atomic force microscopy to evaluate warm mix asphalt.

DOT National Transportation Integrated Search

2013-01-01

The main objective of this study was to use the Atomic Force Microscopy (AFM) to examine the moisture susceptibility : and healing characteristics of Warm Mix Asphalt (WMA) and compare it with those of conventional Hot Mix Asphalt (HMA). To : this en...

Field Ion Microscopy and Atom Probe Tomography of Metamorphic Magnetite Crystals

NASA Technical Reports Server (NTRS)

Kuhlman, K.; Martens, R. L.; Kelly, T. F.; Evans, N. D.; Miller, M. K.

2001-01-01

Magnetite has been analysed using Field Ion Microscopy (FIM) and Atom Probe Tomography (APT), highly attractive techniques for the nanoanalysis of geological materials despite the difficulties inherent in analyzing semiconducting and insulating materials. Additional information is contained in the original extended abstract.

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

PubMed

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

2015-10-01

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

Biofunctional composite coating architectures based on polycaprolactone and nanohydroxyapatite for controlled corrosion activity and enhanced biocompatibility of magnesium AZ31 alloy.

PubMed

Zomorodian, A; Garcia, M P; Moura E Silva, T; Fernandes, J C S; Fernandes, M H; Montemor, M F

2015-03-01

In this work a biofunctional composite coating architecture for controlled corrosion activity and enhanced cellular adhesion of AZ31 Mg alloys is proposed. The composite coating consists of a polycaprolactone (PCL) matrix modified with nanohydroxyapatite (HA) applied over a nanometric layer of polyetherimide (PEI). The protective properties of the coating were studied by electrochemical impedance spectroscopy (EIS), a non-disturbing technique, and the coating morphology was investigated by field emission scanning electron microscopy (FE-SEM). The results show that the composite coating protects the AZ31 substrate. The barrier properties of the coating can be optimized by changing the PCL concentration. The presence of nanohydroxyapatite particles influences the coating morphology and decreases the corrosion resistance. The biocompatibility was assessed by studying the response of osteoblastic cells on coated samples through resazurin assay, confocal laser scanning microscopy (CLSM) and scanning electron microscopy (SEM). The results show that the polycaprolactone to hydroxyapatite ratio affects the cell behavior and that the presence of hydroxyapatite induces high osteoblastic differentiation. Copyright © 2014 Elsevier B.V. All rights reserved.

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.

Metabolomic and high-throughput sequencing analysis-modern approach for the assessment of biodeterioration of materials from historic buildings.

PubMed

Gutarowska, Beata; Celikkol-Aydin, Sukriye; Bonifay, Vincent; Otlewska, Anna; Aydin, Egemen; Oldham, Athenia L; Brauer, Jonathan I; Duncan, Kathleen E; Adamiak, Justyna; Sunner, Jan A; Beech, Iwona B

2015-01-01

Preservation of cultural heritage is of paramount importance worldwide. Microbial colonization of construction materials, such as wood, brick, mortar, and stone in historic buildings can lead to severe deterioration. The aim of the present study was to give modern insight into the phylogenetic diversity and activated metabolic pathways of microbial communities colonized historic objects located in the former Auschwitz II-Birkenau concentration and extermination camp in Oświecim, Poland. For this purpose we combined molecular, microscopic and chemical methods. Selected specimens were examined using Field Emission Scanning Electron Microscopy (FESEM), metabolomic analysis and high-throughput Illumina sequencing. FESEM imaging revealed the presence of complex microbial communities comprising diatoms, fungi and bacteria, mainly cyanobacteria and actinobacteria, on sample surfaces. Microbial diversity of brick specimens appeared higher than that of the wood and was dominated by algae and cyanobacteria, while wood was mainly colonized by fungi. DNA sequences documented the presence of 15 bacterial phyla representing 99 genera including Halomonas, Halorhodospira, Salinisphaera, Salinibacterium, Rubrobacter, Streptomyces, Arthrobacter and nine fungal classes represented by 113 genera including Cladosporium, Acremonium, Alternaria, Engyodontium, Penicillium, Rhizopus, and Aureobasidium. Most of the identified sequences were characteristic of organisms implicated in deterioration of wood and brick. Metabolomic data indicated the activation of numerous metabolic pathways, including those regulating the production of primary and secondary metabolites, for example, metabolites associated with the production of antibiotics, organic acids and deterioration of organic compounds. The study demonstrated that a combination of electron microscopy imaging with metabolomic and genomic techniques allows to link the phylogenetic information and metabolic profiles of microbial communities and to shed new light on biodeterioration processes.

Metabolomic and high-throughput sequencing analysis—modern approach for the assessment of biodeterioration of materials from historic buildings

PubMed Central

Gutarowska, Beata; Celikkol-Aydin, Sukriye; Bonifay, Vincent; Otlewska, Anna; Aydin, Egemen; Oldham, Athenia L.; Brauer, Jonathan I.; Duncan, Kathleen E.; Adamiak, Justyna; Sunner, Jan A.; Beech, Iwona B.

2015-01-01

Preservation of cultural heritage is of paramount importance worldwide. Microbial colonization of construction materials, such as wood, brick, mortar, and stone in historic buildings can lead to severe deterioration. The aim of the present study was to give modern insight into the phylogenetic diversity and activated metabolic pathways of microbial communities colonized historic objects located in the former Auschwitz II–Birkenau concentration and extermination camp in Oświecim, Poland. For this purpose we combined molecular, microscopic and chemical methods. Selected specimens were examined using Field Emission Scanning Electron Microscopy (FESEM), metabolomic analysis and high-throughput Illumina sequencing. FESEM imaging revealed the presence of complex microbial communities comprising diatoms, fungi and bacteria, mainly cyanobacteria and actinobacteria, on sample surfaces. Microbial diversity of brick specimens appeared higher than that of the wood and was dominated by algae and cyanobacteria, while wood was mainly colonized by fungi. DNA sequences documented the presence of 15 bacterial phyla representing 99 genera including Halomonas, Halorhodospira, Salinisphaera, Salinibacterium, Rubrobacter, Streptomyces, Arthrobacter and nine fungal classes represented by 113 genera including Cladosporium, Acremonium, Alternaria, Engyodontium, Penicillium, Rhizopus, and Aureobasidium. Most of the identified sequences were characteristic of organisms implicated in deterioration of wood and brick. Metabolomic data indicated the activation of numerous metabolic pathways, including those regulating the production of primary and secondary metabolites, for example, metabolites associated with the production of antibiotics, organic acids and deterioration of organic compounds. The study demonstrated that a combination of electron microscopy imaging with metabolomic and genomic techniques allows to link the phylogenetic information and metabolic profiles of microbial communities and to shed new light on biodeterioration processes. PMID:26483760

Morphology and Elemental Composition of Recent and Fossil Cyanobacteria

NASA Technical Reports Server (NTRS)

SaintAmand, Ann; Hoover, Richard B.; Jerman, Gregory; Rozanov, Alexei Yu.

2005-01-01

Cyanobacteria (cyanophyta, cyanoprokaryota, and blue-green algae) are an ancient, diverse and abundant group of photosynthetic oxygenic microorganisms. Together with other bacteria and archaea, the cyanobacteria have been the dominant life forms on Earth for over 3.5 billion years. Cyanobacteria occur in some of our planets most extreme environments - hot springs and geysers, hypersaline and alkaline lakes, hot and cold deserts, and the polar ice caps. They occur in a wide variety of morphologies. Unlike archaea and other bacteria, which are typically classified in pure culture by their physiological, biochemical and phylogenetic properties, the cyanobacteria have historically been classified based upon their size and morphological characteristics. These include the presence or absence of heterocysts, sheath, uniseriate or multiseriate trichomes, true or false branching, arrangement of thylakoids, reproduction by akinetes, binary fission, hormogonia, fragmentation, presence/absence of motility etc. Their antiquity, distribution, structural and chemical differentiation, diversity, morphological complexity and large size compared to most other bacteria, makes the cyanobacteria ideal candidates for morphological biomarkers in returned Astromaterials. We have obtained optical (nomarski and phase contrast)/fluorescent (blue and green excitation) microscopy images using an Olympus BX60 compound microscope and Field Emission Scanning Electron Microscopy images and EDAX elemental compositions of living and fossil cyanobacteria. The S-4000 Hitachi Field Emission Scanning Electron Microscope (FESEM) has been used to investigate microfossils in freshly fractured interior surfaces of terrestrial rocks and the cells, hormogonia, sheaths and trichomes of recent filamentous cyanobacteria. We present Fluorescent and FESEM Secondary and Backscattered Electron images and associated EDAX elemental analyses of recent and fossil cyanobacteria, concentrating on representatives of the genera Calothnx, Leptolyngbya, Lyngbya, Planktolyngbya and Oscillatoria.

Morphology and elemental composition of recent and fossil cyanobacteria

NASA Astrophysics Data System (ADS)

St. Amand, Ann; Hoover, Richard B.; Jerman, Gregory A.; Coston, James; Rozanov, Alexei Y.

2005-09-01

Cyanobacteria (cyanophyta, cyanoprokaryota, and blue-green algae) are an ancient, diverse and abundant group of photosynthetic oxygenic microorganisms. Together with other bacteria and archaea, the cyanobacteria have been the dominant life forms on Earth for over 3.5 billion years. Cyanobacteria occur in some of our planets most extreme environments - hot springs and geysers, hypersaline and alkaline lakes, hot and cold deserts, and the polar ice caps. They occur in a wide variety of morphologies. Unlike archaea and other bacteria, which are typically classified in pure culture by their physiological, biochemical and phylogenetic properties, the cyanobacteria have historically been classified based upon their size and morphological characteristics. These include the presence or absence of heterocysts, sheath, uniseriate or multiseriate trichomes, true or false branching, arrangement of thylakoids, reproduction by akinetes, binary fission, hormogonia, fragmentation, presence/absence of motility etc. Their antiquity, distribution, structural and chemical differentiation, diversity, morphological complexity and large size compared to most other bacteria, makes the cyanobacteria ideal candidates for morphological biomarkers in returned Astromaterials. We have obtained optical (nomarski and phase contrast)/fluorescent (blue and green excitation) microscopy images using an Olympus BX60 compound microscope and Field Emission Scanning Electron Microscopy images and EDAX elemental compositions of living and fossil cyanobacteria. The S-4000 Hitachi Field Emission Scanning Electron Microscope (FESEM) has been used to investigate microfossils in freshly fractured interior surfaces of terrestrial rocks and the cells, hormogonia, sheaths and trichomes of recent filamentous cyanobacteria. We present Fluorescent and FESEM Secondary and Backscattered Electron images and associated EDAX elemental analyses of recent and fossil cyanobacteria, concentrating on representatives of the genera Calothrix, Leptolyngbya, Lyngbya, Planktolyngbya and Oscillatoria.

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

PubMed

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

2015-02-25

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

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

NASA Astrophysics Data System (ADS)

Kumar, Virender; Singh, Kulwinder; Jain, Megha; Manju; Kumar, Akshay; Sharma, Jeewan; Vij, Ankush; Thakur, Anup

2018-06-01

We have carried out a systematic study to investigate the effect of Cu doping on the optical properties of SnO2 nanostructures synthesized by chemical route. Synthesized nanostructures were characterized using X-ray diffraction (XRD), Field emission scanning electron microscopy (FE-SEM), High resolution transmission electron microscopy (HR-TEM), Energy dispersive X-ray spectroscopy, Raman spectroscopy, Fourier transform infrared (FTIR) spectroscopy, UV-visible and Photoluminescence (PL) spectroscopy. The Rietveld refinement analysis of XRD patterns of Cu-doped SnO2 samples confirmed the formation of single phase tetragonal rutile structure, however some localized distortion was observed for 5 mol% Cu-doped SnO2. Crystallite size was found to decrease with increase in dopant concentration. FE-SEM images indicated change in morphology of samples with doping. HR-TEM images revealed that synthesized nanostructures were nearly spherical and average crystallite size was in the range 12-21 nm. Structural defects, crystallinity and size effects on doping were investigated by Raman spectroscopy and results were complemented by FTIR spectroscopy. Optical band gap of samples was estimated from reflectance spectra. We have shown that band gap of SnO2 can be engineered from 3.62 to 3.82 eV by Cu doping. PL emission intensity increased as the doping concentration increased, which can be attributed to the development of defect states in the forbidden transition region of band gap of SnO2 with doping. We have also proposed a band model owing to defect states in SnO2 to explain the observed PL in Cu doped SnO2 nanostructures.

Combined use of FE-SEM+EDS, ToF-SIMS, XPS, XRD and OM for the study of ancient gilded artefacts

NASA Astrophysics Data System (ADS)

Ingo, G. M.; Riccucci, C.; Pascucci, M.; Messina, E.; Giuliani, C.; Biocca, P.; Tortora, L.; Fierro, G.; Di Carlo, G.

2018-07-01

Gilded brooches dating back to 16th-17th centuries CE were investigated by means of integrated and complementary analytical techniques such as high spatial resolution field emission scanning electron microscopy coupled with energy dispersive X-ray spectrometry (FE-SEM+EDS), time of flight secondary ion mass spectrometry (ToF-SIMS), X-ray photoelectron spectroscopy (XPS), X-ray diffraction (XRD) and optical microscopy (OM). The results reveal in detail the surface and subsurface morphology and the chemical features of the micrometric decorative Au layer that has been deposited by means of the so-called fire-gilding technique based on the use of an amalgam. Moreover, the results allow to recognise chlorine, sulphur and phosphorous species as the main degradation agents and to identify the corrosion products naturally formed during the long-term interaction with the burial soil constituents. The findings show also that the galvanic coupling between the two dissimilar metals, i.e. Cu and Au, lead to enhancement of corrosion phenomena causing the spalling of the gold thin film and the disfigurement of the object. From a conservation point of view, the results suggest a targeted use of low-toxic inhibitors to hinder the detrimental role of chlorine as possible responsible of future further severe degradation phenomena. In conclusions, the micro and nano-chemical, structural and morphological investigations in a depth range from a few nanometers to micrometers have revealed the complex nature of corroded surface of ancient gold coated artefacts, highlighting some specific aspects related to their peculiar degradation mechanisms thus extending the scientific relevance of the tailored use of complementary and integrated surface and subsurface analytical techniques for the investigation of ancient coated artefacts.

The Effects of Orthophosphate in Drinking Water on the Initial Copper Corrosion Using Atomic Force Microscopy

EPA Science Inventory

Corroding of copper piping used in household drinking water plumbing may potentially impacts consumer’s health and economics. Copper corrosion studies conducted on newly corroding material with atomic force microscopy (AFM) may be particularly useful in understanding the impact ...

Atomic Structures of Silicene Layers Grown on Ag(111): Scanning Tunneling Microscopy and Noncontact Atomic Force Microscopy Observations

PubMed Central

Resta, Andrea; Leoni, Thomas; Barth, Clemens; Ranguis, Alain; Becker, Conrad; Bruhn, Thomas; Vogt, Patrick; Le Lay, Guy

2013-01-01

Silicene, the considered equivalent of graphene for silicon, has been recently synthesized on Ag(111) surfaces. Following the tremendous success of graphene, silicene might further widen the horizon of two-dimensional materials with new allotropes artificially created. Due to stronger spin-orbit coupling, lower group symmetry and different chemistry compared to graphene, silicene presents many new interesting features. Here, we focus on very important aspects of silicene layers on Ag(111): First, we present scanning tunneling microscopy (STM) and non-contact Atomic Force Microscopy (nc-AFM) observations of the major structures of single layer and bi-layer silicene in epitaxy with Ag(111). For the (3 × 3) reconstructed first silicene layer nc-AFM represents the same lateral arrangement of silicene atoms as STM and therefore provides a timely experimental confirmation of the current picture of the atomic silicene structure. Furthermore, both nc-AFM and STM give a unifying interpretation of the second layer (√3 × √3)R ± 30° structure. Finally, we give support to the conjectured possible existence of less stable, ~2% stressed, (√7 × √7)R ± 19.1° rotated silicene domains in the first layer. PMID:23928998

Interaction between single gold atom and the graphene edge: A study via aberration-corrected transmission electron microscopy

NASA Astrophysics Data System (ADS)

Wang, Hongtao; Li, Kun; Cheng, Yingchun; Wang, Qingxiao; Yao, Yingbang; Schwingenschlögl, Udo; Zhang, Xixiang; Yang, Wei

2012-04-01

Interaction between single noble metal atoms and graphene edges has been investigated via aberration-corrected and monochromated transmission electron microscopy. A collective motion of the Au atom and the nearby carbon atoms is observed in transition between energy-favorable configurations. Most trapping and detrapping processes are assisted by the dangling carbon atoms, which are more susceptible to knock-on displacements by electron irradiation. Thermal energy is lower than the activation barriers in transition among different energy-favorable configurations, which suggests electron-beam irradiation can be an efficient way of engineering the graphene edge with metal atoms.Interaction between single noble metal atoms and graphene edges has been investigated via aberration-corrected and monochromated transmission electron microscopy. A collective motion of the Au atom and the nearby carbon atoms is observed in transition between energy-favorable configurations. Most trapping and detrapping processes are assisted by the dangling carbon atoms, which are more susceptible to knock-on displacements by electron irradiation. Thermal energy is lower than the activation barriers in transition among different energy-favorable configurations, which suggests electron-beam irradiation can be an efficient way of engineering the graphene edge with metal atoms. Electronic supplementary information (ESI) available: Additional Figures for characterization of mono-layer CVD graphene samples with free edges and Pt atoms decorations and analysis of the effect of electron irradiation; supporting movie on edge evolution. See DOI: 10.1039/c2nr00059h

Conductive Atomic Force Microscopy | Materials Science | NREL

Science.gov Websites

electrical measurement techniques is the high spatial resolution. For example, C-AFM measurements on : High-resolution image of a sample semiconductor device; the image shows white puff-like clusters on a dark background and was obtained using atomic force microscopy. Bottom: High-resolution image of the

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

NASA Astrophysics Data System (ADS)

Boyes, Edward D.; Gai, Pratibha L.

2014-02-01

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

Atomic force microscopic imaging of Acanthamoeba castellanii and Balamuthia mandrillaris trophozoites and cysts.

PubMed

Aqeel, Yousuf; Siddiqui, Ruqaiyyah; Ateeq, Muhammad; Raza Shah, Muhammad; Kulsoom, Huma; Khan, Naveed Ahmed

2015-01-01

Light microscopy and electron microscopy have been successfully used in the study of microbes, as well as free-living protists. Unlike light microscopy, which enables us to observe living organisms or the electron microscope which provides a two-dimensional image, atomic force microscopy provides a three-dimensional surface profile. Here, we observed two free-living amoebae, Acanthamoeba castellanii and Balamuthia mandrillaris under the phase contrast inverted microscope, transmission electron microscope and atomic force microscope. Although light microscopy was of lower magnification, it revealed functional biology of live amoebae such as motility and osmoregulation using contractile vacuoles of the trophozoite stage, but it is of limited value in defining the cyst stage. In contrast, transmission electron microscopy showed significantly greater magnification and resolution to reveal the ultra-structural features of trophozoites and cysts including intracellular organelles and cyst wall characteristics but it only produced a snapshot in time of a dead amoeba cell. Atomic force microscopy produced three-dimensional images providing detailed topographic description of shape and surface, phase imaging measuring boundary stiffness, and amplitude measurements including width, height and length of A. castellanii and B. mandrillaris trophozoites and cysts. These results demonstrate the importance of the application of various microscopic methods in the biological and structural characterization of the whole cell, ultra-structural features, as well as surface components and cytoskeleton of protist pathogens. © 2014 The Author(s) Journal of Eukaryotic Microbiology © 2014 International Society of Protistologists.

Magnified pseudo-elemental map of atomic column obtained by Moiré method in scanning transmission electron microscopy.

PubMed

Kondo, Yukihito; Okunishi, Eiji

2014-10-01

Moiré method in scanning transmission electron microscopy allows observing a magnified two-dimensional atomic column elemental map of a higher pixel resolution with a lower electron dose unlike conventional atomic column mapping. The magnification of the map is determined by the ratio between the pixel size and the lattice spacing. With proper ratios for the x and y directions, we could observe magnified elemental maps, homothetic to the atomic arrangement in the sample of SrTiO3 [0 0 1]. The map showed peaks at all expected oxygen sites in SrTiO3 [0 0 1]. © The Author 2014. Published by Oxford University Press on behalf of The Japanese Society of Microscopy. All rights reserved. For permissions, please e-mail: journals.permissions@oup.com.

Scanning probe microscopy in mineralogical studies: about origin of the observed roughness of natural silica-rich glasses

NASA Astrophysics Data System (ADS)

Golubev, Ye A.; Isaenko, S. I.

