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1.
In this work, the fungus Penicillium was used for rapid extra-/intracellular biosynthesis of gold nanoparticles. AuCl4 ions reacted with the cell filtrate of Penicillium sp. resulting in extracellular biosynthesis of gold nanoparticles within 1 min. Intracellular biosynthesis of gold nanoparticles was obtained by incubating AuCl4 solution with fungal biomass for 8 h. The gold nanoparticles were characterized by means of visual observation, UV–Vis absorption spectroscopy, X-ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM), and energy-dispersive X-ray spectroscopy (EDX). The extracellular nanoparticles exhibited maximum absorbance at 545 nm in UV–Vis spectroscopy. The XRD spectrum showed Bragg reflections corresponding to the gold nanocrystals. TEM exhibited the formed spherical gold nanoparticles in the size range from 30 to 50 nm with an average size of 45 nm. SEM and TEM revealed that the intracellular gold nanoparticles were well dispersed on the cell wall and within the cell, and they are mostly spherical in shape with an average diameter of 50 nm. The presence of gold was confirmed by EDX analysis.  相似文献   

2.
We report an efficient process for preparing monodisperse SiO2@Y0.95Eu0.05VO4 core–shell phosphors using a simple citrate sol–gel method and without the use of surface-coupling silane agents or large stabilizers. X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM), and photoluminescence (PL) spectra were used to characterize the resulting SiO2@Y0.95Eu0.05VO4 core–shell phosphors. The XRD results demonstrate that the Y0.95Eu0.05VO4 particles crystallization on the surface of SiO2 annealing at 800 °C is perfectly and the crystallinity increases with raising the annealing temperature. The obtained core–shell phosphors have a near perfect spherical shape with narrow size distribution (average size ca. 500 nm and an average thickness of ~50 nm), are not agglomerated, and have a smooth surface. The thickness of the YVO4:Eu3+ shells on the SiO2 cores could be easily tailored by changing the mass ratio of shell to core (W = [YVO4]/[SiO2]) (~50 nm for W = 30%). The Eu3+ shows a strong PL luminescence (dominated by 5D0 − 7F2 red emission at 618 nm) under the excitation of 320 nm UV light. The PL intensity of Eu3+ increases with increasing the annealing temperature and the values of W.  相似文献   

3.
A flower-like boehmite nanostructure was prepared through a template-free chemical route by the self-assembly process of nanosize petals 800–1000 nm long, 200–250 nm wide, 20–50 nm thick and having an average crystallite size of about 2.21 nm. X-ray diffraction analysis (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM), DTA/TGA analyses and Brunauer–Emmet–Teller (BET-N2) analyses were used in order to characterize the product obtained. XRD results exhibited that the obtained nanostructures composed of pure orthorhombic AlOOH phase. The effects of Cl ions and TEA on the growth of boehmite three-dimensional nanoarchitectures in the presence of NO3-\mathrm{NO}_{3}^{-} ions were investigated. BET analyses of as-prepared material demonstrate that this nanostructure material has a high specific surface area, as high as 123 m2 g−1.  相似文献   

4.
Microporous (TiO2) x –(SiO2)100 − x (0 < x < 40) xerogels have been produced by sol–gel methods either by partial pre-hydrolysis or reflux of tetraethoxysilane and titanium isopropoxide. These have been characterised by 29Si nuclear magnetic resonance, X-ray diffraction, EXAFS at the Ti–K edge, X-ray photoelectron spectroscopy, temperature-programmed reduction, FT infrared, N2 adsorption at 78 K (BET), transmission electron microscopy and dynamic light scattering (DLS). These were dip coated onto fused silica and characterised by atomic force microscopy and UV–visible absorption. Their photoactivity in removal of alkylphenol ethoxylate TX100 from water was less than for less porous titania. The advantages of including thermally removable PEG or PPG templates in terms of increasing surface, meso-porosity and photon absorbance at visible wavelengths to give nanoengineered photocatalytic films are described.  相似文献   

