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1.
In this paper we report results of both, material preparation and magnetic characterisation, on CoFe2O4 particles of nanometric size formed by in‐situ precipitation within polymer gels. The size of the particles was controlled within a very narrow volume distribution and its average value was shifted from 2 to 10 nm. The existence of nanoparticles showing, at room temperature, coercive field values between 500 and 900 Oe and saturation magnetisations of about 500 emu/cm3, suggest to use these systems to get magnetic recording media with ultra high density. Poly(vinyl alcohol) (PVA) and Polystyrene (PS) films were prepared from this nanocomposite material. After a magnetic field treatment nanoparticles within the PVA films are free to rotate in response to an applied magnetic field. This PVA based nanocomposite film portends a new class of magnetic material with very little or no electrical and magnetic loss.  相似文献   

2.
The structure and properties of hematite particles obtained by hydrolysis of ferric chloride solution doped with various kinds of amines were examined by TEM, XRD, TG-DTA, N2and H2O adsorption, and zeta potential measurements. The shape of precipitates was concentration dependent; they changed from large spheres (diameter: ca. 820 nm) to cubes (edge length: ca. 400 nm) via double-spheres (long axis length: ca. 600 nm) with increasing monoamine concentrations. This effect was enhanced by increasing their pKavalues. Much pronounced effects of di- and triamines on the particle formation were observed; cubic and double-spherical particles were obtained at a much lower concentration of di- and triamines and small spherical (diameter: ca. 100 nm) and diamond-like (long axis length: ca. 100 nm) particles were further produced at higher concentration. It was suggested that the acceleration of the rate of phase transformation from β-FeOOH to hematite induced by amines plays an important role for producing fairly uniform hematite particles with different shape and size. The hematite particles produced with amines contained small amounts of OHions in the lattice but were confirmed to be nearly single crystal.  相似文献   

3.
In the present work, a novel polymer electrolyte based on poly(methyl methacrylate) (PMMA)/layered lithium trivanadate (LiV3O8) nanocomposite has been investigated. X-ray diffraction (XRD) study shows that d-spacing is increased from 6.3?±?0.1 Å to 12.8?±?0.1 Å upon intercalation of the polymer into the layered LiV3O8. Room temperature ionic conductivity of the obtained nanocomposite gel polymer electrolyte is found to be superior to that of conventional PMMA-based gel polymer electrolyte. Enhancement in ionic conductivity of the nanocomposite gel electrolyte is attributed to the formation of a two-dimensional channel as a result of decreased interaction between Li+ and V3O 8 ? layers as confirmed by FTIR. SEM results show aggregation of nanocomposite particles resulting from extension of some of the polymer chains from interlayer to the edge providing paths for Li+ ion transport. Interfacial stability of nanocomposite gel electrolyte is also found to be better than that of the conventional PMMA-based gel polymer electrolyte.  相似文献   

4.
The effect of the dispersion of zinc oxide (ZnO) nanoparticles in the zinc ion conducting gel polymer electrolyte is studied. Changes in the morphology/structure of the gel polymer electrolyte with the introduction of ZnO particles are distinctly observed using X-ray diffraction and scanning electron microscopy. The nanocomposites offer ionic conductivity values of >10?3 S cm?1 with good thermal and electrochemical stabilities. The variation of ionic conductivity with temperature follows the Vogel–Tamman–Fulcher behavior. AC impedance spectroscopy, cyclic voltammetry, and transport number measurements have confirmed Zn2+ ion conduction in the gel nanocomposites. An electrochemical stability window from ?2.25 to 2.25 V was obtained from voltammetric studies of nanocomposite films. The cationic (i.e., Zn2+ ion) transport number (t +) has been found to be significantly enhanced up to a maximum of 0.55 for the dispersion of 10 wt.% ZnO nanoparticles, indicating substantial enhancement in Zn2+ ion conductivity. The gel polymer electrolyte nanocomposite films with enhanced Zn2+ ion conductivity are useful as separators and electrolytes in Zn rechargeable batteries and other electrochemical applications.  相似文献   

5.
This paper describes a highly sensitive and selective electrochemical sensing of folic acid (FA) using vanadium pentoxide decorated graphene carbon nitride covalently grafted polyvinyl alcohol modified GC electrode (V2O5/G-C3N4/PVA/GCE). The V2O5/G-C3N4/PVA nanocomposite was synthesized by an in-situ oxidative polymerization method and characterized by various techniques such as UV–visible, Raman, FE-SEM, XRD, FT-IR, EDX, HR-TEM, SAED, and electrochemical methods. The V2O5/G-C3N4/PVA nanocomposite modified GCE showed superior electrocatalytic activity towards the FA detection. The superior electrochemical activity of the catalyst is owing to good conductivity, high surface area and enhanced electron transfer efficiency of the nanocomposite. The amperometric (i-t) studies revealed that the V2O5/G-C3N4/PVA nanocomposite modified GCE performed well by attaining a linear response of FA from 0.01 to 60 µM with a lower detection limit 0.00174 µM and the sensitivity of 19.02 μA µM−1 cm−2. Meanwhile, the V2O5/G-C3N4/PVA nanocomposite modified GCE exhibited good selectivity, rapid and stable response towards FA. The proposed method has been successfully applied for the selective determination of FA in various real samples such as apple juice, green tea and tap water with samples with good recoveries.  相似文献   