2017-10-01

We have studied different mineralogical objects: natural glasses of impact (tektites, impactites) and volcanic (obsidians) origin, using atomic force microscopy, X-ray microanalysis, infrared and Raman spectroscopy. The spectroscopy showed the difference in the structure and chemical composition of the glasses of different origin. The analysis of the dependence of nanoscale heterogeneity of the glasses, revealed by the atomic force microscopy, on their structural and chemical features was carried out.

Effects of Co contents on the microstructures and properties of the electrodeposited NiCo–Zr composite coatings

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

Cai, Fei; Jiang, Chuanhai, E-mail: chuanhaijiang1963@163.com; Zhao, Yuantao

2015-05-15

Highlights: • The novel NiCo–Zr coatings were prepared by electro-deposition. • Surface morphology, crystal structure, grain size and microstrain were examined. • Texture, residual stress and corrosion resistance were investigated. • Addition of Co increased the hardness and corrosion resistance of the coatings. - Abstract: In this study, the NiCo–Zr composite coatings were prepared from the electrolytes with different Co{sup 2+} concentrations by electrodeposition method. The effects of Co contents on the crystal structure, surface morphology, grain size, microstrain and residual stress were examined by X-ray diffractometer (XRD), field emission scanning electron microscopy (FESEM), Energy dispersive X-ray spectroscopy (EDX) andmore » atomic force microscope (AFM). The corrosion resistance of the composite coatings was also examined by the potentiodynamic polarization and electrochemical impedance (EIS) measurements. The results revealed that the crystal structures of the coatings were dependent on the Co contents and addition of Co content of 58 wt% resulted in the formation of hexagonal (hcp) Co. The increasing Co contents in the NiCo–Zr composite coatings resulted in the smoother and more compact surface, decreased the grain size and increased the microstrain. The micro-hardness and residual stress also increased with increasing Co contents. The addition of Co increased the corrosion resistance of the NiCo–Zr composite coatings compared with the Ni–Zr coating while the corrosion resistance of the NiCo–Zr composite coatings decreased as the Co contents increased.« less

Anchoring of Cu(II) onto surface of porous metal-organic framework through post-synthesis modification for the synthesis of benzimidazoles and benzothiazoles

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

Kardanpour, Reihaneh; Tangestaninejad, Shahram, E-mail: stanges@sci.ui.ac.ir; Mirkhani, Valiollah, E-mail: mirkhani@sci.ui.ac.ir

2016-03-15

Efficient synthesis of various benzimidazoles and benzothiazoles under mild conditions catalyzed by Cu(II) anchored onto UiO-66–NH{sub 2} metal organic framework is reported. In this manner, first, the aminated UiO-66 was modified with thiophene-2-carbaldehyde and then the prepared Schiff base was reacted with CuCl{sub 2}. The prepared catalyst was characterized by FT-IR, UV–vis, X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), N{sub 2} adsorption, inductively coupled plasma atomic emission spectroscopy (ICP-AES) and field emission scanning electron microscopy (FE-SEM). The UiO-66–NH{sub 2}–TC–Cu was applied as a highly efficient catalyst for synthesis of benzimidazole and benzothiazole derivatives by the reaction of aldehydes with 1,2-diaminobenzenemore » or 2-aminothiophenol. The Cu(II)-containing MOF was reused several times without any appreciable loss of its efficiency. - Graphical abstract: Efficient synthesis of benzimidazoles and benzothiazoles catalyzed by Cu(II) anchored onto UiO-66–NH{sub 2} metal organic framework is reported. - Highlights: • A copper Schiff base was immobilized on UiO-66 via postsynthetic modification. • The modified MOFs were fully characterized by a variety of methods. • The catalyst was used for the preparation of benzimidazoles and benzothiazoles. • In comparison of other catalysts, our catalyst was more efficient and forceful.« less

Luminescent and transparent nanopaper based on rare-earth up-converting nanoparticle grafted nanofibrillated cellulose derived from garlic skin.

PubMed

Zhao, Jingpeng; Wei, Zuwu; Feng, Xin; Miao, Miao; Sun, Lining; Cao, Shaomei; Shi, Liyi; Fang, Jianhui

2014-09-10

Highly flexible, transparent, and luminescent nanofibrillated cellulose (NFC) nanopaper with heterogeneous network, functionalized by rare-earth up-converting luminescent nanoparticles (UCNPs), was rapidly synthesized by using a moderate pressure extrusion paper-making process. NFC was successfully prepared from garlic skin using an efficient extraction approach combined with high frequency ultrasonication and high pressure homogenization after removing the noncellulosic components. An efficient epoxidation treatment was carried out to enhance the activity of the UCNPs (NaYF4:Yb,Er) with oleic acid ligand capped on the surface. The UCNPs after epoxidation then reacted with NFC in aqueous medium to form UCNP-grafted NFC nanocomposite (NFC-UCNP) suspensions at ambient temperature. Through the paper-making process, the assembled fluorescent NFC-UCNP hybrid nanopaper exhibits excellent properties, including high transparency, strong up-conversion luminescence, and good flexibility. The obtained hybrid nanopaper was characterized by transmission electron microscopy (TEM), atomic force microscope (AFM), Fourier transform infrared spectroscopy (FTIR), field emission-scanning electron microscope (FE-SEM), up-conversion luminescence (UCL) spectrum, and ultraviolet and visible (UV-vis) spectrophotometer. The experimental results demonstrate that the UCNPs have been successfully grafted to the NFC matrix with heterogeneous network. And the superiorly optical transparent and luminescent properties of the nanopaper mainly depend on the ratio of UCNPs to NFC. Of importance here is that, NFC and UCNPs afford the nanopaper a prospective candidate for multimodal anti-counterfeiting, sensors, and ion probes applications.

High temperature electrical properties study of Sr{sub 2}(Fe,Ti)O{sub 6} double perovskite materials using impedance spectroscopy method

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

Triyono, D., E-mail: djoko.triyono@sci.ui.ac.id; Laysandra, Heidi

2016-04-19

The structure, thermal, and electrical properties of double perovskite material Sr{sub 2}(Fe,Ti)O{sub 6} at high temperature have been studied. This material was synthesized by a solid state reaction method. X-ray diffraction characterization at room temperature for all samples shows a single phase and having a structure of cubic double perovskite with Pm3m space group. The variation of Fe and Ti atoms are seen in an increasing of lattice parameter and grain size which is found between 30 nm and 80 nm. The electrical properties as a function of temperature and frequency are characterized by using RLC-meter with impedance spectroscopy method. The impedancemore » data are presented in Nyquist and Bode plot resulting in the equivalent circuit and its parameters. The equivalent circuit shows the effect of grain and grain boundary in the electrical properties of materials. DC conductivity of Sr{sub 2}(Fe,Ti)O{sub 6} as a function of temperature was explained by using Arrhenius equation. The value of the activation energy which is evaluated from dc conductivity as a function of temperature shows the effect of grain and grain boundary. The activation energy exhibits of oxygen vacancy in Sr{sub 2}(Fe,Ti)O{sub 6} which is also supported by morphology of Sr{sub 2}(Fe,Ti)O{sub 6} is characterized by field emission scanning electron microscopy (FESEM).« less

Optimization of formaldehyde concentration on electroless copper deposition on alumina surface

NASA Astrophysics Data System (ADS)

Shahidin, S. A. M.; Fadil, N. A.; Yusop, M. Zamri; Tamin, M. N.; Osman, S. A.

2018-05-01

The effect of formaldehyde concentration on electroless copper plating on alumina wafer was studied. The main composition of plating bath was copper sulphate (CuSO4) as precursor and formaldehyde as a reducing agent. The copper deposition films were assessed by varying the ratio of CuSO4 and formaldehyde. The plating rate was calculated from the weight gained after plating process whilst the surface morphology was observed by field emission scanning electron microscopy (FESEM). The results show that 1:3 ratio of copper to formaldehyde is an optimum ratio to produce most uniform coating with good adhesion between copper layer and alumina wafer substrate.

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.

Investigation on structural, optical and electrical properties of polythiophene-Al2O3 composites

NASA Astrophysics Data System (ADS)

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

2018-05-01

The polythiophene (PTH) and polythiophene-Al2O3 composites prepared by in situ chemical polymerisation in the presence of anionic surfactant camphor sulfonic acid (CSA). The formation of composite is confirmed by X-ray Diffraction (XRD) and Energy Dispersive X-ray spectroscopy (EDX) analysis. The surface morphology was studied using Field Emission Electron Microscopy (FESEM). Optical properties was studied using UV-visible spectroscopy, it observed decrease in the band gap reveals material has potential application in optical devices. The dielectric constant and AC conductivity of composite have been studied for different temperature in the frequency range 1 kHz -1 MHz.

Surface morphology and improved electrical conductivity of camphorsulfonic acid surfactant based PANI nano composite

NASA Astrophysics Data System (ADS)

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

2018-05-01

Polyaniline and its composites at different wt. % of Copper oxide nano (PCC1 and PCC5) were prepared by in-situ chemical reaction method. The composites were characterized by Fourier Transform Infrared (FT-IR) Spectroscopy, Field Emission Scanning Electron Microscopy (FESEM) and the impedance measurement was carried out at different temperature. FTIR and SEM image reveals the presence of copper metal ions uniformly embedded into PANI. The dc electrical conductivity increases with increasing nano concentration in PANI and achieved high conductivity for PCC5. These results are suggesting PCC composite is a prominent candidate for supercapacitor properties and optoelectronics devices applications.

Extreme sensitivity of magnetic properties on the synthesis routes in La{sub 0.7}Sr{sub 0.3}MnO{sub 3}

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

Kumar, Ashutosh, E-mail: ashutosh.pph13@iitp.ac.in; Sharma, Himanshu; Tomy, C. V.

2016-05-06

La{sub 0.7}Sr{sub 0.3}MnO{sub 3} polycrystalline samples have been prepared using different synthesis routes. X-ray Diffraction (XRD) confirms that the samples are of single phase with R-3c space group. The surface morphology and particle size has been observed using Field Emission Scanning Electron Microscopy (FESEM). Magnetic measurement shows that the magnetization in the materials are affected by low crystallite size which destroys the spin ordering due to strain at grain boundaries and this also leads to reduction in magnetization as well as high coercivity in the material.

Characterization of Ni-P-SiO2 nano-composite coating on magnesium

NASA Astrophysics Data System (ADS)

Sadreddini, S.; Salehi, Z.; Rassaie, H.

2015-01-01

In this study, the effects of SiO2 nanoparticles added to the electroless Ni-P coating were studied. The surface morphology, corrosion behavior, hardness and porosity of Ni-P-SiO2composite were investigated. The related microstructure was investigated through field emission scanning electron microscopy (FESEM) and the amount of SiO2 was examined by Energy Dispersive Analysis of X-ray (EDX). The corrosion behavior was evaluated through electrochemical impedance spectroscopy (EIS) and polarization techniques. The results illustrated that with increasing the quantity of the SiO2 nanoparticles, the corrosion rate decreased and the hardness increased.

Effect of thermal implying during ageing process of nanorods growth on the properties of zinc oxide nanorod arrays

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

Ismail, A. S., E-mail: kyrin-samaxi@yahoo.com; Mamat, M. H., E-mail: mhmamat@salam.uitm.edu.my; Rusop, M., E-mail: rusop@salam.uitm.my

Undoped and Sn-doped Zinc oxide (ZnO) nanostructures have been fabricated using a simple sol-gel immersion method at 95°C of growth temperature. Thermal sourced by hot plate stirrer was supplied to the solution during ageing process of nanorods growth. The results showed significant decrement in the quality of layer produced after the immersion process where the conductivity and porosity of the samples reduced significantly due to the thermal appliance. The structural properties of the samples have been characterized using field emission scanning electron microscopy (FESEM) electrical properties has been characterized using current voltage (I-V) measurement.

Hydrothermal synthesis of highly crystalline ZnO nanorod arrays: Dependence of morphology and alignment on growth conditions

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

Azzez, Shrook A., E-mail: shurouq44@yahoo.com; Hassan, Z.; Alimanesh, M.

Highly oriented zinc oxide nanorod were successfully grown on seeded p-type silicon substrate by hydrothermal methode. The morphology and the crystallinty of ZnO c-axis (002) arrays were systematically studied using field emission scanning electron microscopy (FESEM) and X-ray diffraction (XRD) methods. The effect of seed layer pre-annealing on nanorods properties was explained according to the nucleation site of ZnO nanoparticles on silicon substrate. In addition, the variation of the equal molarity of zinc nitrate hexahydrate and hexamine concentrations in the reaction vessel play a crucial role related to the ZnO nanorods.

Image and compositional characteristics of the LDEF Big Guy impact crater

NASA Technical Reports Server (NTRS)

Bunch, T. E.; Paque, Julie M.; Zolensky, Michael

1995-01-01

A 5.2 mm crater in Al-metal represents the largest found on LDEF. We have examined this crater by field emission scanning electron microscopy (FESEM), energy dispersive spectroscopy (EDS) and time-of-flight/secondary ion mass spectroscopy (TOF-SIMS) in order to determine if there is any evidence of impactor residue. Droplet and dome-shaped columns, along with flow features, are evidence of melting. EDS from the crater cavity and rim show Mg, C, O and variable amounts of Si, in addition to Al. No evidence for a chondritic impactor was found, and it hypothesized that the crater may be the result of impact with space debris.

Design a sensitive optical thin film sensor based on incorporation of isonicotinohydrazide derivative in sol-gel matrix for determination of trace amounts of copper (II) in fruit juice: Effect of sonication time on immobilization approach.

PubMed

Shahamirifard, Seyed Alireza; Ghaedi, Mehrorang; Montazerozohori, Morteza

2018-04-01

A new selective and sensitive optical sensor based on the incorporation of new synthesized N'-(2-hydroxy-5-iodobenzylidene) isonicotinohydrazide (HIBIN) as an effective reagent into the nanoporous of a transparent glass like material through the sol-gel process was developed which was suitable for the determination of copper (II) ions in aqueous solutions. The thin film sensors were constructed by spin-coating of prepared sol onto glass plate and their surface morphology were studied by field emission scanning electron microscopy (FE-SEM) and atomic force microscope (AFM) technique. Influence of sonication time on immobilization of HIBIN into silica matrix was investigated through calculation of leaching percentage. The Results shown that sonication time of 35 min is suitable to give more stable thin films without fluctuation in sensitivity and response time of presented sensor for a long period of time. The proposed optical sensor can be used for determination of copper (II) ions in the range of 9.1 × 10 -8 -1.12 × 10 -5  mol L -1 with a detection limit of 1.8 × 10 -8  mol L -1 . It also showed relative standard deviation 3.4 and 0.72% for reproducibility and repeatability respectively, along with a fast response time about of 2 min. The constructed optode is stable in wet conditions and could be stored for at least 6 weeks without observing any change in its sensitivity. The developed sensor was successfully applied to the determination of copper (II) in fruit juice and water samples which results were confirmed by atomic absorption spectrometry method. Copyright © 2017 Elsevier B.V. All rights reserved.

Atomic force microscopy of atomic-scale ledges and etch pits formed during dissolution of quartz

NASA Technical Reports Server (NTRS)

Gratz, A. J.; Manne, S.; Hansma, P. K.

1991-01-01

The processes involved in the dissolution and growth of crystals are closely related. Atomic force microscopy (AFM) of faceted pits (called negative crystals) formed during quartz dissolution reveals subtle details of these underlying physical mechanisms for silicates. In imaging these surfaces, the AFM detected ledges less than 1 nm high that were spaced 10 to 90 nm apart. A dislocation pit, invisible to optical and scanning electron microscopy measurements and serving as a ledge source, was also imaged. These observations confirm the applicability of ledge-motion models to dissolution and growth of silicates; coupled with measurements of dissolution rate on facets, these methods provide a powerful tool for probing mineral surface kinetics.

Atomic force microscopy captures length phenotypes in single proteins

PubMed Central

Carrion-Vazquez, Mariano; Marszalek, Piotr E.; Oberhauser, Andres F.; Fernandez, Julio M.

1999-01-01

We use single-protein atomic force microscopy techniques to detect length phenotypes in an Ig module. To gain amino acid resolution, we amplify the mechanical features of a single module by engineering polyproteins composed of up to 12 identical repeats. We show that on mechanical unfolding, mutant polyproteins containing five extra glycine residues added to the folded core of the module extend 20 Å per module farther than the wild-type polyproteins. By contrast, similar insertions near the N or C termini have no effect. Hence, our atomic force microscopy measurements readily discriminate the location of the insert and measure its size with a resolution similar to that of NMR and x-ray crystallography. PMID:10500169

Progress in the Correlative Atomic Force Microscopy and Optical Microscopy

PubMed Central

Zhou, Lulu; Cai, Mingjun; Tong, Ti; Wang, Hongda

2017-01-01

Atomic force microscopy (AFM) has evolved from the originally morphological imaging technique to a powerful and multifunctional technique for manipulating and detecting the interactions between molecules at nanometer resolution. However, AFM cannot provide the precise information of synchronized molecular groups and has many shortcomings in the aspects of determining the mechanism of the interactions and the elaborate structure due to the limitations of the technology, itself, such as non-specificity and low imaging speed. To overcome the technical limitations, it is necessary to combine AFM with other complementary techniques, such as fluorescence microscopy. The combination of several complementary techniques in one instrument has increasingly become a vital approach to investigate the details of the interactions among molecules and molecular dynamics. In this review, we reported the principles of AFM and optical microscopy, such as confocal microscopy and single-molecule localization microscopy, and focused on the development and use of correlative AFM and optical microscopy. PMID:28441775

Surface atomic structure of alloyed Mn 5Ge 3(0 0 0 1) by scanning tunneling microscopy

NASA Astrophysics Data System (ADS)

Kim, Howon; Jung, Goo-Eun; Yoon, Jong Keon; Chung, Kyung Hoon; Kahng, Se-Jong

Surface atomic structure of Mn 5Ge 3(0 0 0 1) is studied by scanning tunneling microscopy. Hexagonal honeycomb ordering is observed at high energy levels, ∣ E - EF∣ ˜ 1.2 eV, on the flat regions of three-dimensional Mn 5Ge 3 islands. At low energy levels, ∣ E - EF∣ ˜ 0.5 eV, however, atomic images exhibit dot-array and ring-array structures, which show complete and partial contrast inversion, compared to the honeycomb ordering. Experimental observations are discussed on the basis of possible atomic models.

Direct quantitative measurement of the C═O⋅⋅⋅H–C bond by atomic force microscopy

PubMed Central

Kawai, Shigeki; Nishiuchi, Tomohiko; Kodama, Takuya; Spijker, Peter; Pawlak, Rémy; Meier, Tobias; Tracey, John; Kubo, Takashi; Meyer, Ernst; Foster, Adam S.

2017-01-01

The hydrogen atom—the smallest and most abundant atom—is of utmost importance in physics and chemistry. Although many analysis methods have been applied to its study, direct observation of hydrogen atoms in a single molecule remains largely unexplored. We use atomic force microscopy (AFM) to resolve the outermost hydrogen atoms of propellane molecules via very weak C═O⋅⋅⋅H–C hydrogen bonding just before the onset of Pauli repulsion. The direct measurement of the interaction with a hydrogen atom paves the way for the identification of three-dimensional molecules such as DNAs and polymers, building the capabilities of AFM toward quantitative probing of local chemical reactivity. PMID:28508080

Computational model for noncontact atomic force microscopy: energy dissipation of cantilever.

PubMed

Senda, Yasuhiro; Blomqvist, Janne; Nieminen, Risto M

2016-09-21

We propose a computational model for noncontact atomic force microscopy (AFM) in which the atomic force between the cantilever tip and the surface is calculated using a molecular dynamics method, and the macroscopic motion of the cantilever is modeled by an oscillating spring. The movement of atoms in the tip and surface is connected with the oscillating spring using a recently developed coupling method. In this computational model, the oscillation energy is dissipated, as observed in AFM experiments. We attribute this dissipation to the hysteresis and nonconservative properties of the interatomic force that acts between the atoms in the tip and sample surface. The dissipation rate strongly depends on the parameters used in the computational model.

Knowledge Extraction from Atomically Resolved Images.

PubMed

Vlcek, Lukas; Maksov, Artem; Pan, Minghu; Vasudevan, Rama K; Kalinin, Sergei V

2017-10-24

Tremendous strides in experimental capabilities of scanning transmission electron microscopy and scanning tunneling microscopy (STM) over the past 30 years made atomically resolved imaging routine. However, consistent integration and use of atomically resolved data with generative models is unavailable, so information on local thermodynamics and other microscopic driving forces encoded in the observed atomic configurations remains hidden. Here, we present a framework based on statistical distance minimization to consistently utilize the information available from atomic configurations obtained from an atomically resolved image and extract meaningful physical interaction parameters. We illustrate the applicability of the framework on an STM image of a FeSe x Te 1-x superconductor, with the segregation of the chalcogen atoms investigated using a nonideal interacting solid solution model. This universal method makes full use of the microscopic degrees of freedom sampled in an atomically resolved image and can be extended via Bayesian inference toward unbiased model selection with uncertainty quantification.