5.
Diluted magnetic semiconductor (DMS) nanoparticles of Sn1−x Er x O2 (x = 0.0, 0.02, 0.04, and 0.1) were prepared by sol–gel method. The X-ray diffraction patterns showed SnO2 rutile structure for all samples with no impurity peaks. The decrease in crystallite size with Er concentration was confirmed from TEM measurements (from 12 to 4 nm). The UV–Visible absorption spectra of Er-doped SnO2 nanoparticles showed blue shift in band gap compared to undoped SnO2. The electron spin resonance analysis of Er-doped SnO2 nanoparticles indicate Er3+ in a rutile lattice and also decrease in intensity with Er concentration above x = 0.02. Temperature-dependent magnetization studies and the inverse susceptibility curves indicated increased antiferromagnetic interaction with Er concentration.  相似文献   

6.
The preparation and application of rod-shaped core–shell structured Fe3O4–Au nanoparticles for immunomagnetic separation and sensing were described for the first time with this study. To synthesize magnetic gold nanorod particles, the seed-mediated synthetic method was carried out and the resulting nanoparticles were characterized with transmission electron microscopy (TEM), ultraviolet visible spectroscopy (UV–Vis), energy-dispersive X-ray (EDX), and X-ray diffraction (XRD). Magnetic properties of the nanoparticles were also examined. Characterization of the magnetic gold nanorod particles has proven that the resulting nanoparticles were composed of Fe3O4 core and the gold shell. The rod-shaped gold-coated iron nanoparticles have an average diameter of 16 ± 2 nm and an average length of about 50 ± 5 nm (corresponding aspect ratio of 3). The saturation magnetization value for the magnetic gold nanorod particles was found to be 37 emu/g at 300 K. Rapid and room temperature reaction synthesis of magnetic gold nanorod particles and subsequent surface modification with E. coli antibodies provide immunomagnetic separation and SERS application. The analytical performance of the SERS-based homogenous sandwich immunoassay system with respect to linear range, detection limit, and response time is also presented.  相似文献   

7.
A simple hydrothermal process has been proposed to systematically synthesize europium-doped yttrium phosphate-vanadates with general formula YV1 − xPxO4:Eu3+ (x = 0–1.0). All the YV1 − xPxO4:Eu3+ products were characterized by x-ray diffraction (XRD) and transmission electron microscopy (TEM), the results of which revealed they were single-phase tetragonal-structured nanocrystals with diameter of 20 nm and their cell parameter a exhibited a linear relationship with the x value. Photoluminescence (PL) excitation and emission intensities of the products were sensitive to the x value and the change of the PL intensity with x was a wave-like curve which reached the peak at x = 0.4 and 0.8. In addition, the x value had an obvious influence on the (5D07F2)/(5D07F1) intensity ratio of Eu3+.  相似文献   

8.
A series of stoichiometric and nonstoichiometric copper–chalcogenide nanocrystallines with different morphologies, e.g., extremely high aspect ratio nanofibers (Cu9S8), tubular structure (Cu x S (x=∼1.86–1.96), nanorods (CuS, Cu31S16), platelets (β-CuSe, Cu3Se2), rope-like Cu3Se2, as well as spherical nanoparticles (Cu7Se4, Cu2−x Se), have been successfully synthesized in 20 vol% water and 80 vol% organic solvents mixture under mild conditions. The products were characterized by various techniques, including X-ray powder diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), electronic diffraction (ED), and high-resolution transmission electron microscopy (HRTEM). The studies of the optical properties revealed that the copper chalcogenides have a wide absorption in the range of about 400–700 nm, with accessional IR band. Systematic studies showed that the mixture of 20 vol% water and 80 vol% organic solvents played a key role in controlling the copper chalcogenides with different morphologies and phases.  相似文献   