Molecular Rotors

DTIC Science & Technology

2006-10-31

microwave signal processing components, and micro-fluidic devices. The projected involved the preparation, surface mounting, and characterization of...Guisinger, R. Basu, and M. C. Hersam, “Atomic-level characterization and control of free radical surface chemistry using scanning tunneling microscopy...Basu, and M. C. Hersam, “Atomic level characterization and control of organosilicon surface chemistry using scanning tunneling microscopy,” presented

Characterization of novel sufraces by FTIR spectroscopy and atomic force microscopy for food pathogen detection

USDA-ARS?s Scientific Manuscript database

Single molecular detection of pathogens and toxins of interest to food safety is within grasp using technology such as Atomic Force Microscopy. Using antibodies or specific aptamers connected to the AFM tip make it possible to detect a pathogen molecule on a surface. However, it also becomes necess...

Mechanical properties of cellulose nanomaterials studied by contact resonance atomic force microscopy

Treesearch

Ryan Wagner; Robert J. Moon; Arvind Raman

2016-01-01

Quantification of the mechanical properties of cellulose nanomaterials is key to the development of new cellulose nanomaterial based products. Using contact resonance atomic force microscopy we measured and mapped the transverse elastic modulus of three types of cellulosic nanoparticles: tunicate cellulose nanocrystals, wood cellulose nanocrystals, and wood cellulose...

Topographical and Chemical Imaging of a Phase Separated Polymer Using a Combined Atomic Force Microscopy/Infrared Spectroscopy/Mass Spectrometry Platform

DOE PAGES

Tai, Tamin; Karácsony, Orsolya; Bocharova, Vera; ...

2016-02-18

This article describes how the use of a hybrid atomic force microscopy/infrared spectroscopy/mass spectrometry imaging platform was demonstrated for the acquisition and correlation of nanoscale sample surface topography and chemical images based on infrared spectroscopy and mass spectrometry.

Asymmetric-detection time-stretch optical microscopy (ATOM) for ultrafast high-contrast cellular imaging in flow

PubMed Central

Wong, Terence T. W.; Lau, Andy K. S.; Ho, Kenneth K. Y.; Tang, Matthew Y. H.; Robles, Joseph D. F.; Wei, Xiaoming; Chan, Antony C. S.; Tang, Anson H. L.; Lam, Edmund Y.; Wong, Kenneth K. Y.; Chan, Godfrey C. F.; Shum, Ho Cheung; Tsia, Kevin K.

2014-01-01

Accelerating imaging speed in optical microscopy is often realized at the expense of image contrast, image resolution, and detection sensitivity – a common predicament for advancing high-speed and high-throughput cellular imaging. We here demonstrate a new imaging approach, called asymmetric-detection time-stretch optical microscopy (ATOM), which can deliver ultrafast label-free high-contrast flow imaging with well delineated cellular morphological resolution and in-line optical image amplification to overcome the compromised imaging sensitivity at high speed. We show that ATOM can separately reveal the enhanced phase-gradient and absorption contrast in microfluidic live-cell imaging at a flow speed as high as ~10 m/s, corresponding to an imaging throughput of ~100,000 cells/sec. ATOM could thus be the enabling platform to meet the pressing need for intercalating optical microscopy in cellular assay, e.g. imaging flow cytometry – permitting high-throughput access to the morphological information of the individual cells simultaneously with a multitude of parameters obtained in the standard assay. PMID:24413677

Harnessing the damping properties of materials for high-speed atomic force microscopy.

PubMed

Adams, Jonathan D; Erickson, Blake W; Grossenbacher, Jonas; Brugger, Juergen; Nievergelt, Adrian; Fantner, Georg E

2016-02-01

The success of high-speed atomic force microscopy in imaging molecular motors, enzymes and microbes in liquid environments suggests that the technique could be of significant value in a variety of areas of nanotechnology. However, the majority of atomic force microscopy experiments are performed in air, and the tapping-mode detection speed of current high-speed cantilevers is an order of magnitude lower in air than in liquids. Traditional approaches to increasing the imaging rate of atomic force microscopy have involved reducing the size of the cantilever, but further reductions in size will require a fundamental change in the detection method of the microscope. Here, we show that high-speed imaging in air can instead be achieved by changing the cantilever material. We use cantilevers fabricated from polymers, which can mimic the high damping environment of liquids. With this approach, SU-8 polymer cantilevers are developed that have an imaging-in-air detection bandwidth that is 19 times faster than those of conventional cantilevers of similar size, resonance frequency and spring constant.

Effectiveness of Modal Decomposition for Tapping Atomic Force Microscopy Microcantilevers in Liquid Environment.

PubMed

Kim, Il Kwang; Lee, Soo Il

2016-05-01

The modal decomposition of tapping mode atomic force microscopy microcantilevers in liquid environments was studied experimentally. Microcantilevers with different lengths and stiffnesses and two sample surfaces with different elastic moduli were used in the experiment. The response modes of the microcantilevers were extracted as proper orthogonal modes through proper orthogonal decomposition. Smooth orthogonal decomposition was used to estimate the resonance frequency directly. The effects of the tapping setpoint and the elastic modulus of the sample under test were examined in terms of their multi-mode responses with proper orthogonal modes, proper orthogonal values, smooth orthogonal modes and smooth orthogonal values. Regardless of the stiffness of the microcantilever under test, the first mode was dominant in tapping mode atomic force microscopy under normal operating conditions. However, at lower tapping setpoints, the flexible microcantilever showed modal distortion and noise near the tip when tapping on a hard sample. The stiff microcantilever had a higher mode effect on a soft sample at lower tapping setpoints. Modal decomposition for tapping mode atomic force microscopy can thus be used to estimate the characteristics of samples in liquid environments.

Indigenous Carbonaceous Matter in the Nakhla Mars Meteorite

NASA Technical Reports Server (NTRS)

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

2016-01-01

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

Atomic structure of self-organizing iridium induced nanowires on Ge(001)

NASA Astrophysics Data System (ADS)

Kabanov, N. S.; Heimbuch, R.; Zandvliet, H. J. W.; Saletsky, A. M.; Klavsyuk, A. L.

2017-05-01

The atomic structure of self-organizing iridium (Ir) induced nanowires on Ge(001) is studied by density functional theory (DFT) calculations and variable-temperature scanning tunneling microscopy. The Ir induced nanowires are aligned in a direction perpendicular to the Ge(001) substrate dimer rows, have a width of two atoms and are completely kink-less. Density functional theory calculations show that the Ir atoms prefer to dive into the Ge(001) substrate and push up the neighboring Ge substrate atoms. The nanowires are composed of Ge atoms and not Ir atoms as previously assumed. The regions in the vicinity of the nanowires are very dynamic, even at temperatures as low as 77 K. Time-resolved scanning tunneling microscopy measurements reveal that this dynamics is caused by buckled Ge substrate dimers that flip back and forth between their two buckled configurations.

Dose limited reliability of quantitative annular dark field scanning transmission electron microscopy for nano-particle atom-counting.

PubMed

De Backer, A; Martinez, G T; MacArthur, K E; Jones, L; Béché, A; Nellist, P D; Van Aert, S

2015-04-01

Quantitative annular dark field scanning transmission electron microscopy (ADF STEM) has become a powerful technique to characterise nano-particles on an atomic scale. Because of their limited size and beam sensitivity, the atomic structure of such particles may become extremely challenging to determine. Therefore keeping the incoming electron dose to a minimum is important. However, this may reduce the reliability of quantitative ADF STEM which will here be demonstrated for nano-particle atom-counting. Based on experimental ADF STEM images of a real industrial catalyst, we discuss the limits for counting the number of atoms in a projected atomic column with single atom sensitivity. We diagnose these limits by combining a thorough statistical method and detailed image simulations. Copyright © 2014 Elsevier B.V. All rights reserved.

Tribological characterization of TiN coatings prepared by magnetron sputtering

NASA Astrophysics Data System (ADS)

Makwana, Nishant S.; Chauhan, Kamlesh V.; Sonera, Akshay L.; Chauhan, Dharmesh B.; Dave, Divyeshkumar P.; Rawal, Sushant K.

2018-05-01

Titanium nitride (TiN) coating deposited on aluminium and brass pin substrates using RF reactive magnetron sputtering. The structural properties and surface morphology were characterized by X-ray diffraction (XRD), atomic force microscope (AFM) and field emission scanning electron microscope (FE-SEM). There was formation of (101) Ti2N, (110) TiN2 and (102) TiN0.30 peaks at 3.5Pa, 2Pa and 1.25Pa sputtering pressure respectively. The tribological properties of coating were inspected using pin on disc tribometer equipment. It was observed that TiN coated aluminium and brass pins demonstrated improved wear resistance than uncoated aluminium and brass pins.

SERS substrate based on silver nanoparticles and graphene: Dependence on the layer number of graphene

NASA Astrophysics Data System (ADS)

Garg, Preeti; Soni, R. K.; Raman, R.

2018-05-01

In this report, we describe a low-cost fabrication process for highly sensitive SERS substrate by using thermal evaporation technique. The SERS substrate structure consists of silver nanoparticles deposited on monolayer, bilayer and few layer graphene. The fabricated SERS substrates are investigated by field emission scanning electron microscope (FE-SEM), atomic force microscope (AFM), and confocal Raman spectroscope. From the surface morphology we have verified that the fabricated SERS substrate consist of high-density of silver nanoparticles with their size distribution varies from 10 to 150 nm. The surface-enhanced Raman scattering activities of these nanostructures is highest for monolayer graphene.

Spectroscopy and atomic force microscopy of biomass.

PubMed

Tetard, L; Passian, A; Farahi, R H; Kalluri, U C; Davison, B H; Thundat, T

2010-05-01

Scanning probe microscopy has emerged as a powerful approach to a broader understanding of the molecular architecture of cell walls, which may shed light on the challenge of efficient cellulosic ethanol production. We have obtained preliminary images of both Populus and switchgrass samples using atomic force microscopy (AFM). The results show distinctive features that are shared by switchgrass and Populus. These features may be attributable to the lignocellulosic cell wall composition, as the collected images exhibit the characteristic macromolecular globule structures attributable to the lignocellulosic systems. Using both AFM and a single case of mode synthesizing atomic force microscopy (MSAFM) to characterize Populus, we obtained images that clearly show the cell wall structure. The results are of importance in providing a better understanding of the characteristic features of both mature cells as well as developing plant cells. In addition, we present spectroscopic investigation of the same samples.

Three-Dimensional Intercalated Porous Graphene on Si(111)

NASA Astrophysics Data System (ADS)

Pham, Trung T.; Sporken, Robert

2018-02-01

Three-dimensional intercalated porous graphene has been formed on Si(111) by electron beam evaporation under appropriate conditions and its structural and electronic properties investigated in detail by reflection high-energy electron diffraction, x-ray photoemission spectroscopy, Raman spectroscopy, high-resolution scanning electron microscopy, atomic force microscopy, and scanning tunneling microscopy. The results show that the crystalline quality of the porous graphene depended not only on the substrate temperature but also on the SiC layer thickness during carbon atom deposition.

Chemical bond imaging using higher eigenmodes of tuning fork sensors in atomic force microscopy

NASA Astrophysics Data System (ADS)

Ebeling, Daniel; Zhong, Qigang; Ahles, Sebastian; Chi, Lifeng; Wegner, Hermann A.; Schirmeisen, André

2017-05-01

We demonstrate the ability of resolving the chemical structure of single organic molecules using non-contact atomic force microscopy with higher normal eigenmodes of quartz tuning fork sensors. In order to achieve submolecular resolution, CO-functionalized tips at low temperatures are used. The tuning fork sensors are operated in ultrahigh vacuum in the frequency modulation mode by exciting either their first or second eigenmode. Despite the high effective spring constant of the second eigenmode (on the order of several tens of kN/m), the force sensitivity is sufficiently high to achieve atomic resolution above the organic molecules. This is observed for two different tuning fork sensors with different tip geometries (small tip vs. large tip). These results represent an important step towards resolving the chemical structure of single molecules with multifrequency atomic force microscopy techniques where two or more eigenmodes are driven simultaneously.

A review of demodulation techniques for amplitude-modulation atomic force microscopy

PubMed Central

Harcombe, David M; Ragazzon, Michael R P; Moheimani, S O Reza; Fleming, Andrew J

2017-01-01

In this review paper, traditional and novel demodulation methods applicable to amplitude-modulation atomic force microscopy are implemented on a widely used digital processing system. As a crucial bandwidth-limiting component in the z-axis feedback loop of an atomic force microscope, the purpose of the demodulator is to obtain estimates of amplitude and phase of the cantilever deflection signal in the presence of sensor noise or additional distinct frequency components. Specifically for modern multifrequency techniques, where higher harmonic and/or higher eigenmode contributions are present in the oscillation signal, the fidelity of the estimates obtained from some demodulation techniques is not guaranteed. To enable a rigorous comparison, the performance metrics tracking bandwidth, implementation complexity and sensitivity to other frequency components are experimentally evaluated for each method. Finally, the significance of an adequate demodulator bandwidth is highlighted during high-speed tapping-mode atomic force microscopy experiments in constant-height mode. PMID:28900596

Solid-state electrochemistry on the nanometer and atomic scales: the scanning probe microscopy approach

DOE PAGES

Strelcov, Evgheni; Yang, Sang Mo; Jesse, Stephen; ...

2016-04-21

Energy technologies of the 21st century require an understanding and precise control over ion transport and electrochemistry at all length scales – from single atoms to macroscopic devices. Our short review provides a summary of recent studies dedicated to methods of advanced scanning probe microscopy for probing electrochemical transformations in solids at the meso-, nano- and atomic scales. In this discussion we present the advantages and limitations of several techniques and a wealth of examples highlighting peculiarities of nanoscale electrochemistry.

Solid-state electrochemistry on the nanometer and atomic scales: the scanning probe microscopy approach

PubMed Central

Strelcov, Evgheni; Yang, Sang Mo; Jesse, Stephen; Balke, Nina; Vasudevan, Rama K.; Kalinin, Sergei V.

2016-01-01

Energy technologies of the 21st century require understanding and precise control over ion transport and electrochemistry at all length scales – from single atoms to macroscopic devices. This short review provides a summary of recent works dedicated to methods of advanced scanning probe microscopy for probing electrochemical transformations in solids at the meso-, nano- and atomic scales. Discussion presents advantages and limitations of several techniques and a wealth of examples highlighting peculiarities of nanoscale electrochemistry. PMID:27146961

Facile synthesis of graphene on dielectric surfaces using a two-temperature reactor CVD system

NASA Astrophysics Data System (ADS)

Zhang, C.; Man, B. Y.; Yang, C.; Jiang, S. Z.; Liu, M.; Chen, C. S.; Xu, S. C.; Sun, Z. C.; Gao, X. G.; Chen, X. J.

2013-10-01

Direct deposition of graphene on a dielectric substrate is demonstrated using a chemical vapor deposition system with a two-temperature reactor. The two-temperature reactor is utilized to offer sufficient, well-proportioned floating Cu atoms and to provide a temperature gradient for facile synthesis of graphene on dielectric surfaces. The evaporated Cu atoms catalyze the reaction in the presented method. C atoms and Cu atoms respectively act as the nuclei for forming graphene film in the low-temperature zone and the zones close to the high-temperature zones. A uniform and high-quality graphene film is formed in an atmosphere of sufficient and well-proportioned floating Cu atoms. Raman spectroscopy, scanning electron microscopy and atomic force microscopy confirm the presence of uniform and high-quality graphene.

Swelling and tribological properties of melt-mixed fluoroelastomer/nitrile rubber blends under crude oil

NASA Astrophysics Data System (ADS)

Tagelsir, Yasin; Li, San-Xi; Lv, Xiaoren; Wang, Shijie; Wang, Song; Osman, Zeinab

2018-01-01

The melt-mixed fluoroelastomer (FKM)/ nitrile rubber (NBR) blends of (90/10, 80/20, 70/30, 60/40 and 50/50) ratios with same hardness were prepared, and their swelling and tribological properties under crude oil were investigated for the purpose of developing high performance cost-effective elastomers meeting requirement of oil extraction progressive cavity pump stator. Differential scanning calorimetry confirmed compatible blend system for all blends. Field emission scanning electron microscopy (FE-SEM) showed co-continuous morphology of 200-400 nm phase size for all blends, expect FKM/NBR (90/10) which exhibited partially continuous phase morphology of 100-250 nm phase size. The results of swelling and linear wear tests under crude oil indicated that swelling percentage, coefficient of friction and specific wear rate of FKM/NBR blends were much better than NBR, with FKM/NBR (90/10 and 80/20) showing swelling percentage and specific wear rate very close to FKM. Attenuated total reflectance-Fourier transform infrared spectroscopy disclosed that fracture of macromolecular chains was the main mechanochemical effect of unswollen and swollen worn surfaces, in addition to oxygenated degradation detected with increasing NBR ratio in the blends. The fracture of macromolecular chains resulted in slight fatigue wear mechanism, which was also confirmed by FE-SEM of the worn surfaces.

Synthesis of Hierarchical Self-Assembled CuO and Their Structure-Enhanced Photocatalytic Performance

NASA Astrophysics Data System (ADS)

Wang, Dagui; Yan, Bing; Song, Caixiong; Ye, Ting; Wang, Yongqian

2018-01-01

Hierarchical self-assembled CuO hollow microspheres with superior photocatalytic performance are synthesized via a simple hydrothermal process in the presence of cationic surfactants (cetyltrimethylammonium bromide, CTAB). The structure, morphology, and optical absorption performance of CuO samples prepared with different surfactants including CTAB, nonionic surfactant (polyvinylpyrrolidone, PVP) and anionic surfactant (sodium dodecyl sulfate, SDS) are characterized by x-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), ultraviolet-visible (UV-vis) absorption spectra. Moreover, the photocatalytic performances of the CuO samples are evaluated by the photo-degradation of a simulative contaminant methylene blue. The XRD patterns and FESEM images demonstrate that the category of surfactants have effects on the phase structure and morphology of CuO. Compared with bulk CuO (1.20 eV at room temperature), the band gap of CuO microspheres prepared with different surfactants including CTAB, PVP and SDS are measured at 2.16 eV, 2.29 eV, 2.44 eV, respectively, which exhibits a blue shift in the UV-vis spectra. The synthesized hierarchical self-assembled CuO hollow microspheres reveal commendable photocatalytic activity, in which the photo-degradation rate could rise to 94.1%. Additionally, a reasonable growth mechanism of CuO microspheres synthesized with different surfactants is discussed in detail.

The effect of microstructure on the sheared edge quality and hole expansion ratio of hot-rolled 700 MPa steel

NASA Astrophysics Data System (ADS)

Kaijalainen, A.; Kesti, V.; Vierelä, R.; Ylitolva, M.; Porter, D.; Kömi, J.

2017-09-01

The effects of microstructure on the cutting and hole expansion properties of three thermomechanically rolled steels have been investigated. The yield strength of the studied 3 mm thick strip steels was approximately 700 MPa. Detailed microstructural studies using laser scanning confocal microscopy (LCSM), FESEM and FESEM-EBSD revealed that the three investigated materials consist of 1) single-phase polygonal ferrite, 2) polygonal ferrite with precipitates and 3) granular bainite. The quality of mechanically sheared edges were evaluated using visual inspection and LSCM, while hole expansion properties were characterised according to the methods described in ISO 16630. Roughness values (Ra and Rz) of the sheet edge with different cutting clearances varied between 12 µm to 21 µm and 133 µm to 225 µm, respectively. Mean hole expansion ratios varied from 28.4% to 40.5%. It was shown that granular bainite produced the finest cutting edge, but the hole expansion ratio remained at the same level as in the steel comprising single-phase ferrite. This indicates that a single-phase ferritic matrix enhances hole expansion properties even with low quality edges. A brief discussion of the microstructural features controlling the cutting quality and hole expansion properties is given.

Novel anode catalyst for direct methanol fuel cells.

PubMed

Basri, S; Kamarudin, S K; Daud, W R W; Yaakob, Z; Kadhum, A A H

2014-01-01

PtRu catalyst is a promising anodic catalyst for direct methanol fuel cells (DMFCs) but the slow reaction kinetics reduce the performance of DMFCs. Therefore, this study attempts to improve the performance of PtRu catalysts by adding nickel (Ni) and iron (Fe). Multiwalled carbon nanotubes (MWCNTs) are used to increase the active area of the catalyst and to improve the catalyst performance. Electrochemical analysis techniques, such as energy dispersive X-ray spectrometry (EDX), X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), and X-ray photoelectron spectroscopy (XPS), are used to characterize the kinetic parameters of the hybrid catalyst. Cyclic voltammetry (CV) is used to investigate the effects of adding Fe and Ni to the catalyst on the reaction kinetics. Additionally, chronoamperometry (CA) tests were conducted to study the long-term performance of the catalyst for catalyzing the methanol oxidation reaction (MOR). The binding energies of the reactants and products are compared to determine the kinetics and potential surface energy for methanol oxidation. The FESEM analysis results indicate that well-dispersed nanoscale (2-5 nm) PtRu particles are formed on the MWCNTs. Finally, PtRuFeNi/MWCNT improves the reaction kinetics of anode catalysts for DMFCs and obtains a mass current of 31 A g(-1) catalyst.

Novel Anode Catalyst for Direct Methanol Fuel Cells

PubMed Central

Basri, S.; Kamarudin, S. K.; Daud, W. R. W.; Yaakob, Z.; Kadhum, A. A. H.

2014-01-01

PtRu catalyst is a promising anodic catalyst for direct methanol fuel cells (DMFCs) but the slow reaction kinetics reduce the performance of DMFCs. Therefore, this study attempts to improve the performance of PtRu catalysts by adding nickel (Ni) and iron (Fe). Multiwalled carbon nanotubes (MWCNTs) are used to increase the active area of the catalyst and to improve the catalyst performance. Electrochemical analysis techniques, such as energy dispersive X-ray spectrometry (EDX), X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), and X-ray photoelectron spectroscopy (XPS), are used to characterize the kinetic parameters of the hybrid catalyst. Cyclic voltammetry (CV) is used to investigate the effects of adding Fe and Ni to the catalyst on the reaction kinetics. Additionally, chronoamperometry (CA) tests were conducted to study the long-term performance of the catalyst for catalyzing the methanol oxidation reaction (MOR). The binding energies of the reactants and products are compared to determine the kinetics and potential surface energy for methanol oxidation. The FESEM analysis results indicate that well-dispersed nanoscale (2–5 nm) PtRu particles are formed on the MWCNTs. Finally, PtRuFeNi/MWCNT improves the reaction kinetics of anode catalysts for DMFCs and obtains a mass current of 31 A g−1 catalyst. PMID:24883406

Synthesis and Characterization of Yttria-Stabilized Zirconia Nanoparticles Doped with Ytterbium and Gadolinium: ZrO2 9.5Y2O3 5.6Yb2O3 5.2Gd2O3

NASA Astrophysics Data System (ADS)

Bahamirian, M.; Hadavi, S. M. M.; Rahimipour, M. R.; Farvizi, M.; Keyvani, A.

2018-06-01

Defect cluster thermal barrier coatings (TBCs) are attractive alternatives to Yttria-stabilized zirconia (YSZ) in advanced applications. In this study, YSZ nanoparticles doped with ytterbium and gadolinium (ZrO2 9.5Y2O3 5.6Yb2O3 5.2Gd2O3 (ZGYbY)) were synthesized through a chemical co-precipitation and calcination method, and characterized by in situ high-temperature X-ray diffraction analysis in the temperature range of 25 °C to 1000 °C (HTK-XRD), thermogravimetric analysis, differential thermal analysis, Fourier transform infrared spectroscopy, Raman spectroscopy, and field emission scanning electron microscopy (FE-SEM). Precise cell parameters of t-prime phase and the best zirconia phase for TBC applications were calculated by Cohen's and Rietveld refinement methods. Optimum crystallization temperature of the precursor powder was found to be 1000 °C. Furthermore, FE-SEM results for the calcined ZGYbY powders indicated orderly particles of uniform shape and size with a small tendency toward agglomeration. Average lattice thermal expansion coefficient in the temperature range of 25 °C to 1000 °C was determined to be 31.71 × 10-6 K-1.

Effects of multiwall carbon nanotubes on viscoelastic properties of magnetorheological elastomers

NASA Astrophysics Data System (ADS)

Aziz, Siti Aishah Abdul; Amri Mazlan, Saiful; Intan Nik Ismail, Nik; Ubaidillah, U.; Choi, Seung-Bok; Khairi, Muntaz Hana Ahmad; Azhani Yunus, Nurul

2016-07-01

The effect of different types of multiwall carbon nanotubes (MWCNTs) on the morphological, magnetic and viscoelastic properties of magnetorheological elastomers (MREs) are studied in this work. A series of natural rubber MRE are prepared by adding MWCNTs as a new additive in MRE. Effects of functionalized MWCNT namely carboxylated MWCNT (COOH-MWCNT) and hydroxylated MWCNT (OH-MWCNT) on the rheological properties of MREs are investigated and the pristine MWCNTs is referred as a control. Epoxidised palm oil (EPO) is used as a medium to disperse carbonyl iron particle (CIP) and sonicate the MWCNTs. Morphological and magnetic properties of MREs are characterized by field emission scanning electron microscopy (FESEM) and vibrating sample magnetometer (VSM), respectively. Rheological properties under different magnetic field are evaluated by using parallel plate rheometer. From the results obtained, FESEM images indicate that COOH-MWCNT and CIP have better compatibility which leads to the formation of interconnected network in the matrix. In addition, by adding functionalized COOH-MWCNT, it is shown that the saturation magnetization is 5% higher than the pristine MWCNTs. It is also found that with the addition of COOH-MWCNT, the magnetic properties are improved parallel with enhancement of MR effect particularly at low strain amplitude. It is finally shown that the use of EPO also can contribute to the enhancement of MR performance.

Mechanical, thermal and morphological characterisation of 3D porous Pennisetum purpureum/PLA biocomposites scaffold.

PubMed

Revati, R; Abdul Majid, M S; Ridzuan, M J M; Normahira, M; Mohd Nasir, N F; Rahman Y, M N; Gibson, A G

2017-06-01

The mechanical, thermal, and morphological properties of a 3D porous Pennisetum purpureum (PP)/polylactic acid (PLA) based scaffold were investigated. In this study, a scaffold containing P. purpureum and PLA was produced using the solvent casting and particulate leaching method. P. purpureum fibre, also locally known as Napier grass, is composed of 46% cellulose, 34% hemicellulose, and 20% lignin. PLA composites with various P. purpureum contents (10%, 20%, and 30%) were prepared and subsequently characterised. The morphologies, structures and thermal behaviours of the prepared composite scaffolds were characterised using field-emission scanning electron microscopy (FESEM), Fourier transform infrared spectroscopy (FTIR), and thermogravimetric analysis (TGA). The morphology was studied using FESEM; the scaffold possessed 70-200μm-sized pores with a high level of interconnectivity. The moisture content and mechanical properties of the developed porous scaffolds were further characterised. The P. purpureum/PLA scaffold had a greater porosity factor (99%) and compression modulus (5.25MPa) than those of the pure PLA scaffold (1.73MPa). From the results, it can be concluded that the properties of the highly porous P. purpureum/PLA scaffold developed in this study can be controlled and optimised. This can be used to facilitate the construction of implantable tissue-engineered cartilage. Copyright © 2017 Elsevier B.V. All rights reserved.

Synthesis and Characterization of Yttria-Stabilized Zirconia Nanoparticles Doped with Ytterbium and Gadolinium: ZrO2 9.5Y2O3 5.6Yb2O3 5.2Gd2O3

NASA Astrophysics Data System (ADS)

Bahamirian, M.; Hadavi, S. M. M.; Rahimipour, M. R.; Farvizi, M.; Keyvani, A.

2018-03-01

Defect cluster thermal barrier coatings (TBCs) are attractive alternatives to Yttria-stabilized zirconia (YSZ) in advanced applications. In this study, YSZ nanoparticles doped with ytterbium and gadolinium (ZrO2 9.5Y2O3 5.6Yb2O3 5.2Gd2O3 (ZGYbY)) were synthesized through a chemical co-precipitation and calcination method, and characterized by in situ high-temperature X-ray diffraction analysis in the temperature range of 25 °C to 1000 °C (HTK-XRD), thermogravimetric analysis, differential thermal analysis, Fourier transform infrared spectroscopy, Raman spectroscopy, and field emission scanning electron microscopy (FE-SEM). Precise cell parameters of t-prime phase and the best zirconia phase for TBC applications were calculated by Cohen's and Rietveld refinement methods. Optimum crystallization temperature of the precursor powder was found to be 1000 °C. Furthermore, FE-SEM results for the calcined ZGYbY powders indicated orderly particles of uniform shape and size with a small tendency toward agglomeration. Average lattice thermal expansion coefficient in the temperature range of 25 °C to 1000 °C was determined to be 31.71 × 10-6 K-1.

Effect of Temperature and Growth Time on Vertically Aligned ZnO Nanorods by Simplified Hydrothermal Technique for Photoelectrochemical Cells.

PubMed

Mohd Fudzi, Laimy; Zainal, Zulkarnain; Lim, Hong Ngee; Chang, Sook-Keng; Holi, Araa Mebdir; Sarif Mohd Ali, Mahanim

2018-04-29

Despite its large band gap, ZnO has wide applicability in many fields ranging from gas sensors to solar cells. ZnO was chosen over other materials because of its large exciton binding energy (60 meV) and its stability to high-energy radiation. In this study, ZnO nanorods were deposited on ITO glass via a simple dip coating followed by a hydrothermal growth. The morphological, structural and compositional characteristics of the prepared films were analyzed using X-ray diffractometry (XRD), field emission scanning electron microscopy (FESEM), and ultraviolet-visible spectroscopy (UV-Vis). Photoelectrochemical conversion efficiencies were evaluated via photocurrent measurements under calibrated halogen lamp illumination. Thin film prepared at 120 °C for 4 h of hydrothermal treatment possessed a hexagonal wurtzite structure with the crystallite size of 19.2 nm. The average diameter of the ZnO nanorods was 37.7 nm and the thickness was found to be 2680.2 nm. According to FESEM images, as the hydrothermal growth temperature increases, the nanorod diameter become smaller. Moreover, the thickness of the nanorods increase with the growth time. Therefore, the sample prepared at 120 °C for 4 h displayed an impressive photoresponse by achieving high current density of 0.1944 mA/cm².

Improving anti-felting characteristics of Merino wool fiber by 2.5 MHz atmosphere pressure air plasma

NASA Astrophysics Data System (ADS)

Chandwani, Nisha; Dave, Purvi; Jain, Vishal; Nema, Sudhir; Mukherjee, Subroto

2017-04-01

The present work investigates the effect of high frequency (2.5 MHz) Dielectric Barrier Discharge (DBD) in air on surface characteristics of Merino wool as a function of plasma exposure time (5s to 15s). The FE-SEM (Field Emission Scanning Electron Microscopy), EDS (Energy Dispersive X-ray spectrum) and Derivative ATR-FTIR (Attenuated Total Reflection- Fourier Transform Infrared) Spectroscopy are used to study physio-chemical changes induced by plasma. These physio-chemical properties of fibers can be co-related with the felting behaviour of the wool fiber, which leads to shrinkage and pilling of garments while laundering. Felting occurs mainly because of presence of outermost hydrophobic cuticle layer having sharp scales. The FE-SEM analysis of wool fiber surface reveals that cuticle scales on wool fiber become blunt after plasma processing. The ATR-FTIR analysis along with second order derivative spectroscopy demonstrates the cleavage of di-sulphide bonds of cuticle and formation of sulphur-oxygen groups such as Cystine Sulphonate (-S-SO3-), cysteic acid (-SO3-), cystine monoxide(-SO-S-), cysteine di-oxide (-SO2-S-). A possible explanation about how the combined effect of morphological and chemical changes induced by plasma results in minimizing the felting of wool fibers is discussed.

Sol gel synthesis and characterization studies of Cupromanganite CaCu3Mn4O12

NASA Astrophysics Data System (ADS)

Nurulhuda, A.; Warikh, A. R. M.; Hafizzal, Y.

2017-08-01

A single-phase CaCu3Mn4O12 electroceramic had been prepared via sol gel method and fairly well densified at relative low temperature under atmospheric condition where the crystallization of CaCu3Mn4O12 occurred due to amorphous polymeric mixture. The precursor was prepared by mixing the solutions with 0.6 M citric acid (C6H8O7) as a chelating reagent with the mol ratio 1:2. The precursor gel formed was calcined and sintered at range 400 °C to 800°C by varying dwell time. Material formations under the reported conditions have been confirmed by X-ray diffraction (XRD). The results show that the formation of CaCu3Mn4O12 started at 500 ° C and was formed completely at 700 ° C for 18 hours. The microstructure of all CaCu3Mn4O12 was analysed using field emission scanning electron microscopy (FESEM). A smaller particle size with higher grain boundary was obtained at sintering 700°C to 800°C. FESEM results show the significant influence of calcinations and sintering parameter on the microstructure behaviour of CaCu2Mn4O12.

Ultrasound-assisted fabrication of nanoporous CdS films.

PubMed

Singh, R S; Sanagapalli, S; Jayaraman, V; Singh, V P

2004-01-01

A new method for fabricating nanoporous CdS films is reported. It involves exposing the CdS solution with ultrasound waves during the process of dip coating. Indium tin oxide (ITO)-coated glass and plastic (commercial transparency) were used as substrates. In each case three different precursors were used for dip coating. The precursors used were CdCl2 and thiourea in one case and CdS nanoparticles prepared by sonochemical and microwave-assisted methods in the other two cases. X-ray diffraction studies performed on these powders show a phase corresponding to cubic CdS. The Field Emission Scanning Electron Microscopy (FE-SEM) images of the films on plastic showed uniform pores with a diameter of 80 nm for all three methods. Optical absorption measurements indicated a blue shift and multiple peaks in the absorption curve. The FE-SEM observations of the films on an ITO/glass substrate indicated a crystalline film with voids. The UV-vis absorption results indicated a blue shift in the absorption with an absorption edge at 435, 380, and 365 nm for CdS films made by solution growth, sonochemical, and microwave routes, respectively. The magnitude of the absorption is dependent on film thickness, and the observed blue shift in the absorption can be explained on the basis of quantum confinement effects.

Effects of swift heavy ion irradiation on structural, optical and photocatalytic properties of ZnO–CuO nanocomposites prepared by carbothermal evaporation method

PubMed Central

Kuriakose, Sini; Avasthi, D K

2015-01-01

Summary ZnO–CuO nanocomposite thin films were prepared by carbothermal evaporation of ZnO and Cu, combined with annealing. The effects of 90 MeV Ni7+ ion irradiation on the structural and optical properties of ZnO–CuO nanocomposites were studied by using X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), UV–visible absorption spectroscopy and Raman spectroscopy. XRD studies showed the presence of ZnO and CuO nanostructures in the nanocomposites. FESEM images revealed the presence of nanosheets and nanorods in the nanocomposites. The photocatalytic activity of ZnO–CuO nanocomposites was evaluated on the basis of degradation of methylene blue (MB) and methyl orange (MO) dyes under sun light irradiation and it was observed that swift heavy ion irradiation results in significant enhancement in the photocatalytic efficiency of ZnO–CuO nanocomposites towards degradation of MB and MO dyes. The possible mechanism for the enhanced photocatalytic activity of ZnO–CuO nanocomposites is proposed. We attribute the observed enhanced photocatalytic activity of ZnO–CuO nanocomposites to the combined effects of improved sun light utilization and suppression of the recombination of photogenerated charge carriers in ZnO–CuO nanocomposites. PMID:25977864

Co-precipitation synthesis of nano-composites consists of zinc and tin oxides coatings on glass with enhanced photocatalytic activity on degradation of Reactive Blue 160 KE2B.

PubMed

Habibi, Mohammad Hossein; Mardani, Maryam

2015-02-25

Nano-composite containing zinc oxide-tin oxide was obtained by a facile co-precipitation route using tin chloride tetrahydrate and zinc chloride as precursors and coated on glass by Doctor Blade deposition. The crystalline structure and morphology of composites were evaluated by X-ray diffraction (XRD) and field emission scanning electron microscopy (FESEM). The XRD results showed peaks relative to zinc oxide with hexagonal wurtzite structure and tin oxide with tetragonal structure. FESEM observations showed that the nano-composite consisted of aggregates of particles with an average particle size of 18 nm. The photocatalytic activity of the pure SnO2, pure ZnO, ZnSnO3-Zn2SnO4 and ZnO-SnO2 nano-structure thin films was examined using the degradation of a textile dye Reactive Blue 160 (KE2B). ZnO-SnO2 nano-composite showed enhanced photo-catalytic activity than the pure zinc oxide and tin oxide. The enhanced photo-catalytic activity of the nano-composite was ascribed to an improved charge separation of the photo-generated electron-hole pairs. Copyright © 2014 Elsevier B.V. All rights reserved.

A study on photoelectrochemical properties of ZnO@ZnS nanostructures synthesized via facile ion-exchange approach

NASA Astrophysics Data System (ADS)

Sharma, Akash; Sahoo, Pooja; Thangavel, R.

2018-05-01

In this work, ZnO nanorods (NRs) were fabricated, on cleaned ITO substrates by using sol-gel spin coating followed by hydrothermal technique. In order to coat zinc sulphide (ZnS) layers on the earlier prepared NRs a facile ion-exchange approach was adopted. The ZnO@ZnS nanostructures so prepared were characterised by using X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), UV-visible spectroscopy and photoelectrochemical study. XRD spectra confirmed the hexagonal wurtzite structure of all the samples along with preferential c-axis orientation. Further it was also observed from the FESEM images that sulfidation process doesn't affect the structure of ZnO NRs arrays. From the absorption spectra it can be clearly observed that the light absorbing property has increased in within the visible range due to the formation of ZnS layer on the ZnO nanostructures, which is not possible for either of the material individually. The cyclic voltammetry results indicates the enhancement in photocurrent density after illumination for the synthesized nanostructures. The electrocatalytic behaviour of ZnO@ZnS electrodes have been studied using a 3-electrode system in presence of 0.1M NaOH electrolyte solution with respect to an Ag/AgCl reference electrode.

Growth of Au nanoparticle films and the effect of nanoparticle shape on plasmon peak wavelength

NASA Astrophysics Data System (ADS)

Horikoshi, S.; Matsumoto, N.; Omata, Y.; Kato, T.

2014-05-01

Metal nanoparticles (NPs) exhibit localized surface plasmon resonance (LSPR) and thus have potential for use in a wide range of applications. A facile technique for the preparation of NP films using an electron-cyclotron-resonance plasma sputtering method without a dewetting process is described. Field emission scanning electron microscopy (FE-SEM) observations revealed that the Au NPs grew independently as island-like particles during the first stage of sputtering and then coalesced with one another as sputtering time increased to ultimately form a continuous film. A plasmon absorption peak was observed via optical measurement of absorption efficiency. The LSPR peak shifted toward longer wavelengths (red shift) with an increase in sputtering time. The cause of this plasmon peak shift was theoretically investigated using the finite-difference time-domain calculation method. A realistic statistical distribution of the particle shapes based on FE-SEM observations was applied for the analysis, which has not been previously reported. It was determined that the change in the shape of the NPs from spheroidal to oval or slender due to coalescence with neighbouring NPs caused the LSPR peak shift. These results may enable the design of LSPR devices by controlling the characteristics of the nanoparticles, such as their size, shape, number density, and coverage.

Laboratory Exercise for Studying the Morphology of Heat-Denatured and Amyloid Aggregates of Lysozyme by Atomic Force Microscopy

ERIC Educational Resources Information Center

Gokalp, Sumeyra; Horton, William; Jónsdóttir-Lewis, Elfa B.; Foster, Michelle; Török, Marianna

2018-01-01

To facilitate learning advanced instrumental techniques, essential tools for visualizing biomaterials, a simple and versatile laboratory exercise demonstrating the use of Atomic Force Microscopy (AFM) in biomedical applications was developed. In this experiment, the morphology of heat-denatured and amyloid-type aggregates formed from a low-cost…

Surface conformations of anti-ricin aptamer and its affinity to ricin determined by atomic force microscopy and surface plasmon resonance

USDA-ARS?s Scientific Manuscript database

The specific interactions between ricin and anti-ricin aptamer were measured with atomic force microscopy (AFM) and surface plasmon resonance (SPR) spectrometry and the results were compared. In AFM, a single-molecule experiment with ricin functionalized AFM tip was used for scanning the aptamer mol...