9.
N. Osman  A. M. Jani  I. A. Talib 《Ionics》2006,12(6):379-384
This study was aimed to synthesize a ceramic electrolyte of BaCe0.76Zr0.19Yb0.05O2.975 using acetate and chloride precursors. The transparent sol was stable for more than 10 months but only 3 months for the gel. The dried gel was characterized using thermogravimetric analysis/differential scanning calorimetry, particle analyzer, X-ray diffraction (XRD), and scanning electron microscopy/dispersive X-ray (SEM/EDX) analysis. Thermal behavior analysis showed three steps of weight losses. All the processes were exothermic reactions as shown by derivative thermogravimetric analysis signal. Two groups of particle size were observed in the particle size distribution for the sample in the form of sol and powders ranging from 100 to 1,100 nm. A high purity single-phase sample with orthorhombic structure was identified by XRD. The theoretical density estimated from the unit cell parameters was 6.40 g cm−3. SEM of the powdered sample showed homogeneous distribution of particles and the grains size were in the range of 0.7–1.3 μm. EDX data revealed that the residue of small amount of chloride (≈0.25%) was still present in the final product of the compound.  相似文献   

10.
In this paper, data concerning the effect of pH on the morphology of Ag–TiO2 nanocomposite during photodeposition of Ag on TiO2 nanoparticles is reported. TiO2 nanoparticles prepared by sol–gel method were coated with Ag by photodeposition from an aqueous solution of AgNO3 at various pH levels ranging from 1 to 10 in a titania sol, under UV light. The as-prepared nanocomposite particles were characterized by UV–vis absorption spectroscopy, transmission electron microscopy (TEM), X-ray diffraction (XRD), and N2 adsorption/desorption method at liquid nitrogen temperature (−196 °C) from Brunauer–Emmett–Teller (BET) measurements. It is shown that at a Ag loading of 1.25 wt.% on TiO2, a high-surface area nanocomposite morphology corresponding to an average of one Ag nanoparticle per titania nanoparticle was achieved. The diameter of the titania crystallites/particles were in the range of 10–20 nm while the size of Ag particles attached to the larger titania particles were 3 ± 1 nm as deduced from crystallite size by XRD and particle size by TEM. Ag recovery by photo harvesting from the solution was nearly 100%. TEM micrographs revealed that Ag-coated TiO2 nanoparticles showed a sharp increase in the degree of agglomeration for nanocomposites prepared at basic pH values, with a corresponding sharp decrease in BET surface area especially at pH > 9. The BET surface area of the Ag–TiO2 nanoparticles was nearly constant at around a value of 140 m2 g−1 at all pH from 1–8 with an anomalous maximum of 164 m2 g−1 when prepared from a sol at pH of 4, and a sharp decrease to 78 m2 g−1 at pH of 10.  相似文献   

11.
The production of low-dimensional nanoparticles (NPs) with appropriate surface modification has attracted increasing attention in biological, biochemical, and environmental applications including chemical sensing, photocatalytic degradation, separation, and purification of toxic molecules from the matrices. In this study, iron oxide NPs have been prepared by hydrothermal method using ferric chloride and urea in aqueous medium under alkaline condition (pH 9 ~ 10). As-grown low-dimensional NPs have been characterized by UV–vis spectroscopy, FT-IR, X-ray diffraction, Field emission scanning electron microscopy, Raman spectroscopy, High-resolution Transmission electron microscopy, and Electron Diffraction System. The uniformity of the NPs size was measured by the scanning electron microscopy, while the single phase of the nanocrystalline β-Fe2O3 was characterized using powder X-ray diffraction technique. As-grown NPs were extensively applied for the photocatalytic degradation of acridine orange (AO) and electrochemical sensing of ammonia in liquid phase. Almost 50% photo-catalytic degradation with AO was observed in the presence of UV sources (250 W) with NPs. β-Fe2O3 NP-coated gold electrodes (GE, surface area 0.0216 cm2) have enhanced ammonia-sensing performances in their electrical response (IV characterization) for detecting ammonia in liquid phase. The performances of chemical sensor were investigated, and the results exhibited that the sensitivity, stability, and reproducibility of the sensor improved significantly using β-Fe2O3 NPs on GE surface. The sensitivity was approximately 0.5305 ± 0.02 μAcm−2mM−1, with a detection limit of 21.8 ± 0.1 μM, based on a signal/noise ratio of 3 with short response time.  相似文献   