Single-molecule force spectroscopy: optical tweezers, magnetic tweezers and atomic force microscopy

PubMed Central

Neuman, Keir C.; Nagy, Attila

2012-01-01

Single-molecule force spectroscopy has emerged as a powerful tool to investigate the forces and motions associated with biological molecules and enzymatic activity. The most common force spectroscopy techniques are optical tweezers, magnetic tweezers and atomic force microscopy. These techniques are described and illustrated with examples highlighting current capabilities and limitations. PMID:18511917

Nanoscale Probing of Electrical Signals in Biological Systems

DTIC Science & Technology

2012-03-18

Membranes Anodized aluminum oxide ( AAO ) is an ideal prototype substrate for studying ion transport through nanoporous membranes . For optimal...electrochemical microscopy, scanning ion conductance microscopy, nanoporous membranes , anodized aluminum oxide , atomic layer deposition, focused ion beam...capacity. This approach utilizes atomic layer deposition (ALD) of a thin conformal Ir film into a nanoporous anodized aluminum oxide (

Atomic force microscopy of torus-bearing pit membranes

Treesearch

Roland R. Dute; Thomas Elder

2011-01-01

Atomic force microscopy was used to compare the structures of dried, torus-bearing pit membranes from four woody species, three angiosperms and one gymnosperm. Tori of Osmanthus armatus are bipartite consisting of a pustular zone overlying parallel sets of microfibrils that form a peripheral corona. Microfibrils of the corona form radial spokes as they traverse the...

Convergent Inquiry in Science & Engineering: The Use of Atomic Force Microscopy in a Biology Class

ERIC Educational Resources Information Center

Lee, Il-Sun; Byeon, Jung-Ho; Kwon, Yong-Ju

2013-01-01

The purpose of this study was to design a teaching method suitable for science high school students using atomic force microscopy. During their scientific inquiry procedure, high school students observed a micro-nanostructure of a biological sample, which is unobservable via an optical microscope. The developed teaching method enhanced students'…

Scanning electron and atomic force microscopy, and raman and x-ray photoelectron spectroscopy characterization of near-isogenic soft and hard wheat kernels and corresponding flours

USDA-ARS?s Scientific Manuscript database

Atomic force microscopy (AFM), Raman spectroscopy and X-ray photoelectron spectroscopy (XPS) are used to investigate vitreous (hard) and non-vitreous (soft) wheat kernels and their corresponding wheat flours. AFM data reveal two different microstructures. The vitreous kernel reveals a granular text...

Methods and apparatus of spatially resolved electroluminescence of operating organic light-emitting diodes using conductive atomic force microscopy

NASA Technical Reports Server (NTRS)

Hersam, Mark C. (Inventor); Pingree, Liam S. C. (Inventor)

2008-01-01

A conductive atomic force microscopy (cAFM) technique which can concurrently monitor topography, charge transport, and electroluminescence with nanometer spatial resolution. This cAFM approach is particularly well suited for probing the electroluminescent response characteristics of operating organic light-emitting diodes (OLEDs) over short length scales.

Detection of percolating paths in polyhedral segregated network composites using electrostatic force microscopy and conductive atomic force microscopy

NASA Astrophysics Data System (ADS)

Waddell, J.; Ou, R.; Capozzi, C. J.; Gupta, S.; Parker, C. A.; Gerhardt, R. A.; Seal, K.; Kalinin, S. V.; Baddorf, A. P.

2009-12-01

Composite specimens possessing polyhedral segregated network microstructures require a very small amount of nanosize filler, <1 vol %, to reach percolation because percolation occurs by accumulation of the fillers along the edges of the deformed polymer matrix particles. In this paper, electrostatic force microscopy (EFM) and conductive atomic force microscopy (C-AFM) were used to confirm the location of the nanosize fillers and the corresponding percolating paths in polymethyl methacrylate/carbon black composites. The EFM and C-AFM images revealed that the polyhedral polymer particles were coated with filler, primarily on the edges as predicted by the geometric models provided.

Super-resolution atomic force photoactivated microscopy of biological samples (Conference Presentation)

NASA Astrophysics Data System (ADS)

Lee, Seunghyun; Kim, Hyemin; Shin, Seungjun; Doh, Junsang; Kim, Chulhong

2017-03-01

Optical microscopy (OM) and photoacoustic microscopy (PAM) have previously been used to image the optical absorption of intercellular features of biological cells. However, the optical diffraction limit ( 200 nm) makes it difficult for these modalities to image nanoscale inner cell structures and the distribution of internal cell components. Although super-resolution fluorescence microscopy, such as stimulated emission depletion microscopy (STED) and stochastic optical reconstruction microscopy (STORM), has successfully performed nanoscale biological imaging, these modalities require the use of exogenous fluorescence agents, which are unfavorable for biological samples. Our newly developed atomic force photoactivated microscopy (AFPM) can provide optical absorption images with nanoscale lateral resolution without any exogenous contrast agents. AFPM combines conventional atomic force microscopy (AFM) and an optical excitation system, and simultaneously provides multiple contrasts, such as the topography and magnitude of optical absorption. AFPM can detect the intrinsic optical absorption of samples with 8 nm lateral resolution, easily overcoming the diffraction limit. Using the label-free AFPM system, we have successfully imaged the optical absorption properties of a single melanoma cell (B16F10) and a rosette leaf epidermal cell of Arabidopsis (ecotype Columbia (Col-0)) with nanoscale lateral resolution. The remarkable images show the melanosome distribution of a melanoma cell and the biological structures of a plant cell. AFPM provides superior imaging of optical absorption with a nanoscale lateral resolution, and it promises to become widely used in biological and chemical research.

Optimisation of specimen temperature and pulse fraction in atom probe microscopy experiments on a microalloyed steel.

PubMed

Yao, L; Cairney, J M; Zhu, C; Ringer, S P

2011-05-01

This paper details the effects of systematic changes to the experimental parameters for atom probe microscopy of microalloyed steels. We have used assessments of the signal-to-noise ratio (SNR), compositional measurements and field desorption images to establish the optimal instrumental parameters. These corresponded to probing at the lowest possible temperature (down to 20K) with the highest possible pulse fraction (up to 30%). A steel containing a fine dispersion of solute atom clusters was used as an archetype to demonstrate the importance of running the atom probe at optimum conditions. Crown Copyright © 2010. Published by Elsevier B.V. All rights reserved.

A kilobyte rewritable atomic memory

NASA Astrophysics Data System (ADS)

Kalff, Floris; Rebergen, Marnix; Fahrenfort, Nora; Girovsky, Jan; Toskovic, Ranko; Lado, Jose; FernáNdez-Rossier, JoaquíN.; Otte, Sander

The ability to manipulate individual atoms by means of scanning tunneling microscopy (STM) opens op opportunities for storage of digital data on the atomic scale. Recent achievements in this direction include data storage based on bits encoded in the charge state, the magnetic state, or the local presence of single atoms or atomic assemblies. However, a key challenge at this stage is the extension of such technologies into large-scale rewritable bit arrays. We demonstrate a digital atomic-scale memory of up to 1 kilobyte (8000 bits) using an array of individual surface vacancies in a chlorine terminated Cu(100) surface. The chlorine vacancies are found to be stable at temperatures up to 77 K. The memory, crafted using scanning tunneling microscopy at low temperature, can be read and re-written automatically by means of atomic-scale markers, and offers an areal density of 502 Terabits per square inch, outperforming state-of-the-art hard disk drives by three orders of magnitude.

Detection of isolated protein-bound metal ions by single-particle cryo-STEM.

PubMed

Elad, Nadav; Bellapadrona, Giuliano; Houben, Lothar; Sagi, Irit; Elbaum, Michael

2017-10-17

Metal ions play essential roles in many aspects of biological chemistry. Detecting their presence and location in proteins and cells is important for understanding biological function. Conventional structural methods such as X-ray crystallography and cryo-transmission electron microscopy can identify metal atoms on protein only if the protein structure is solved to atomic resolution. We demonstrate here the detection of isolated atoms of Zn and Fe on ferritin, using cryogenic annular dark-field scanning transmission electron microscopy (cryo-STEM) coupled with single-particle 3D reconstructions. Zn atoms are found in a pattern that matches precisely their location at the ferroxidase sites determined earlier by X-ray crystallography. By contrast, the Fe distribution is smeared along an arc corresponding to the proposed path from the ferroxidase sites to the mineral nucleation sites along the twofold axes. In this case the single-particle reconstruction is interpreted as a probability distribution function based on the average of individual locations. These results establish conditions for detection of isolated metal atoms in the broader context of electron cryo-microscopy and tomography.

Detection of isolated protein-bound metal ions by single-particle cryo-STEM

PubMed Central

Elad, Nadav; Bellapadrona, Giuliano; Houben, Lothar; Sagi, Irit; Elbaum, Michael

2017-01-01

Metal ions play essential roles in many aspects of biological chemistry. Detecting their presence and location in proteins and cells is important for understanding biological function. Conventional structural methods such as X-ray crystallography and cryo-transmission electron microscopy can identify metal atoms on protein only if the protein structure is solved to atomic resolution. We demonstrate here the detection of isolated atoms of Zn and Fe on ferritin, using cryogenic annular dark-field scanning transmission electron microscopy (cryo-STEM) coupled with single-particle 3D reconstructions. Zn atoms are found in a pattern that matches precisely their location at the ferroxidase sites determined earlier by X-ray crystallography. By contrast, the Fe distribution is smeared along an arc corresponding to the proposed path from the ferroxidase sites to the mineral nucleation sites along the twofold axes. In this case the single-particle reconstruction is interpreted as a probability distribution function based on the average of individual locations. These results establish conditions for detection of isolated metal atoms in the broader context of electron cryo-microscopy and tomography. PMID:28973937

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.

Galvanostatically deposited Fe: MnO2 electrodes for supercapacitor application

NASA Astrophysics Data System (ADS)

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

2012-01-01

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

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

PubMed Central

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

2016-01-01

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

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

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

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

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

PubMed

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

2013-06-01

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

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

PubMed

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

2016-10-20

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

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

NASA Astrophysics Data System (ADS)

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

2018-02-01

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

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

NASA Astrophysics Data System (ADS)

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

2018-04-01

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

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

NASA Astrophysics Data System (ADS)

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

2018-05-01

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

Highly branched RuO2 Nanorods on Electrospun TiO2 Nanofibers toward Electrochemical Catalysts

NASA Astrophysics Data System (ADS)

Cho, Yukyung; Kim, Su-Jin; Lee, Nam-Suk; Kim, Myung Hwa; Lee, Youngmi

2014-03-01

We report a facile growth route to synthesize hierarchically grown single crystalline metallic RuO2 nanorods on electrospun TiO2 nanofibers via a combination of a simple vapour phase transport process with an electrospinning process. This synthetic strategy could be very useful to design a variety of highly branched network architectures of the functional hetero-nanostructures for electrochemical applications. Particularly, Ruthenium oxide (RuO2) 1-dimensional nanostructures can be used as the effective catalysts or electrochemical electrode materials. Thus, we first synthesize TiO2 nanofibers from mixture of titanium isopropoxide precursor and polymer and then ruthenium hydroxide precursor on TiO2 nanofibers are transformed into RuO2 nanorods by thermal treatment at 250oC in air. The crystalline structures of products are confirmed using scanning electron microscopy (FE-SEM), X-ray diffraction (XRD) spectrum, Raman spectroscopy, and high resolution electron microscopy (HRTEM). The fundamental electrochemical performances are examined using cyclic voltammetry (CV).

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

NASA Astrophysics Data System (ADS)

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

2018-01-01

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

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

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

NASA Astrophysics Data System (ADS)

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

2012-11-01

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

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

PubMed

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

2016-03-15

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

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

PubMed

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

2004-06-22

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

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

NASA Astrophysics Data System (ADS)

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

2016-10-01

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

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.

Highly Sensitive NiO Nanoparticle based Chlorine Gas Sensor

NASA Astrophysics Data System (ADS)

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

2018-03-01

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

Enhanced materials from nature: nanocellulose from citrus waste.

PubMed

Mariño, Mayra; Lopes da Silva, Lucimara; Durán, Nelson; Tasic, Ljubica

2015-04-03

Nanocellulose is a relatively inexpensive, highly versatile bio-based renewable material with advantageous properties, including biodegradability and nontoxicity. Numerous potential applications of nanocellulose, such as its use for the preparation of high-performance composites, have attracted much attention from industry. Owing to the low energy consumption and the addition of significant value, nanocellulose extraction from agricultural waste is one of the best alternatives for waste treatment. Different techniques for the isolation and purification of nanocellulose have been reported, and combining these techniques influences the morphology of the resultant fibers. Herein, some of the extraction routes for obtaining nanocellulose from citrus waste are addressed. The morphology of nanocellulose was determined by Scanning Electron Microscopy (SEM) and Field Emission Scanning Electron Microscopy (FESEM), while cellulose crystallinity indexes (CI) from lyophilized samples were determined using solid-state Nuclear Magnetic Resonance (NMR) and X-Ray Diffraction (XRD) measurements. The resultant nanofibers had 55% crystallinity, an average diameter of 10 nm and a length of 458 nm.

Rapidly synthesized ZnO nanowires by ultraviolet decomposition process in ambient air for flexible photodetector.

PubMed

Wu, Jyh Ming; Chen, Yi-Ru; Lin, Yu-Hung

2011-03-01

We are the first group to use a simple direct ultraviolet light (UV, λ=365 nm, I=76 mW cm(-2)) in a decomposition process to fabricate ZnO nanowires on a flexible substrate using a zinc acetylacetonate hydrate precursor in ambient air. ZnO nanocrystal (or nanowire) production only requires three to ten minutes. A field emission scanning electron microscopy (FESEM) image reveals a high aspect ratio of the ZnO nanowires, which are grown on a substrate with a diameter of ∼50-100 nm, and a length of up to several hundred microns. High resolution transmission electron microscopy (HRTEM) images reveal that the nanowires consist of many single crystalline ZnO nanoparticles that grow along the c axis, which suggests an oriented attachment process. A potential application for flexible UV photodetectors was investigated using a UV lamp (λ=365 nm, I=2.34 mW cm(-2)). A significant ratio of photocurrent to dark current--around 11,300%--was achieved.

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

PubMed

Khodadadi, Bahar; Bordbar, Maryam; Nasrollahzadeh, Mahmoud

2017-05-01

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

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.

Atom probe field ion microscopy and related topics: A bibliography 1993

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

Godfrey, R.D.; Miller, M.K.; Russell, K.F.

1994-10-01

This bibliography, covering the period 1993, includes references related to the following topics: atom probe field ion microscopy (APFIM), field emission (FE), and field ion microscopy (FIM). Technique-oriented studies and applications are included. The references contained in this document were compiled from a variety of sources including computer searches and personal lists of publications. To reduce the length of this document, the references have been reduced to the minimum necessary to locate the articles. The references are listed alphabetically by authors, an Addendum of references missed in previous bibliographies is included.

Microcontroller-driven fluid-injection system for atomic force microscopy.

PubMed

Kasas, S; Alonso, L; Jacquet, P; Adamcik, J; Haeberli, C; Dietler, G

2010-01-01

We present a programmable microcontroller-driven injection system for the exchange of imaging medium during atomic force microscopy. Using this low-noise system, high-resolution imaging can be performed during this process of injection without disturbance. This latter circumstance was exemplified by the online imaging of conformational changes in DNA molecules during the injection of anticancer drug into the fluid chamber.

Dynamics-Enabled Nanoelectromechanical Systems (NEMS) Oscillators

DTIC Science & Technology

2014-06-01

it becomes strongly nonlinear, and thus constitutes an archetypal candidate for nonlinear engineering • its fundamental resonant frequency...width of spectral peaks of atomic force microscopy (AFM) resonators as they are brought close to a surface. 39 Approved for public release...alternating current AD Allan Deviation AFM atomic force microscopy AFRL Air Force Research Laboratory AlN aluminum nitride APN Anomalous Phase

Influence of the dopant concentration on structural, optical and photovoltaic properties of Cu-doped ZnS nanocrystals based bulk heterojunction hybrid solar cells

NASA Astrophysics Data System (ADS)

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

2017-06-01

Zinc sulphide (ZnS) and Cu-doped ZnS nanoparticles were synthesized by the wet chemical method. The nanoparticles were characterized by UV-visible, fluorescence, fourier transform infra-red (FTIR) spectrometry, X-ray diffraction (XRD), X-ray photoelectron spectrometry (XPS), field emission scanning electron microscopy (FESEM) and high resolution transmission electron microscopy (HRTEM). Scanning electron microscopy supplemented with EDAX was employed to observe the morphology and chemical composition of the un-doped and doped samples. A significant blue shift of the absorption band with respect to the un-doped zinc sulphide was sighted by increasing the Cu concentration in the doped sample with decreasing the size of nanoparticles. Consequently, the band gap was tuned from 3.13 to 3.49 eV due to quantum confinement. The green emission arises from the recombination between the shallow donor level (sulfur vacancy) and the t2 level of Cu2+. However, the fluorescence emission spectrum of the undoped ZnS nanoparticles was deconvoluted into two bands, which are centered at 419 and 468 nm. XRD analysis showed that the nanomaterials were in cubic crystalline state. XRD peaks show that there were no massive crystalline distortions in the crystal lattice when the Cu concentration (0.05-0.1 M) was increased in the ZnS lattice. However, in the case of Cu-doped samples (0.15-0.2 M), the XRD pattern showed an additional peak at 37° due to incomplete substitution occurring during the experimental reaction step. A comparative study of surfaces of undoped and Cu-doped ZnS nanoparticles were investigated using X-ray photoelectron spectroscopy (XPS). The synthesized nanomaterial in combination with poly(3-hexylthiophene) (P3HT) was used in the fabrication of solar cells. The devices with ZnS nanoparticles showed an efficiency of 0.31%. The overall power conversion efficiency of the solar cells at 0.1 M Cu content in doped ZnS nanoparticles was found to be 1.6 times higher than the reference device (P3HT:ZnS). Furthermore, atomic force microscopy and X-ray diffraction techniques were employed to study morphology and packing behavior of blends of nanocrystals and polymer respectively. Contribution to the topical issue "Materials for Energy harvesting, conversion and storage II (ICOME 2016)", edited by Jean-Michel Nunzi, Rachid Bennacer and Mohammed El Ganaoui

Observation of multicellular spinning behavior of Proteus mirabilis by atomic force microscopy and multifunctional microscopy.

PubMed

Liu, Yanxia; Deng, Yuanxin; Luo, Shuxiu; Deng, Yu; Guo, Linming; Xu, Weiwei; Liu, Lei; Liu, Junkang

2014-01-01

This study aimed to observe the multicellular spinning behavior of Proteus mirabilis by atomic force microscopy (AFM) and multifunctional microscopy in order to understand the mechanism underlying this spinning movement and its biological significance. Multifunctional microscopy with charge-coupled device (CCD) and real-time AFM showed changes in cell structure and shape of P. mirabilis during multicellular spinning movement. Specifically, the morphological characteristics of P. mirabilis, multicellular spinning dynamics, and unique movement were observed. Our findings indicate that the multicellular spinning behavior of P. mirabilis may be used to collect nutrients, perform colonization, and squeeze out competitors. The movement characteristics of P. mirabilis are vital to the organism's biological adaptability to the surrounding environment. Copyright © 2013 Elsevier Ltd. All rights reserved.

VEDA: a web-based virtual environment for dynamic atomic force microscopy.

PubMed

Melcher, John; Hu, Shuiqing; Raman, Arvind

2008-06-01

We describe here the theory and applications of virtual environment dynamic atomic force microscopy (VEDA), a suite of state-of-the-art simulation tools deployed on nanoHUB (www.nanohub.org) for the accurate simulation of tip motion in dynamic atomic force microscopy (dAFM) over organic and inorganic samples. VEDA takes advantage of nanoHUB's cyberinfrastructure to run high-fidelity dAFM tip dynamics computations on local clusters and the teragrid. Consequently, these tools are freely accessible and the dAFM simulations are run using standard web-based browsers without requiring additional software. A wide range of issues in dAFM ranging from optimal probe choice, probe stability, and tip-sample interaction forces, power dissipation, to material property extraction and scanning dynamics over hetereogeneous samples can be addressed.

Invited Article: VEDA: A web-based virtual environment for dynamic atomic force microscopy

NASA Astrophysics Data System (ADS)

Melcher, John; Hu, Shuiqing; Raman, Arvind

2008-06-01

We describe here the theory and applications of virtual environment dynamic atomic force microscopy (VEDA), a suite of state-of-the-art simulation tools deployed on nanoHUB (www.nanohub.org) for the accurate simulation of tip motion in dynamic atomic force microscopy (dAFM) over organic and inorganic samples. VEDA takes advantage of nanoHUB's cyberinfrastructure to run high-fidelity dAFM tip dynamics computations on local clusters and the teragrid. Consequently, these tools are freely accessible and the dAFM simulations are run using standard web-based browsers without requiring additional software. A wide range of issues in dAFM ranging from optimal probe choice, probe stability, and tip-sample interaction forces, power dissipation, to material property extraction and scanning dynamics over hetereogeneous samples can be addressed.

Preparation and characterization of ultraflat Pt facets by atom-height-resolved differential optical microscopy

NASA Astrophysics Data System (ADS)

Azhagurajan, M.; Wen, R.; Kim, Y. G.; Itoh, T.; Sashikata, K.; Itaya, K.

2015-01-01

We recently demonstrated that improvements to our technique, laser confocal microscopy with differential interference microscopy (LCM-DIM), has rendered it fully capable of resolving monatomic steps with heights of ca. 0.25 nm on Au(111) and Pd(111) surfaces, even as low as 0.14 nm on Si(100), in aqueous solution. In this paper, we describe in detail a method to prepare and characterize, via atomic-layer-resolved LCM-DIM, ultraflat Pt(111) and Pt(100) facets over a wide surface area. The preparation of ultraflat surfaces is important in the characterization at the atomic scale of electrochemical processes under reaction conditions. To showcase the elegance of LCM-DIM, the anodic dissolution of Pt in aqueous HCl is briefly recounted.

Three-dimensional atomic force microscopy mapping at the solid-liquid interface with fast and flexible data acquisition

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

Söngen, Hagen, E-mail: soengen@uni-mainz.de; Graduate School Materials Science in Mainz, Staudinger Weg 9, 55128 Mainz; Nalbach, Martin

2016-06-15

We present the implementation of a three-dimensional mapping routine for probing solid-liquid interfaces using frequency modulation atomic force microscopy. Our implementation enables fast and flexible data acquisition of up to 20 channels simultaneously. The acquired data can be directly synchronized with commercial atomic force microscope controllers, making our routine easily extendable for related techniques that require additional data channels, e.g., Kelvin probe force microscopy. Moreover, the closest approach of the tip to the sample is limited by a user-defined threshold, providing the possibility to prevent potential damage to the tip. The performance of our setup is demonstrated by visualizing themore » hydration structure above the calcite (10.4) surface in water.« less

Imaging contrast and tip-sample interaction of non-contact amplitude modulation atomic force microscopy with Q-control

NASA Astrophysics Data System (ADS)

Shi, Shuai; Guo, Dan; Luo, Jianbin

2017-10-01

Active quality factor (Q) exhibits many promising properties in dynamic atomic force microscopy. Energy dissipation and image contrasts are investigated in the non-contact amplitude modulation atomic force microscopy (AM-AFM) with an active Q-control circuit in the ambient air environment. Dissipated power and virial were calculated to compare the highly nonlinear interaction of tip-sample and image contrasts with different Q gain values. Greater free amplitudes and lower effective Q values show better contrasts for the same setpoint ratio. Active quality factor also can be employed to change tip-sample interaction force in non-contact regime. It is meaningful that non-destructive and better contrast images can be realized in non-contact AM-AFM by applying an active Q-control to the dynamic system.

Effect of bismuth substitution in strontium hexaferrite

NASA Astrophysics Data System (ADS)

Sahoo, M. R.; Kuila, S.; Sweta, K.; Barik, A.; Vishwakarma, P. N.

2018-05-01

Bismuth (Bi) substituted M-type strontium hexaferrite (Sr1-xBix Fe12O19, x=0 and 0.02) are synthesized by sol-gel auto combustion method. Powder X-ray diffraction (XRD) and field emission scanning electron microscopy (FESEM) shows increase in lattice parameter and particle size (500 nm to 3 micron) respectively, for Bi substituted sample. Magnetization via M-H shows decrease in magnetic hardness for Bi substituted samples. M-T data for parent (x=0) sample shows an antiferromagnetic transition in the ZFC plot at 495 °C. This antiferromagnetic transition is replaced by a ferromagnetic transition for FCW measurement. Similar behavior is displayed by the Bi substituted sample with transition temperature reduced to 455 °C.

The Synthesis and Photoluminescent Properties of CaMoO₄:Eu³⁺ Nanocrystals by a Soft Chemical Route.

PubMed

Li, Fuhai; Yu, Lixin; Sun, Jiaju; Li, Songchu; Wei, Shuilin

2017-04-01

In this paper, the CaMoO4:Eu3+ phosphors were prepared by a simple hydrothermal method assisted by the citric acid as the surfactant, and characterized by X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM), and fluorescent spectrophotometry. The results of XRD show that the as-prepared samples are single phase. The process of the Ostwald ripening is controlled by the content of the citric acid in the hydrothermal reaction. The pH value of the precursor affects the shift of the charge transition band (CTB) in the excitation spectra. The reaction condition can strongly affect the luminescent intensity of the samples.

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.

Sonochemically synthesized iron-doped zinc oxide nanoparticles: Influence of precursor composition on characteristics

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

Roy, Anirban; Maitra, Saikat; Ghosh, Sobhan

Highlights: • Sonochemical synthesis of iron-doped zinc oxide nanoparticles. • Green synthesis without alkali at room temperature. • Characterization by UV–vis spectroscopy, FESEM, XRD and EDX. • Influence of precursor composition on characteristics. • Composition and characteristics are correlated. - Abstract: Iron-doped zinc oxide nanoparticles have been synthesized sonochemically from aqueous acetyl acetonate precursors of different proportions. Synthesized nanoparticles were characterized with UV–vis spectroscopy, X-ray diffraction and microscopy. Influences of precursor mixture on the characteristics have been examined and modeled. Linear correlations have been proposed between dopant dosing, extent of doping and band gap energy. Experimental data corroborated with themore » proposed models.« less

Local carrier distribution imaging on few-layer MoS2 exfoliated on SiO2 by scanning nonlinear dielectric microscopy

NASA Astrophysics Data System (ADS)

Yamasue, Kohei; Cho, Yasuo

2018-06-01

We demonstrate that scanning nonlinear dielectric microscopy (SNDM) can be used for the nanoscale characterization of dominant carrier distribution on atomically thin MoS2 mechanically exfoliated on SiO2. For stable imaging without damaging microscopy tips and samples, SNDM was combined with peak-force tapping mode atomic force microscopy. The identification of dominant carriers and their spatial distribution becomes possible even for single and few-layer MoS2 on SiO2 using the proposed method allowing differential capacitance (dC/dV) imaging. We can expect that SNDM can also be applied to the evaluation of other two-dimensional semiconductors and devices.

Applications of AFM for atomic manipulation and spectroscopy

NASA Astrophysics Data System (ADS)

Custance, Oscar

2009-03-01

Since the first demonstration of atom-by-atom assembly [1], atomic manipulation with scanning tunneling microscopy has yielded stunning realizations in nanoscience. A new exciting panorama has been recently opened with the possibility of manipulating atoms at surfaces using atomic force microscopy (AFM) [2-5]. In this talk, we will present two different approaches that enable patterning structures at semiconductor surfaces by manipulating individual atoms with AFM and at room temperature [2, 3]. We will discuss the physics behind each protocol through the analysis of the measured forces associated with these manipulations [3-5]. Another challenging issue in scanning probe microscopy is the ability to disclose the local chemical composition of a multi-element system at atomic level. Here, we will introduce a single-atom chemical identification method, which is based on detecting the forces between the outermost atom of the AFM tip and the atoms at a surface [6]. We demonstrate this identification procedure on a particularly challenging system, where any discrimination attempt based solely on topographic measurements would be impossible to achieve. [4pt] References: [0pt] [1] D. M. Eigler and E. K. Schweizer, Nature 344, 524 (1990); [0pt] [2] Y. Sugimoto, M. Abe, S. Hirayama, N. Oyabu, O. Custance and S. Morita, Nature Materials 4, 156 (2005); [0pt] [3] Y. Sugimoto, P. Pou, O. Custance, P. Jelinek, M. Abe, R. Perez and S. Morita, Science 322, 413 (2008); [0pt] [4] Y. Sugimoto, P. Jelinek, P. Pou, M. Abe, S. Morita, R. Perez and O. Custance, Phys. Rev. Lett. 98, 106104 (2007); [0pt] [5] M. Ternes, C. P. Lutz, C. F. Hirjibehedin, F. J. Giessibl and A. J. Heinrich, Science 319, 1066 (2008); [0pt] [6] Y. Sugimoto, P. Pou, M. Abe, P. Jelinek, R. Perez, S. Morita, and O. Custance, Nature 446, 64 (2007)

Conductive atomic force microscopy studies on the transformation of GeSi quantum dots to quantum rings.

PubMed

Zhang, S L; Xue, F; Wu, R; Cui, J; Jiang, Z M; Yang, X J

2009-04-01

Conductive atomic force microscopy has been employed to study the topography and conductance distribution of individual GeSi quantum dots (QDs) and quantum rings (QRs) during the transformation from QDs to QRs by depositing an Si capping layer on QDs. The current distribution changes significantly with the topographic transformation during the Si capping process. Without the capping layer, the QDs are dome-shaped and the conductance is higher at the ring region between the center and boundary than that at the center. After capping with 0.32 nm Si, the shape of the QDs changes to pyramidal and the current is higher at both the center and the arris. When the Si capping layer increases to 2 nm, QRs are formed and the current of individual QRs is higher at the rim than that at the central hole. By comparing the composition distributions obtained by scanning Auger microscopy and atomic force microscopy combined with selective chemical etching, the origin of the current distribution change is discussed.

Manipulating Si(100) at 5 K using qPlus frequency modulated atomic force microscopy: Role of defects and dynamics in the mechanical switching of atoms

NASA Astrophysics Data System (ADS)

Sweetman, A.; Jarvis, S.; Danza, R.; Bamidele, J.; Kantorovich, L.; Moriarty, P.

2011-08-01

We use small-amplitude qPlus frequency modulated atomic force microscopy (FM-AFM), at 5 K, to investigate the atomic-scale mechanical stability of the Si(100) surface. By operating at zero applied bias the effect of tunneling electrons is eliminated, demonstrating that surface manipulation can be performed by solely mechanical means. Striking differences in surface response are observed between different regions of the surface, most likely due to variations in strain associated with the presence of surface defects. We investigate the variation in local energy surface by ab initio simulation, and comment on the dynamics observed during force spectroscopy.

Effects of the local structure dependence of evaporation fields on field evaporation behavior

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

Yao, Lan; Marquis, Emmanuelle A., E-mail: emarq@umich.edu; Withrow, Travis

2015-12-14

Accurate three dimensional reconstructions of atomic positions and full quantification of the information contained in atom probe microscopy data rely on understanding the physical processes taking place during field evaporation of atoms from needle-shaped specimens. However, the modeling framework for atom probe microscopy has only limited quantitative justification. Building on the continuum field models previously developed, we introduce a more physical approach with the selection of evaporation events based on density functional theory calculations. This model reproduces key features observed experimentally in terms of sequence of evaporation, evaporation maps, and depth resolution, and provides insights into the physical limit formore » spatial resolution.« less

Concept for room temperature single-spin tunneling force microscopy with atomic spatial resolution

NASA Astrophysics Data System (ADS)

Payne, Adam

A study of a force detected single-spin magnetic resonance measurement concept with atomic spatial resolution is presented. The method is based upon electrostatic force detection of spin-selection rule controlled single electron tunneling between two electrically isolated paramagnetic states. Single-spin magnetic resonance detection is possible by measuring the force detected tunneling charge noise on and off spin resonance. Simulation results of this charge noise, based upon physical models of the tunneling and spin physics, are directly compared to measured atomic force microscopy (AFM) system noise. The results show that the approach could provide single-spin measurement of electrically isolated defect states with atomic spatial resolution at room temperature.

Atomic-resolution single-spin magnetic resonance detection concept based on tunneling force microscopy

NASA Astrophysics Data System (ADS)

Payne, A.; Ambal, K.; Boehme, C.; Williams, C. C.

2015-05-01

A study of a force detected single-spin magnetic resonance measurement concept with atomic spatial resolution is presented. The method is based upon electrostatic force detection of spin-selection rule controlled single-electron tunneling between two electrically isolated paramagnetic states. Single-spin magnetic resonance detection is possible by measuring the force detected tunneling charge noise on and off spin resonance. Simulation results of this charge noise, based upon physical models of the tunneling and spin physics, are directly compared to measured atomic force microscopy system noise. The results show that the approach could provide single-spin measurement of electrically isolated qubit states with atomic spatial resolution at room temperature.

Imaging and manipulation of adatoms on an alumina surface by noncontact atomic force microscopy

NASA Astrophysics Data System (ADS)

Simon, G. H.; Heyde, M.; Freund, H.-J.

2012-02-01

Noncontact atomic force microscopy (NC-AFM) has been performed on an aluminum oxide film grown on NiAl(110) in ultrahigh vacuum (UHV) at low temperature (5 K). Results reproduce the topography of the structural model, unlike scanning tunnelling microscopy (STM) images. Equipped with this extraordinary contrast the network of extended defects, which stems from domain boundaries intersecting the film surface, can be analysed in atomic detail. The knowledge of occurring surface structures opens up the opportunity to determine adsorption sites of individual adsorbates on the alumina film. The level of difficulty for such imaging depends on the imaging characteristics of the substrate and the interaction which can be maintained above the adsorbate. Positions of single adsorbed gold atoms within the unit cell have been determined despite their easy removal at slightly higher interaction strength. Preliminary manipulation experiments indicate a pick-up process for the vanishing of the gold adatoms from the film surface.

Influence of atomic tip structure on the intensity of inelastic tunneling spectroscopy data analyzed by combined scanning tunneling spectroscopy, force microscopy, and density functional theory

NASA Astrophysics Data System (ADS)

Okabayashi, Norio; Gustafsson, Alexander; Peronio, Angelo; Paulsson, Magnus; Arai, Toyoko; Giessibl, Franz J.

2016-04-01

Achieving a high intensity in inelastic scanning tunneling spectroscopy (IETS) is important for precise measurements. The intensity of the IETS signal can vary by up to a factor of 3 for various tips without an apparent reason accessible by scanning tunneling microscopy (STM) alone. Here, we show that combining STM and IETS with atomic force microscopy enables carbon monoxide front-atom identification, revealing that high IETS intensities for CO/Cu(111) are obtained for single-atom tips, while the intensity drops sharply for multiatom tips. Adsorption of the CO molecule on a Cu adatom [CO/Cu/Cu(111)] such that the molecule is elevated over the substrate strongly diminishes the tip dependence of IETS intensity, showing that an elevated position channels most of the tunneling current through the CO molecule even for multiatom tips, while a large fraction of the tunneling current bypasses the CO molecule in the case of CO/Cu(111).

SEM and AFM Studies of Two-Phase Magnetic Alkali Borosilicate Glasses

PubMed Central

Tomkovich, M.; Nacke, B.; Filimonov, A.; Alekseeva, O.; Vanina, P.; Nizhankovskii, V.

2017-01-01

The morphology and composition of four types of two-phase alkali borosilicate glasses with magnetic atoms prepared by inductive melting have been studied. The results of scanning electron microscopy point to uniform distribution of Na, Si, and O atoms in these samples while magnetic iron atoms form ball-shaped agglomerates. The magnetic properties of these agglomerates have been confirmed by magnetic force microscopy. Atomic force microscopy had shown that in these samples two different morphological structures, drop-like and dendrite net, are formed. The formation of dendrite-like structure is a necessary condition for production of porous magnetic glasses. The obtained results allow us to optimize the melting and heat treatment processes leading to production of porous alkali borosilicate glasses with magnetic properties. The first results for nanocomposite materials on the basis of magnetic glasses containing the embedded ferroelectrics KH2PO4 demonstrate the effect of applied magnetic field on the ferroelectric phase transition. PMID:28428976

The significance of Bragg's law in electron diffraction and microscopy, and Bragg's second law.

PubMed

Humphreys, C J

2013-01-01

Bragg's second law, which deserves to be more widely known, is recounted. The significance of Bragg's law in electron diffraction and microscopy is then discussed, with particular emphasis on differences between X-ray and electron diffraction. As an example of such differences, the critical voltage effect in electron diffraction is described. It is then shown that the lattice imaging of crystals in high-resolution electron microscopy directly reveals the Bragg planes used for the imaging process, exactly as visualized by Bragg in his real-space law. Finally, it is shown how in 2012, for the first time, on the centennial anniversary of Bragg's law, single atoms have been identified in an electron microscope using X-rays emitted from the specimen. Hence atomic resolution X-ray maps of a crystal in real space can be formed which give the positions and identities of the different atoms in the crystal, or of a single impurity atom in the crystal.

Two-probe STM experiments at the atomic level.

PubMed

Kolmer, Marek; Olszowski, Piotr; Zuzak, Rafal; Godlewski, Szymon; Joachim, Christian; Szymonski, Marek

2017-11-08

Direct characterization of planar atomic or molecular scale devices and circuits on a supporting surface by multi-probe measurements requires unprecedented stability of single atom contacts and manipulation of scanning probes over large, nanometer scale area with atomic precision. In this work, we describe the full methodology behind atomically defined two-probe scanning tunneling microscopy (STM) experiments performed on a model system: dangling bond dimer wire supported on a hydrogenated germanium (0 0 1) surface. We show that 70 nm long atomic wire can be simultaneously approached by two independent STM scanners with exact probe to probe distance reaching down to 30 nm. This allows direct wire characterization by two-probe I-V characteristics at distances below 50 nm. Our technical results presented in this work open a new area for multi-probe research, which can be now performed with precision so far accessible only by single-probe scanning probe microscopy (SPM) experiments.

Learning about Modes in Atomic Force Microscopy by Means of Hands-On Activities Based on a Simple Apparatus

ERIC Educational Resources Information Center

Phuapaiboon, Unchada; Panijpan, Bhinyo; Osotchan, Tanakorn

2009-01-01

This study was conducted to examine the results of using a low-cost hands-on setup in combination with accompanying activities to promote understanding of the contact mode of atomic force microscopy (AFM). This contact mode setup enabled learners to study how AFM works by hand scanning using probing cantilevers with different characteristics on…

Optimization of a constrained linear monochromator design for neutral atom beams.

PubMed

Kaltenbacher, Thomas

2016-04-01

A focused ground state, neutral atom beam, exploiting its de Broglie wavelength by means of atom optics, is used for neutral atom microscopy imaging. Employing Fresnel zone plates as a lens for these beams is a well established microscopy technique. To date, even for favorable beam source conditions a minimal focus spot size of slightly below 1μm was reached. This limitation is essentially given by the intrinsic spectral purity of the beam in combination with the chromatic aberration of the diffraction based zone plate. Therefore, it is important to enhance the monochromaticity of the beam, enabling a higher spatial resolution, preferably below 100nm. We propose to increase the monochromaticity of a neutral atom beam by means of a so-called linear monochromator set-up - a Fresnel zone plate in combination with a pinhole aperture - in order to gain more than one order of magnitude in spatial resolution. This configuration is known in X-ray microscopy and has proven to be useful, but has not been applied to neutral atom beams. The main result of this work is optimal design parameters based on models for this linear monochromator set-up followed by a second zone plate for focusing. The optimization was performed for minimizing the focal spot size and maximizing the centre line intensity at the detector position for an atom beam simultaneously. The results presented in this work are for, but not limited to, a neutral helium atom beam. Copyright © 2016 Elsevier B.V. All rights reserved.

Investigation on Adsorption and the Corrosion Inhibition Effect of Some Novel Hydrazide Derivatives for Mild Steel in HCl Solution

NASA Astrophysics Data System (ADS)

Singh, Dharmendra Kumar; Behera, Debasis; Singh, Mantu Kumar; Udayabhanu, G.; John, Rohith P.

2017-10-01

Two hydrazide derivatives, namely, N'-(thiophene-2-ylmethylene)nicotinic hydrazone (TNH) and N'-(pyrrol-2-ylmethylene)nicotinic hydrazone (PNH), have been synthesized and investigated as corrosion inhibitors for mild steel in 1 M HCl solution by electrochemical, weight loss, field emission-scanning electron microscope (FE-SEM), atomic force microscope (AFM), and quantum chemical calculation methods. The experimental results show that both the compounds are good inhibitors for mild steel in 1 M HCl. They act as mixed type inhibitors with predominating cathodic character. The adsorption of inhibitors obeys the Langmuir adsorption isotherm. Correlation between quantum chemical parameters and experimental results is discussed.

A Filtering Method to Reveal Crystalline Patterns from Atom Probe Microscopy Desorption Maps

DTIC Science & Technology

2016-03-26

Gault, S.P. Ringer, J.M. Cairney, Atom probe crystallography : characterization of grain boundary orientation relationships in nanocrystalline...J.M. Cairney, Atom probe crystallography : atomic- scale 3-D orientation mapping, Scr. Mater. 66 (11) (2012) 907. L. Yao /MethodsX 3 (2016) 268–273 273

Surface Characterization.