12.
SrZr1−x Y x O3 coatings were co-sputtered from metallic Zr–Y (84–16 at.%) and Sr targets in the presence of a reactive argon–oxygen gas mixture. The structural and chemical features of the film have been assessed by X-ray diffraction and scanning electron microscopy. The electrical properties have been investigated for different substrates by Complex Impedance Spectroscopy as a function of crystalline state, temperature and atmosphere. The as-deposited coatings are amorphous and crystallise after annealing at 673 K for 2 h under air. The stabilisation of the perovskite structure is a function of the nominal composition. The films are dense and present a good adhesion on different substrates. Crystallisation and mechanical stresses are detected by alternating current (AC) impedance spectroscopy. Significant ionic conductivity in the 473–823 K temperature range is evidenced in air. Two different conduction regimes in the presence of steam are attributed to a modification of the charge carrier nature. In spite of low conductivity values (σ ~10−6 S.cm−1 at 881 K), the activation energies are in agreement with that of Y-doped strontium zirconate ceramics (~0.7 eV in air).  相似文献   

13.
Polycrystalline samples of Pr1−x Sr x Fe0.8Co0.2 O3−δ (x=0.1, 0.2, 0.3) (PSFC) were prepared by the combustion synthesis route at 1200°C. The structure of the polycrystalline powders was analysed with X-ray powder diffraction data. The X-ray diffraction (XRD) patterns were indexed as the orthoferrite similar to that of PrFeO3 having a single-phase orthorhombic perovskite structure (Pbnm). Pr1−x Sr x Fe0.8Co0.2O3−δ (x=0.1, 0.2, 0.3) films have been deposited on yttria-stabilized zirconia (YSZ) single-crystal substrates at 700°C by pulsed laser deposition (PLD) for application to thin film solid oxide fuel cell cathodes. The structure of the films was analysed by XRD, scanning electron microscopy (SEM) and atomic force microscopy (AFM). All films are polycrystalline with a marked texture and present pyramidal grains in the surface with different size distributions. Electrochemical impedance spectroscopy (EIS) measurements of PSFC/YSZ single crystal/PSFC test cells were conducted. The Pr0.7Sr0.3Fe0.8Co0.2O3−δ film at 850°C presents a lower area specific resistance (ASR) value, 1.65 Ω cm2, followed by the Pr0.8Sr0.2Fe0.8Co0.2O3−δ (2.29 Ω cm2 at 850°C) and the Pr0.9Sr0.1Fe0.8Co0.2O3−δ films (5.45 Ω cm2 at 850°C).  相似文献   

14.
A new method to produce elaborate nanostructure with magnetic and fluorescent properties in one entity is reported in this article. Magnetite (Fe3O4) coated with fluorescent silica (SiO2) shell was produced through the one-pot reaction, in which one reactor was utilized to realize the synthesis of superparamagnetic core of Fe3O4, the formation of SiO2 coating through the condensation and polymerization of tetraethylorthosilicate (TEOS), and the encapsulation of tetramethyl rhodamine isothiocyanate-dextran (TRITC-dextran) within silica shell. Transmission electron microscopy (TEM), energy dispersive X-ray (EDX) analysis, and X-ray diffraction (XRD) were carried out to investigate the core–shell structure. The magnetic core of the core–shell nanoparticles is 60 ± 10 nm in diameter. The thickness of the fluorescent SiO2 shell is estimated at 15 ± 5 nm. In addition, the fluorescent signal of the SiO2 shell has been detected by the laser confocal scanning microscopy (LCSM) with emission wavelength (λem) at 566 nm. In addition, the magnetic properties of TRITC-dextran loaded silica-coating iron oxide nanoparticles (Fe3O4@SiO2 NPs) were studied. The hysteresis loop of the core–shell NPs measured at room temperature shows that the saturation magnetization (M s) is not reached even at the field of 70 kOe (7T). Meanwhile, the very low coercivity (H c) and remanent magnetization (M r) are 0.375 kOe and 6.6 emu/g, respectively, at room temperature. It indicates that the core–shell particles have the superparamagnetic properties. The measured blocking temperature (T B) of the TRITC-dextran loaded Fe3O4@SiO2 NPs is about 122.5 K. It is expected that the multifunctional core–shell nanoparticles can be used in bio-imaging.  相似文献   