ERIC Educational Resources Information Center

Fulghum, J. E.; And Others

1989-01-01

This review is divided into the following analytical methods: ion spectroscopy, electron spectroscopy, scanning tunneling microscopy, atomic force microscopy, optical spectroscopy, desorption techniques, and X-ray techniques. (MVL)

Atomic-Scale Variations of the Mechanical Response of 2D Materials Detected by Noncontact Atomic Force Microscopy.

PubMed

de la Torre, B; Ellner, M; Pou, P; Nicoara, N; Pérez, Rubén; Gómez-Rodríguez, J M

2016-06-17

We show that noncontact atomic force microscopy (AFM) is sensitive to the local stiffness in the atomic-scale limit on weakly coupled 2D materials, as graphene on metals. Our large amplitude AFM topography and dissipation images under ultrahigh vacuum and low temperature resolve the atomic and moiré patterns in graphene on Pt(111), despite its extremely low geometric corrugation. The imaging mechanisms are identified with a multiscale model based on density-functional theory calculations, where the energy cost of global and local deformations of graphene competes with short-range chemical and long-range van der Waals interactions. Atomic contrast is related with short-range tip-sample interactions, while the dissipation can be understood in terms of global deformations in the weakly coupled graphene layer. Remarkably, the observed moiré modulation is linked with the subtle variations of the local interplanar graphene-substrate interaction, opening a new route to explore the local mechanical properties of 2D materials at the atomic scale.

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

Phuthong, Witchukorn; Huang, Zubin; Wittkopp, Tyler M.

To investigate the dynamics of photosynthetic pigment-protein complexes in vascular plants at high resolution in an aqueous environment, membrane-protruding oxygen-evolving complexes (OECs) associated with photosystem II (PSII) on spinach ( Spinacia oleracea) grana membranes were examined using contact mode atomic force microscopy. This study represents, to our knowledge, the first use of atomic force microscopy to distinguish the putative large extrinsic loop of Photosystem II CP47 reaction center protein (CP47) from the putative oxygen-evolving enhancer proteins 1, 2, and 3 (PsbO, PsbP, and PsbQ) and large extrinsic loop of Photosystem II CP43 reaction center protein (CP43) in the PSII-OEC extrinsicmore » domains of grana membranes under conditions resulting in the disordered arrangement of PSII-OEC particles. Moreover, we observed uncharacterized membrane particles that, based on their physical characteristics and electrophoretic analysis of the polypeptides associated with the grana samples, are hypothesized to be a domain of photosystem I that protrudes from the stromal face of single thylakoid bilayers. Furthermore, our results are interpreted in the context of the results of others that were obtained using cryo-electron microscopy (and single particle analysis), negative staining and freeze-fracture electron microscopy, as well as previous atomic force microscopy studies.« less

Surface modifications with Lissajous trajectories using atomic force microscopy

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

Cai, Wei; Yao, Nan, E-mail: nyao@princeton.edu

2015-09-14

In this paper, we report a method for atomic force microscopy surface modifications with single-tone and multiple-resolution Lissajous trajectories. The tip mechanical scratching experiments with two series of Lissajous trajectories were carried out on monolayer films. The scratching processes with two scan methods have been illustrated. As an application, the tip-based triboelectrification phenomenon on the silicon dioxide surface with Lissajous trajectories was investigated. The triboelectric charges generated within the tip rubbed area on the surface were characterized in-situ by scanning Kelvin force microscopy. This method would provide a promising and cost-effective approach for surface modifications and nanofabrication.

An observation of nanotwin lamellae in Cd 0.6Mn 0.4Te crystal by atomic force microscopy

NASA Astrophysics Data System (ADS)

George, M. A.; Azoulay, M.; Collins, W. E.; Burger, A.; Silberman, E.

1993-05-01

Atomic force microscopy (AFM) is used to examine the structure of freshly cleaved Cd 0.6Mn 0.4Te surfaces. The present report complements previous results obtained with X-ray diffraction and optical microscopy which showed the existence of microtwins. The AFM analysis was performed under ambient conditions and yielded nanometer scale resolution images of single twin lamellae that ranged between 20 and 100 nm in width. This is a first observation using AFM of such a substructure, which we interpret as evidence for the presence of nonotwins.

Co-axial Electrospun Polyacrylonitrile-Poly(methylmethacrylate) Nanofibers: Atomic Force Microscopy and Compositional Characterization

PubMed Central

Zander, N.E.; Strawhecker, K.E.; Orlicki, J.A.; Rawlett, A.M.; Beebe, T.P.

2011-01-01

Poly(methylmethacrylate) (PMMA)- Polyacrylonitrile (PAN) fibers were prepared using a conventional single-nozzle electrospinning technique. The as-spun fibers exhibited core-shell morphology as verified by transmission electron microscopy (TEM) and atomic force microscopy (AFM). AFM-phase and modulus mapping images of the fiber cross-section and x-ray photoelectron spectroscopy (XPS) analysis indicated PAN formed the shell and PMMA the core material. XPS, thermal gravimetric analysis (TGA), and elemental analysis were used to determine fiber compositional information. Soaking the fibers in solvent demonstrated removal of the core material, generating hollow PAN fibers. PMID:21928836

Understanding amyloid aggregation by statistical analysis of atomic force microscopy images

NASA Astrophysics Data System (ADS)

Adamcik, Jozef; Jung, Jin-Mi; Flakowski, Jérôme; de Los Rios, Paolo; Dietler, Giovanni; Mezzenga, Raffaele

2010-06-01

The aggregation of proteins is central to many aspects of daily life, including food processing, blood coagulation, eye cataract formation disease and prion-related neurodegenerative infections. However, the physical mechanisms responsible for amyloidosis-the irreversible fibril formation of various proteins that is linked to disorders such as Alzheimer's, Creutzfeldt-Jakob and Huntington's diseases-have not yet been fully elucidated. Here, we show that different stages of amyloid aggregation can be examined by performing a statistical polymer physics analysis of single-molecule atomic force microscopy images of heat-denatured β-lactoglobulin fibrils. The atomic force microscopy analysis, supported by theoretical arguments, reveals that the fibrils have a multistranded helical shape with twisted ribbon-like structures. Our results also indicate a possible general model for amyloid fibril assembly and illustrate the potential of this approach for investigating fibrillar systems.

Effects of Starting Precursor Ratio on Optoelectrical Properties and Blue Emission of Nanostructured C-ZnS Thin Films Prepared by Spin Coating

NASA Astrophysics Data System (ADS)

Rahimzadeh, N.; Ghodsi, F. E.; Mazloom, J.

2018-02-01

Nanocrystalline cubic zinc sulfide (C-ZnS) thin films have been elaborated by sol-gel spin-coating of Zn(Ac)/thiourea starting precursors at different molar ratios, and their structural, morphological, compositional, optical, electrical, and photoluminescence properties comprehensively investigated. x-ray diffraction results showed that the samples had dominant cubic structure and their crystallinity improved with increasing S content. Morphological characterization of the C-ZnS thin films was carried out by field-emission scanning electron microscopy (FESEM), revealing that the films were smooth with spherical grains included in clusters. Energy-dispersive x-ray and Fourier-transform infrared spectra of ZnS compounds did not show any evidence of impurities. Optical characterization revealed increases of the average optical transmittance and bandgap (from 3.2 eV to 3.56 eV) with increasing S content. The refractive index in the visible region increased with the S content, while the extinction coefficient decreased. The compositional dependence of the optical dispersion parameters (oscillator and dispersion energy), dielectric constant, and surface energy loss function of the films was evaluated. Electrical characterization of the films was carried out using Hall-effect measurements. The ZnS thin films exhibited n-type conductivity, and the electrical resistivity decreased with increasing carrier concentration and mobility due to enhanced crystallite size and reduced structural disorder. Photoluminescence (PL) measurements indicated a blue-shift of the near-band-edge emission. The blue emission peaks centered at about 438 nm and 487 nm were enhanced due to transitions involving interstitial S atoms, surface states, and zinc vacancies.

Allochthonous Addition of Meteoritic Organics to the Lunar Regolith

NASA Technical Reports Server (NTRS)

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

2013-01-01

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

Nano-Electrochemistry and Nano-Electrografting with an Original Combined AFM-SECM

PubMed Central

Ghorbal, Achraf; Grisotto, Federico; Charlier, Julienne; Palacin, Serge; Goyer, Cédric; Demaille, Christophe; Ben Brahim, Ammar

2013-01-01

This study demonstrates the advantages of the combination between atomic force microscopy and scanning electrochemical microscopy. The combined technique can perform nano-electrochemical measurements onto agarose surface and nano-electrografting of non-conducting polymers onto conducting surfaces. This work was achieved by manufacturing an original Atomic Force Microscopy-Scanning ElectroChemical Microscopy (AFM-SECM) electrode. The capabilities of the AFM-SECM-electrode were tested with the nano-electrografting of vinylic monomers initiated by aryl diazonium salts. Nano-electrochemical and technical processes were thoroughly described, so as to allow experiments reproducing. A plausible explanation of chemical and electrochemical mechanisms, leading to the nano-grafting process, was reported. This combined technique represents the first step towards improved nano-processes for the nano-electrografting. PMID:28348337

Polymeric spatial resolution test patterns for mass spectrometry imaging using nano-thermal analysis with atomic force microscopy

DOE PAGES

Tai, Tamin; Kertesz, Vilmos; Lin, Ming -Wei; ...

2017-05-11

As the spatial resolution of mass spectrometry imaging technologies has begun to reach into the nanometer regime, finding readily available or easily made resolution reference materials has become particularly challenging for molecular imaging purposes. This study describes the fabrication, characterization and use of vertical line array polymeric spatial resolution test patterns for nano-thermal analysis/atomic force microscopy/mass spectrometry chemical imaging.

Effect of thermo-mechanical refining pressure on the properties of wood fibers as measured by nanoindentation and atomic force microscopy

Treesearch

Cheng Xing; Siqun Wang; George M. Pharr; Leslie H. Groom

2008-01-01

Refined wood fibers of a 54-year-old loblolly pine (Pinus taeda L.) mature wood were investigated by nanoindentation and atomic force microscopy (AFM). The effect of steam pressure, in the range of 2?18 bar, during thermomechanical refining was investigated and the nanomechanical properties and nano- or micro-level damages of the cell wall were...

The theoretical current-voltage dependence of a non-degenerate disordered organic material obtained with conductive atomic force microscopy

NASA Astrophysics Data System (ADS)

Woellner, Cristiano F.; Freire, José A.; Guide, Michele; Nguyen, Thuc-Quyen

2011-08-01

We develop a simple continuum model for the current voltage characteristics of a material as measured by the conducting atomic force microscopy, including space charge effects. We address the effect of the point contact on the magnitude of the current and on the transition voltages between the different current regimes by comparing these with the corresponding expressions obtained with planar electrodes.

Polymeric spatial resolution test patterns for mass spectrometry imaging using nano-thermal analysis with atomic force microscopy

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

Tai, Tamin; Kertesz, Vilmos; Lin, Ming -Wei

As the spatial resolution of mass spectrometry imaging technologies has begun to reach into the nanometer regime, finding readily available or easily made resolution reference materials has become particularly challenging for molecular imaging purposes. This study describes the fabrication, characterization and use of vertical line array polymeric spatial resolution test patterns for nano-thermal analysis/atomic force microscopy/mass spectrometry chemical imaging.

Atomic force microscopy visualization of injuries in Enterococcus faecalis surface caused by Er,Cr:YSGG and diode lasers

PubMed Central

López-Jiménez, Lidia; Viñas, Miguel; Vinuesa, Teresa

2015-01-01

Aim: To visualize by Atomic Force Microscopy the alterations induced on Enterococcus. faecalis surface after treatment with 2 types of laser: Erbium chromium:yttrium-scandium-gallium-garnet (Er,Cr:YSGG) laser and Diode laser. Material and Methods: Bacterial suspensions from overnight cultures of E. faecalis were irradiated during 30 seconds with the laser-lights at 1 W and 2 W of power, leaving one untreated sample as control. Surface alterations on treated E. faecalis were visualized by Atomic Force Microscopy (AFM) and its surface roughness determined. Results: AFM imaging showed that at high potency of laser both cell morphology and surface roughness resulted altered, and that several cell lysis signs were easily visualized. Surface roughness clearly increase after the treatment with Er,Cr:YSGG at 2W of power, while the other treatments gave similar values of surface roughness. The effect of lasers on bacterial surfaces visualized by AFM revealed drastic alterations. Conclusions: AFM is a good tool to evaluate surface injuries after laser treatment; and could constitute a measure of antimicrobial effect that can complete data obtained by determination of microbial viability. Key words:Atomic force microscopy, Er,Cr:YSGG laser, diode laser, Enterococcus faecalis, surface roughness. PMID:25475770

High indium content homogenous InAlN layers grown by plasma-assisted molecular beam epitaxy

NASA Astrophysics Data System (ADS)

Kyle, Erin C. H.; Kaun, Stephen W.; Wu, Feng; Bonef, Bastien; Speck, James S.

2016-11-01

InAlN grown by plasma-assisted molecular beam epitaxy often contains a honeycomb microstructure. The honeycomb microstructure consists of 5-10 nm diameter aluminum-rich regions which are surrounded by indium-rich regions. Layers without this microstructure were previously developed for nominally lattice-matched InAlN and have been developed here for higher indium content InAlN. In this study, InAlN was grown in a nitrogen-rich environment with high indium to aluminum flux ratios at low growth temperatures. Samples were characterized by high-resolution x-ray diffraction, atomic force microscopy, high-angle annular dark-field scanning transmission electron microscopy, and atom probe tomography. Atomic force microscopy showed InAlN layers grown at temperatures below 450 °C under nitrogen-rich conditions were free of droplets. InAlN films with indium contents up to 81% were grown at temperatures between 410 and 440 °C. High-angle annular dark-field scanning transmission electron microscopy and atom probe tomography showed no evidence of honeycomb microstructure for samples with indium contents of 34% and 62%. These layers are homogeneous and follow a random alloy distribution. A growth diagram for InAlN of all indium contents is reported.

Delaminated graphene at silicon carbide facets: atomic scale imaging and spectroscopy.

PubMed

Nicotra, Giuseppe; Ramasse, Quentin M; Deretzis, Ioannis; La Magna, Antonino; Spinella, Corrado; Giannazzo, Filippo

2013-04-23

Atomic-resolution structural and spectroscopic characterization techniques (scanning transmission electron microscopy and electron energy loss spectroscopy) are combined with nanoscale electrical measurements (conductive atomic force microscopy) to study at the atomic scale the properties of graphene grown epitaxially through the controlled graphitization of a hexagonal SiC(0001) substrate by high temperature annealing. This growth technique is known to result in a pronounced electron-doping (∼10(13) cm(-2)) of graphene, which is thought to originate from an interface carbon buffer layer strongly bound to the substrate. The scanning transmission electron microscopy analysis, carried out at an energy below the knock-on threshold for carbon to ensure no damage is imparted to the film by the electron beam, demonstrates that the buffer layer present on the planar SiC(0001) face delaminates from it on the (112n) facets of SiC surface steps. In addition, electron energy loss spectroscopy reveals that the delaminated layer has a similar electronic configuration to purely sp2-hybridized graphene. These observations are used to explain the local increase of the graphene sheet resistance measured around the surface steps by conductive atomic force microscopy, which we suggest is due to significantly lower substrate-induced doping and a resonant scattering mechanism at the step regions. A first-principles-calibrated theoretical model is proposed to explain the structural instability of the buffer layer on the SiC facets and the resulting delamination.

Joint denoising and distortion correction of atomic scale scanning transmission electron microscopy images

NASA Astrophysics Data System (ADS)

Berkels, Benjamin; Wirth, Benedikt

2017-09-01

Nowadays, modern electron microscopes deliver images at atomic scale. The precise atomic structure encodes information about material properties. Thus, an important ingredient in the image analysis is to locate the centers of the atoms shown in micrographs as precisely as possible. Here, we consider scanning transmission electron microscopy (STEM), which acquires data in a rastering pattern, pixel by pixel. Due to this rastering combined with the magnification to atomic scale, movements of the specimen even at the nanometer scale lead to random image distortions that make precise atom localization difficult. Given a series of STEM images, we derive a Bayesian method that jointly estimates the distortion in each image and reconstructs the underlying atomic grid of the material by fitting the atom bumps with suitable bump functions. The resulting highly non-convex minimization problems are solved numerically with a trust region approach. Existence of minimizers and the model behavior for faster and faster rastering are investigated using variational techniques. The performance of the method is finally evaluated on both synthetic and real experimental data.

Investigation of magnetic and structural properties of Ni-Zr co-doped M-type Sr-La hexaferrites

NASA Astrophysics Data System (ADS)

Yang, Yujie; Wang, Fanhou; Shao, Juxiang; Huang, Duohui; Tang, Jin; Rehman, Khalid Mehmood Ur

2018-02-01

In this research, Ni2+ and Zr4+ co-doped Sr-La hexaferrites Sr0.7La0.3Fe12.0-2 x (NiZr) x O19 (0.0 ≤ x ≤ 0.5) were synthesized by the standard ceramic method. The phase identification of the hexaferrites was confirmed by X-ray diffraction analysis. X-ray diffraction analysis showed that all the samples were in single phase M-type hexagonal structure and no impurity phase was observed. Lattice parameters ( c and a) increased with increasing NiZr content ( x) from 0.0 to 0.5. The morphology of the hexaferrites was analyzed by a field emission scanning electron microscopy (FE-SEM). FE-SEM micrographs showed that the grains exhibited hexagonal shape in a plate-like structure with clear grain boundaries. Magnetization properties of the hexaferrites were carried out at room temperature using a physical property measurement system-vibrating sample magnetometer. The values of saturation magnetization ( M s), remanent magnetization ( M r) and coercivity ( H c) were calculated from magnetic hysteresis ( M- H) loops. M s and H c decreased with increasing NiZr content ( x) from 0.0 to 0.5. M r and M r/ M s ratio first increased with increasing NiZr content ( x) from 0.0 to 0.1, and then decreased when NiZr content ( x) ≥ 0.1.

Production of bacterial cellulose using different carbon sources and culture media.

PubMed

Mohammadkazemi, Faranak; Azin, Mehrdad; Ashori, Alireza

2015-03-06

In this work, the effects of carbon sources and culture media on the production and structural properties of bacterial cellulose (BC) have been studied. BC nanofibers were synthesized using Gluconacetobacter xylinus strain PTCC 1734. Media used were Hestrin-Schramm (H), Yamanaka (Y), and Zhou (Z). Five different carbon sources, namely date syrup, glucose, mannitol, sucrose, and food-grade sucrose were used in these media. All the produced BC pellicles were characterized in terms of dry weight production, biomass yield, thermal stability, crystallinity and morphology by thermogravimetric analysis (TGA), x-ray diffraction (XRD), and field emission scanning electron microscopy (FE-SEM). The obtained results showed that mannitol lead to the highest yield, followed by sucrose. The highest production efficiency of mannitol might be due to the nitrogen source, which plays an important role. The maximum improvement on the thermal stability of the composites was achieved when mannitol was used in H medium. In addition, the crystallinity was higher in BC formed in H medium compared to other media. FE-SEM micrographs illustrated that the BC pellicles, synthesized in the culture media H and Z, were stable, unlike those in medium Y that were unstable. The micrographs of BC produced in media containing mannitol and sucrose provided evidence of the strong interfacial adhesion between the BC fibers without noticeable aggregates. Copyright © 2014 Elsevier Ltd. All rights reserved.

A high-sensitivity electrochemical immunosensor based on mobile crystalline material-41-polyvinyl alcohol nanocomposite and colloidal gold nanoparticles.

PubMed

Omidfar, Kobra; Zarei, Hajar; Gholizadeh, Fatemeh; Larijani, Bagher

2012-02-15

A novel competitive immunosensor was developed as a model system using anti-human serum albumin (HSA)-conjugated gold nanoparticles (AuNPs) as an electrochemical label and mobile crystalline material-41 (MCM-41)-polyvinyl alcohol (PVA) mesoporous nanocomposite as an immobilization platform. However, no attempt has yet been made to use the MCM-41 as the supporting electrolyte for the electrosynthesis of nonconducting polymer nanocomposite. This hybrid membrane was evaluated extensively by using field emission scanning electron microscopy (FESEM), cyclic voltammetry (CV), and differential pulse voltammetry (DPV) to determine its physicochemical and electrochemical properties in immunosensor application. FESEM revealed an appropriate and stable attachment between HSA and MCM-41 and also a dense layer deposition of MCM-41-HSA-PVA film onto the electrode surfaces. DPV was developed for quantitative determination of antigen in biological samples. A decrease in DPV responses was observed with increasing concentrations of HSA in standard and real samples. In optimal conditions, this immunosensor based on MCM-41-PVA nanocomposite film could detect HSA in a high linear range (0.5-200 μg ml⁻¹) with a low detection limit of 1 ng ml⁻¹. The proposed method showed acceptable reproducibility, stability, and reliability and could also be applied to detect the other antigens. Copyright © 2011 Elsevier Inc. All rights reserved.

Preparation and Characterization of Polyvinyl Alcohol-Chitosan Composite Films Reinforced with Cellulose Nanofiber

PubMed Central

Choo, Kaiwen; Ching, Yern Chee; Chuah, Cheng Hock; Julai, Sabariah; Liou, Nai-Shang

2016-01-01

In this study microcrystalline cellulose (MCC) was oxidized by 2,2,6,6-tetramethylpiperidine-1-oxyl radical (TEMPO)-mediated oxidation. The treated cellulose slurry was mechanically homogenized to form a transparent dispersion which consisted of individual cellulose nanofibers with uniform widths of 3–4 nm. Bio-nanocomposite films were then prepared from a polyvinyl alcohol (PVA)-chitosan (CS) polymeric blend with different TEMPO-oxidized cellulose nanofiber (TOCN) contents (0, 0.5, 1.0 and 1.5 wt %) via the solution casting method. The characterizations of pure PVA/CS and PVA/CS/TOCN films were performed in terms of field emission scanning electron microscopy (FESEM), tensile tests, thermogravimetric analysis (TGA), Fourier transform infrared spectroscopy (FTIR), and X-ray diffraction (XRD). The results from FESEM analysis justified that low loading levels of TOCNs were dispersed uniformly and homogeneously in the PVA-CS blend matrix. The tensile strength and thermal stability of the films were increased with the increased loading levels of TOCNs to a maximum level. The thermal study indicated a slight improvement of the thermal stability upon the reinforcement of TOCNs. As evidenced by the FTIR and XRD, PVA and CS were considered miscible and compatible owing to hydrogen bonding interaction. These analyses also revealed the good dispersion of TOCNs within the PVA/CS polymer matrix. The improved properties due to the reinforcement of TOCNs can be highly beneficial in numerous applications. PMID:28773763

Effect of substrate surface treatment on electrochemically assisted photocatalytic activity of N-S co-doped TiO2 films

NASA Astrophysics Data System (ADS)

Parada-Gamboa, N. J.; Pedraza-Avella, J. A.; Meléndez, A. M.

2017-01-01

To investigate whether different metal surface treatments, performed on meshes of stainless steel 304 and titanium, affect the photocatalytic activity (PCA) of supported modified anodic TiO2 films, metallic substrates were coated with titanium isopropoxide sol-gel precursor modified with thiourea. Substrates were pretreated by some of the following techniques: a) sandblasting, b) pickling, c) hydroxylation and d) passivation. The as-prepared electrode materials were characterized by X-ray photoelectron spectroscopy (XPS), field emission scanning electron microscopy (FESEM), and voltammetry in the dark and under light UVA irradiation. PCA of modified N-S-TiO2 electrodes was evaluated by electrochemically assisted photocatalytic degradation of methyl orange. The results of XPS revealed that N and S were incorporated into the lattice of TiO2. FESEM showed that surface roughness and thickness of films varies depending on surface treatment. Voltammetric and XPS characterization of N-S co-doped TiO2 films supported on stainless steel revealed that their surface contains alpha-Fe2O3/FeOOH. Accordingly, iron contamination of the films coming from stainless steel was detrimental to the degradation of methyl orange. Prior to sol-gel coating process, sandblasting followed by nitric acid passivation for stainless steel or hydrofluoric acid pickling process in the case of titanium improved the PCA of N-S co-doped TiO2 films.

Eu2+,Dy3+ codoped SrAl2O4 nanocrystalline phosphor for latent fingerprint detection in forensic applications

NASA Astrophysics Data System (ADS)

Sharma, Vishal; Das, Amrita; Kumar, Vinay

2016-01-01

In this work, europium and dysprosium doped strontium aluminate (SrAl2O4:Eu2+,Dy3+) nanophosphor is synthesized and its novel application for the detection of latent fingerprints on various contact surfaces is reported. The SrAl2O4:Eu2+,Dy3+ is synthesized using a combustion method and shows long-lasting afterglow luminescence. The powder particles are characterized using field emission scanning electron microscopy (FE-SEM), SEM-energy dispersive x-ray analysis, x-ray diffraction and photoluminescence spectrophotometry. The FE-SEM image analysis reveals that the nanoparticles are mostly 8-15 nm in size with an irregular spherical shape. This nano-structured powder was applied to fresh and aged fingerprints deposited on porous, semi-porous and non-porous contact surfaces, such as ordinary colored paper, glossy paper, glass, aluminum foil, a yellow foil chocolate wrapper, a soft drink can, a PET bottle, a compact disc and a computer mouse. The results are reproducible and show great sensitivity and high contrast in the developed fingermark regions on these surfaces. These nanophosphor particles also show a strong and long-lasting afterglow property, making them a suitable candidate for use as a fingerprint developing agent on luminescent and highly patterned surfaces. These kinds of powders have shown that they can remove the interference from background luminescence, which is not possible using ordinary luminescent fingerprinting powders.

TiO2-BASED Composite Films for the Photodegradation of Oxytetracycline

NASA Astrophysics Data System (ADS)

Li, Hui; Guan, Ling-Xiao; Feng, Ji-Jun; Li, Fang; Yao, Ming-Ming

2015-02-01

The spread of the antibiotic oxytetracycline (OTC) has been thought as a threat to the safety of drinking water. In this paper, the photocatalytic activity of the nanocrystalline Fe/Ca co-doped TiO2-SiO2 composite film for the degradation of OTC was studied. The films were characterized by field emission scanning electron microscopy (FE-SEM) equipped with energy-dispersive spectroscopy (EDS), N2 adsorption/desorption isotherms, photoluminescence (PL) spectra, and UV-Vis diffraction reflectance absorption spectra (DRS). The FE-SEM results indicated that the Fe/Ca co-doped TiO2-SiO2 film was composed of smaller nanoparticles compared to pure TiO2 or TiO2-SiO2 film. The BET surface area results showed that the specific surface area of the pure TiO2, TiO2-SiO2 and Ca2+/Fe3+ co-doped TiO2-SiO2 is 118.3 m2g-1, 294.3 m2g-1 and 393.7 m2g-1, respectively. The DRS and PL spectra revealed that the Fe/Ca co-doped TiO2-SiO2 film had strong visible light adsorption and diminished electrons/holes recombination. Experimental results showed that the Fe/Ca co-doped TiO2-SiO2 film is effective in the degradation of OTC under both UV and visible light irradiation.

Effect of sintering temperature on physical, structural and optical properties of wollastonite based glass-ceramic derived from waste soda lime silica glasses

NASA Astrophysics Data System (ADS)

Almasri, Karima Amer; Sidek, Hj. Ab Aziz; Matori, Khamirul Amin; Zaid, Mohd Hafiz Mohd

The impact of different sintering temperatures on physical, optical and structural properties of wollastonite (CaSiO3) based glass-ceramics were investigated for its potential application as a building material. Wollastonite based glass-ceramics was provided by a conventional melt-quenching method and followed by a controlled sintering process. In this work, soda lime silica glass waste was utilized as a source of silicon. The chemical composition and physical properties of glass were characterized by using Energy Dispersive X-ray Fluorescence (EDXRF) and Archimedes principle. The Archimedes measurement results show that the density increased with the increasing of sintering temperature. The generation of CaSiO3, morphology, size and crystal phase with increasing the heat-treatment temperature were examined by field emission scanning electron microscopy (FESEM), Fourier transforms infrared reflection spectroscopy (FTIR), and X-ray diffraction (XRD). The average calculated crystal size gained from XRD was found to be in the range 60 nm. The FESEM results show a uniform distribution of particles and the morphology of the wollastonite crystal is in relict shapes. The appearance of CaO, SiO2, and Ca-O-Si bands disclosed from FTIR which showed the formation of CaSiO3 crystal phase. In addition to the calculation of the energy band gap which found to be increased with increasing sintering temperature.

Temperature dependent dielectric relaxation and ac-conductivity of alkali niobate ceramics studied by impedance spectroscopy

NASA Astrophysics Data System (ADS)

Yadav, Abhinav; Mantry, Snigdha Paramita; Fahad, Mohd.; Sarun, P. M.

2018-05-01

Sodium niobate (NaNbO3) ceramics is prepared by conventional solid state reaction method at sintering temperature 1150 °C for 4 h. The structural information of the material has been investigated by X-ray diffraction (XRD) and Field emission scanning electron microscopy (FE-SEM). The XRD analysis of NaNbO3 ceramics shows an orthorhombic structure. The FE-SEM micrograph of NaNbO3 ceramics exhibit grains with grain sizes ranging between 1 μm to 5 μm. The surface coverage and average grain size of NaNbO3 ceramics are found to be 97.6 % and 2.5 μm, respectively. Frequency dependent electrical properties of NaNbO3 is investigated from room temperature to 500 °C in wide frequency range (100 Hz-5 MHz). Dielectric constant, ac-conductivity, impedance, modulus and Nyquist analysis are performed. The observed dielectric constant (1 kHz) at transition temperature (400 °C) are 975. From conductivity analysis, the estimated activation energy of NaNbO3 ceramics is 0.58 eV at 10 kHz. The result of Nyquist plot shows that the electrical behavior of NaNbO3 ceramics is contributed by grain and grain boundary responses. The impedance and modulus spectrum asserts that the negative temperature coefficient of resistance (NTCR) behavior and non-Debye type relaxation in NaNbO3.

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

NASA Astrophysics Data System (ADS)

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

2018-03-01

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

Effects of silica and zinc oxide doping on mechanical and biological properties of 3D printed tricalcium phosphate tissue engineering scaffolds.

PubMed

Fielding, Gary A; Bandyopadhyay, Amit; Bose, Susmita

2012-02-01

To evaluate the effects of silica (SiO(2)) (0.5 wt%) and zinc oxide (ZnO) (0.25 wt%) dopants on the mechanical and biological properties of tricalcium phosphate (TCP) scaffolds with three dimensionally (3D) interconnected pores. Scaffolds were created with a commercial 3D printer. Post sintering phase analysis was determined by X-ray diffraction. Surface morphology of the scaffolds was examined by field emission scanning electron microscopy (FESEM). Mechanical strength was evaluated with a screw driven universal testing machine. MTT assay was used for cellular proliferation characteristics and cellular morphology was examined by FESEM. Addition of dopants into TCP increased the average density of pure TCP from 90.8 ± 0.8% to 94.1 ± 1.6% and retarded the β to α phase transformation at high sintering temperatures, which resulted in up to 2.5 fold increase in compressive strength. In vitro cell-materials interaction studies, carried out using hFOB cells, confirmed that the addition of SiO(2) and ZnO to the scaffolds facilitated faster cell proliferation when compared to pure TCP scaffolds. Addition of SiO(2) and ZnO dopants to the TCP scaffolds showed increased mechanical strength as well as increased cellular proliferation. Copyright © 2011 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Characterisation of rheology and microstructures of κ-carrageenan in ethanol-water mixtures.

PubMed

Yang, Zhi; Yang, Huijuan; Yang, Hongshun

2018-05-01

The effects of ethanol (up to 20 wt%) on the rheological properties and structural characteristics of κ-carrageenan gel were investigated by Field Emission Scanning Electron Microscopy (FESEM) and Small Angle X-ray Scattering (SAXS). Both the sol-gel and gel-sol transition temperatures shifted to higher degree (from 36.8 ± 0.5 to 52.5 ± 1.4 °C and from 51.2 ± 0.6 to 67.0 ± 0.5 °C, respectively) upon 20 wt% ethanol addition (P < 0.05). The critical relaxation exponent n and the critical gel strength S g obtained from Winter-Chambon criterion decreased and increased, respectively as the ethanol concentration increased. The κ-carrageenan gel was formed due to the formation of fibrillar networks, and the fibrillar density increased upon ethanol addition via FESEM. Moreover, upon 20 wt% ethanol addition, the average radius of gyration of κ-carrageenan strand increased from 1.18 ± 0.03 of control to 1.55 ± 0.02 nm by SAXS. A mechanism underlying the effect of ethanol on the κ-carrageenan gelation was proposed based on coil to double helix transition followed by the helix aggregation. Copyright © 2018 Elsevier Ltd. All rights reserved.

Microstructure control of SOFC cathode material: The role of dispersing agent

NASA Astrophysics Data System (ADS)

Ismail, Ismariza; Jani, Abdul Mutalib Md; Osman, Nafisah

2017-09-01

In the present works, La0.6Sr0.4Co0.2Fe0.8O3-δ (LSCF) cathode powders were synthesized by a sol-gel method with the aid of ethylene glycol which served as the dispersing agent. The phase formation and morphology of the powders were examined by X-Ray diffractometer (XRD) and field emission scanning electron microscopy (FESEM), respectively. The electrochemical properties of the synthesized cathode were obtained using an electrochemical impedance spectroscopy (EIS). The characteristic peaks for LSCF phase appears in the X-ray diffractogram after calcined at 500 °C and complete formation of LSCF single phase was attained at 700 °C. FESEM micrographs showed the presence of spherical particles of the powders with approximate particle size between 10 to 60 nm along with agglomerate morphologies. Well dispersed particles and fewer aggregates were observed for samples prepared with addition of ethylene glycol as the synthesizing aid. The surface area obtained for powder sample prepared with the aid of dispersing agent is 12.0 m2g-1. The EIS measurement results depicts a lower area specific resistance (ASR) obtained for sample prepared with addition of the ethylene glycol as compared to the pristine sample. The present results encourage the optimization of the cathode particle design in order to further improve the cathode performance.

Nanoscale quantification of intracellular element concentration by X-ray fluorescence microscopy combined with X-ray phase contrast nanotomography

NASA Astrophysics Data System (ADS)

Gramaccioni, Chiara; Yang, Yang; Procopio, Alessandra; Pacureanu, Alexandra; Bohic, Sylvain; Malucelli, Emil; Iotti, Stefano; Farruggia, Giovanna; Bukreeva, Inna; Notargiacomo, Andrea; Fratini, Michela; Valenti, Piera; Rosa, Luigi; Berlutti, Francesca; Cloetens, Peter; Lagomarsino, Stefano

2018-01-01

We present here a correlative X-ray microscopy approach for quantitative single cell imaging of molar concentrations. By combining the elemental content provided by X-ray fluorescence microscopy and the morphology information extracted from X-ray phase nanotomography, we determine the intracellular molarity distributions. This correlative method was demonstrated on a freeze-dried human phagocytic cell to obtain the absolute elemental concentration maps of K, P, and Fe. The cell morphology results showed a very good agreement with atomic-force microscopy measurements. This work opens the way for non-destructive single cell chemical analysis down to the sub-cellular level using exclusively synchrotron radiation techniques. It will be of high interest in the case where it is difficult to access the morphology using atomic-force microscopy, for example, on frozen-hydrated cells or tissues.

Incorporation of multilayered silver nanoparticles into polymer brushes as 3-dimensional SERS substrates and their application for bacteria detection

NASA Astrophysics Data System (ADS)

Zhang, Qian; Wang, Xiang-Dong; Tian, Ting; Chu, Li-Qiang

2017-06-01

Surface-enhanced Raman scattering (SERS) sensors have been extensively studied for ultrasensitive detection of diverse chemical or biological analytes. Facile fabrication of highly sensitive SERS substrates is believed to be of crucial importance in these analytical applications. In this regard, the preparation of 3-dimensional (3D) SERS substrates are explored via the incorporation of multilayered silver nanoparticles (AgNPs) into poly (oligo(ethylene glycol) methacrylate) (POEGMA) brushes by repeating the immersion-rinsing-drying steps for different lengths of time (i.e., the so-called in-stacking method). The POEGMA brushes of different chain lengths are synthesized by surface-initiated atom transfer radical polymerization (ATRP) with various reaction time. The resulting POEGMA/AgNP nanocomposites are characterized by FE-SEM, UV-vis and Raman spectroscopy. FE-SEM and UV-vis results indicate that the AgNPs are successfully incorporated into the POEGMA brushes with a 3D configuration. The nanocomposite films are employed as SERS substrates for the detection of a Raman reporter molecule (i.e., 4-aminothiophenol), giving rise to an enhancement factor of up to 1.29 × 107 and also having relatively good uniformity and reproducibility. The obtained 3D SERS substrates are also used for the detection of a typical gram-positive bacterium, Staphylococcus aureus. The limit of detection is found to be as low as ca. 8 CFU/mL.

Insights into radiation damage from atomic resolution scanning transmission electron microscopy imaging of mono-layer CuPcCl16 films on graphene.

PubMed

Mittelberger, Andreas; Kramberger, Christian; Meyer, Jannik C

2018-03-19

Atomically resolved images of monolayer organic crystals have only been obtained with scanning probe methods so far. On the one hand, they are usually prepared on surfaces of bulk materials, which are not accessible by (scanning) transmission electron microscopy. On the other hand, the critical electron dose of a monolayer organic crystal is orders of magnitudes lower than the one for bulk crystals, making (scanning) transmission electron microscopy characterization very challenging. In this work we present an atomically resolved study on the dynamics of a monolayer CuPcCl 16 crystal under the electron beam as well as an image of the undamaged molecules obtained by low-dose electron microscopy. The results show the dynamics and the radiation damage mechanisms in the 2D layer of this material, complementing what has been found for bulk crystals in earlier studies. Furthermore, being able to image the undamaged molecular crystal allows the characterization of new composites consisting of 2D materials and organic molecules.

Scanning superlens microscopy for non-invasive large field-of-view visible light nanoscale imaging

NASA Astrophysics Data System (ADS)

Wang, Feifei; Liu, Lianqing; Yu, Haibo; Wen, Yangdong; Yu, Peng; Liu, Zhu; Wang, Yuechao; Li, Wen Jung

2016-12-01

Nanoscale correlation of structural information acquisition with specific-molecule identification provides new insight for studying rare subcellular events. To achieve this correlation, scanning electron microscopy has been combined with super-resolution fluorescent microscopy, despite its destructivity when acquiring biological structure information. Here we propose time-efficient non-invasive microsphere-based scanning superlens microscopy that enables the large-area observation of live-cell morphology or sub-membrane structures with sub-diffraction-limited resolution and is demonstrated by observing biological and non-biological objects. This microscopy operates in both non-invasive and contact modes with ~200 times the acquisition efficiency of atomic force microscopy, which is achieved by replacing the point of an atomic force microscope tip with an imaging area of microspheres and stitching the areas recorded during scanning, enabling sub-diffraction-limited resolution. Our method marks a possible path to non-invasive cell imaging and simultaneous tracking of specific molecules with nanoscale resolution, facilitating the study of subcellular events over a total cell period.

Noncontact atomic force microscopy in liquid environment with quartz tuning fork and carbon nanotube probe

NASA Astrophysics Data System (ADS)

Kageshima, Masami; Jensenius, Henriette; Dienwiebel, Martin; Nakayama, Yoshikazu; Tokumoto, Hiroshi; Jarvis, Suzanne P.; Oosterkamp, Tjerk H.

2002-03-01

A force sensor for noncontact atomic force microscopy in liquid environment was developed by combining a multiwalled carbon nanotube (MWNT) probe with a quartz tuning fork. Solvation shells of octamethylcyclotetrasiloxane on a graphite surface were detected both in the frequency shift and dissipation. Due to the high aspect ratio of the CNT probe, the long-range background force was barely detectable in the solvation region.

Mapping of Proteomic Composition on the Surfaces of Bacillus spores by Atomic Force Microscopy-based Immunolabeling

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

Plomp, M; Malkin, A J

2008-06-02

Atomic force microscopy provides a unique capability to image high-resolution architecture and structural dynamics of pathogens (e.g. viruses, bacteria and bacterial spores) at near molecular resolution in native conditions. Further development of atomic force microscopy in order to enable the correlation of pathogen protein surface structures with specific gene products is essential to understand the mechanisms of the pathogen life cycle. We have applied an AFM-based immunolabeling technique for the proteomic mapping of macromolecular structures through the visualization of the binding of antibodies, conjugated with nanogold particles, to specific epitopes on Bacillus spore surfaces. This information is generated while simultaneouslymore » acquiring the surface morphology of the pathogen. The immunospecificity of this labeling method was established through the utilization of specific polyclonal and monoclonal antibodies that target spore coat and exosporium epitopes of Bacillus atrophaeus and Bacillus anthracis spores.« less