15.
Nano-sized Al3+-doped V2O5 cathode materials, Al0.2V2O5.3−δ , were prepared by an oxalic acid assisted sol–gel method at 350 °C (sample A) and 400 °C (sample B). X-ray diffraction confirmed that samples A and B were pure phase Al0.2V2O5.3−δ with an orthorhombic structure close to that of V2O5. Scanning electron microscopy showed that sample A was in nanoscale with a mean particle size about 50 nm. Cyclic voltammetry showed the good electrochemical and structural reversibility of the Al0.2V2O5.3−δ nanoparticles during the Li+ insertion/extraction process. The Al0.2V2O5.3−δ nanoparticles exhibited excellent charge–discharge cycling performance and rate capability compared to that of bulky V2O5 electrodes. For instance, the materials delivered a reversible specific capacity about 180 mAh g−1 (sample A) and 150 mAh g−1 (sample B), in the potential window of 4.0–2.0 V at the current density of 150 mA g−1. The Al0.2V2O5.3−δ nanoparticles in particular showed almost no capacity fading for at least 50 cycles.  相似文献   

16.
Zn/Fe oxide compound powders were obtained by the hydrothermal method using ferric nitrate Fe(NO3)3·9H2O and zinc nitrate Zn(NO3)2·6H2O at 200 °C and different precursor molar ratios x = Fe3+/Zn2+ equal to 2.8/0.2, 2.5/0.5, 1.8/1.2 and 1.5/1.5. The samples were characterized by X-ray diffraction (XRD) and scanning electron microscopy/energy dispersive X-ray analysis (SEM–EDAX). Room temperature measurements of the frequency dependence of the complex magnetic permeability and complex dielectric permittivity, over the frequency range from 0.1 to 6 GHz, were performed. For precursor molar ratios x = 2.8/0.2, x = 1.8/1.2 and x = 1.5/1.5 the obtained samples showed a ferromagnetic-like resonance behaviour. This behaviour was assigned to the prevalent compounds in the obtained samples, Fe2O3 (for x = 2.8/0.2) and ZnFe2O4 (for x = 1.8/1.2 and x = 1.5/1.5). Based on the magnetic and dielectric measurements, the microwave absorbent properties of the four samples were analysed, and the sample containing mostly of ZnFe2O4 (for x = 1.8/1.2) was found to be the best electromagnetic absorber in the frequency range 1.36–6 GHz.  相似文献   

17.
Sr1−x La x Zn x Fe12−x O19/poly(vinylpyrrolidone) (PVP) (0.0≤x≤0.5) precursor nanofibers were prepared by the sol–gel assisted electrospinning method from starting reagents of metal salts and PVP. Subsequently, the Sr1−x La x Zn x Fe12−x O19 nanofibers with diameters of around 100 nm were obtained by calcination of the precursor at 800 to 1000°C for 2 h. The precursor and resultant Sr1−x La x Zn x Fe12−x O19 nanofibers were characterized by X-ray diffraction, scanning electron microscopy, energy-dispersive X-ray spectrometer and vibrating sample magnetometer. The grain sizes of Sr0.8La0.2Zn0.2Fe11.8O19 nanofibers are in a nanoscale from 40 to 48 nm corresponding to the calcination temperature from 800 to 1000°C. With La–Zn substitution content increase from 0 to 0.5, the grain size and lattice constants for the Sr1−x La x Zn x Fe12−x O19 nanofibers obtained at 900°C show a steady reduction trend. With variations of the ferrite particle size arising from the La–Zn substitution, the nanofiber morphology changes from the necklace-like structure linking by single elongated plate-like particles to the structure building of multi-particles on the nanofiber cross-section. The specific saturation magnetization of Sr1−x La x Zn x Fe12−x O19 nanofibers initially increases with the La–Zn content, reaching a maximum value 72 A m2 kg−1 at x=0.2, and then decreases with a further La–Zn content increase up to x=0.5, while the coercivity exhibits a continuous reduction from 413 (x=0) to 219 kA m−1 (x=0.5). The mechanism for the La–Zn substitution and the nanofiber magnetic property are analyzed.  相似文献   

18.
Wei Yuan  Ji Yan  Zhiyuan Tang  Li Ma 《Ionics》2012,18(3):329-335
A novel ultrasonic-assisted sol–gel method is proposed to prepare Li3V2(PO4)3/C cathode material. X-ray diffraction analyses show that both Li3V2(PO4)3/C(A) synthesized by the ultrasonic-assisted sol–gel method and Li3V2(PO4)3/C(B) synthesized by a traditional sol–gel method have monoclinic structure. Scanning electron microscopy images indicate that the Li3V2(PO4)3/C(A) composite has a more uniform morphology than that of the Li3V2(PO4)3/C(B) composite. In the voltage range of 3.0–4.3 V (vs. Li/Li+), the initial specific discharge capacities of the Li3V2(PO4)3/C(A) and Li3V2(PO4)3/C(B) samples are 129.8 and 125.9 mAh g−1 at 1C rate (1C = 133 mA g−1), respectively. Furthermore, at 2-C charge/10-C discharge rate, the specific discharge capacity of the Li3V2(PO4)3/C(A) composite retains 113.2 mAh g−1 after 50 cycles, but the Li3V2(PO4)3/C(B) composite only presents a capacity of 94.8 mAh g−1.  相似文献   

19.
A simple solvothermal method for the selective synthesis of β-HgS (meta cinnabar) nanoparticles in aqueous solutions is reported with bis(dibenzyldithiocarbamato)mercury(II) as the precursor. Crystal structure, size, morphology and composition of the products are characterized by X-ray powder diffraction (XRD), scanning electron microscopy (SEM), energy-dispersive X-ray (EDX) analysis, high-resolution transmission electron microscopy (HRTEM), SAED and X-ray photoelectron spectroscopy (XPS). PXRD shows (111), (220), (200), (311), (222), (400), (331), (420) reflections characteristic of β-HgS. SEM micrographs display the spherical nature of the nano-β-HgS. EDX analysis showed the presence of Hg and S. HRTEM images indicate the spherical nature of the nanoparticles with their size in the range of 10–15 nm and the FFT pattern shows the crystalline nature of the spherical particles. The results are in agreement with those estimated from the XRD pattern. XPS signals observed at 162.6 and 162.8 eV are due to S2p 3/2 and S2p 1/2 electrons and the S2s was observed at 222.3 eV. The band gap of nano-β-HgS has been found to be 3.6 eV from the UV–visible spectral measurement. The blue-shifted band gap compared to the bulk HgS is a consequence of “size quantization” effect. A comprehensive characterization of the precursor by IR and single crystal X-ray crystallography shows the presence of HgS4 coordination environment, with a distinct Hg–S bond asymmetry.  相似文献   

20.
In this work, ZnO thin films have been prepared by spray pyrolysis deposition method on the glass substrates. The effect of deposition parameters, such as deposition rate, substrate temperature and solution volume has been studied by X-ray diffraction (XRD) method, UV–Vis–NIR spectroscopy, scanning electron microscopy (SEM), and electrical measurements. The XRD patterns indicate polycrystalline wurtzite structure with preferred direction along (0 0 2) planes. Thin films have transparency around 90% in the visible range. The optical band gap was determined at 3.27 eV which did not change significantly. Evolution of electrical results containing the carriers’ density, sheet resistance and resistivity are in agreement with structural results. All the results suggest the best deposition parameters are: deposition rate, R = 3 ml/min, substrate temperature, T s = 450°C and thickness of the thin films t = 110–130 nm.  相似文献   

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