6.
Graphene oxide (GO) nanoparticles were synthesized by modified Hummers method. The synthesized GO nanoparticles were incorporated in polyvinyl alcohol/polyvinyl pyrrolidone (PVA/PVP) blend polymers for the preparation of nanocomposite polymer films by solution cast technique. Different characterizations such as XRD, UV–Vis and FTIR were carried-out on to the prepared nanocomposite polymer films. The thermal analysis of the films was studied by DSC. The morphology of PVA/PVP:GO polymer films confirms GO was exfoliated within the PVA/PVP matrix and also reveals the heterogeneous phase of nanocomposite polymer electrolyte systems. From the conductivity studies the highest conductivity of PVA/PVP: GO (0.45: 0.3) was found to be 8.05 × 10–4 S/cm at room temperature. Solid state battery has been fabricated with the configuration of Mg+/(PVA/PVP:GO)/(I2 + C + electrolyte) and its cell parameters were calculated for a constant load of 100 kΩ.  相似文献   

7.
We have reported the synthesis of water dispersible alginic acid (AA)-Fe3O4 nanocomposites. The crystallite size was obtained as 9 ± 2 nm from X-ray line profile fitting. As compared to the particle size of 9.2 nm obtained from TEM analysis, these particles show dominantly single crystalline nature. Dielectric analysis show that the real and imaginary parts of the permittivity of both pure AA and AA-Fe3O4 nanocomposite obey the ionic polarization mechanism comprised of ionic conductivity and interfacial or space charge polarization. Magnetization measurements show that the saturation magnetization of AA-capped magnetite is significantly lower than the theoretical bulk value, partly due to the structural distortions on the surface of the particles. Moreover, magnetite does not saturate and exhibits no coercivity above a certain temperature, revealing superparamagnetic behavior of the nanocomposite above a blocking temperature, TB, of ∼175 K. The magnetic core size, determined by theoretical fitting to the magnetization data at room temperature, is 9.55 nm.  相似文献   

8.
Effect of fumed silica dispersion on poly(vinylidene fluoride-co-hexafluoropropylene)-based magnesium ion-conducting gel polymer electrolyte has been studied using various physical and electrochemical techniques. The composite gel electrolytes are free-standing and flexible films with enough mechanical strength. The optimized composition with 3 wt.% filler offers a maximum ionic conductivity of ∼1.1 × 10−2 S cm−1 at ∼25 °C with good thermal and electrochemical stabilities. The Mg2+ ion conduction in the gel nanocomposite film is confirmed from the cyclic voltammetry, impedance spectroscopy, and transport number measurements. The space-charge layers formed between filler particles and gel electrolyte are responsible for the enhancement in ionic conductivity. The applicability of the gel nanocomposite to a rechargeable battery is examined by fabricating a prototype cell consisting of Mg [or Mg-multiwalled carbon nanotube (MWCNT) composite] and MoO3 as negative and positive electrodes, respectively. The discharge capacity and the rechargeability of the cell have been improved when Mg metal is substituted by Mg-MWCNT composite. The discharge capacity of the optimized cell has found to be ∼175 mAh g−1 of MoO3 for an initial ten charge–discharge cycles.  相似文献   

9.
Novel core–shell SDC (Ce0.8Sm0.2O1.9)/amorphous Na2CO3 nanocomposite was prepared for the first time. The core–shell nanocomposite particles are smaller than 100 nm with amorphous Na2CO3 shell of 4–6 nm in thickness. The nanocomposite electrolyte shows superionic conductivity above 300 °C, where the conductivity reaches over 0.1 S cm−1. Such high conductive nanocomposite has been applied in low-temperature solid oxide fuel cells (LTSOFCs) with an excellent performance of 0.8 W cm−2 at 550 °C. A new potential approach of designing and developing superionic conductors for LTSOFCs was presented to develop interface as ‘superionic highway’ in two-phase materials based on coated SDC.  相似文献   

10.
《Electroanalysis》2005,17(20):1854-1860
A novel type of sol‐gel inorganic‐organic hybrid material coated on glassy carbon electrode used for immobilization of double‐stranded DNA (dsDNA) and study of dsDNA with redox‐active molecules was developed. The hybrid material coating was produced by sol‐gel method with nano hydroxyapatite (HAp)‐polyvinyl alcohol (PVA). The optimum composition of the hybrid material was first examined, and the morphology of the nano HAp‐PVA coatings was investigated with the help of Scanning Electron Microscope (SEM). DsDNA was immobilized in/on the nano HAp‐PVA hybrid coatings by adsorption and the characteristics of the dsDNA/HAp‐PVA/GCE were studied by cyclic voltammetry (CV) using the probes of Co(phen) and Fe(CN) . The results indicate that the dsDNA can be immobilized on the nano porous HAp‐PVA coating effectively and its stability can satisfy the necessity of study on the interactions of dsDNA with redox‐active molecules on the electrode surface. Co(bpy) and Co(phen) were used as the model molecule to study the interactions of dsDNA with redox‐active molecules. Information such as ratio (KOx/KRed) of the binding constant for the oxidized and reduced forms of a bound species, interaction mode, including change in the mode of interaction, and “limiting” ratio K /K at zero ionic strength (μ) can be obtained using dsDNA/HAp‐PVA/GCE with about 2 μg of DNA samples.  相似文献   

11.
Organic-inorganic hybrid membranes based on poly(ethylene oxide) (PEO) 6.25 wt%/poly(vinylidene fluoride hexa fluoro propylene) [P(VdF-HFP)] 18.75 wt% were prepared by using various concentration of nanosized barium titanate (BaTiO3) filler. Structural characterizations were made by X-ray diffraction and Fourier transform infrared spectroscopy, which indicate the inclusion of BaTiO3 in to the polymer matrix. Addition of filler creates an effective route of polymer-filler interface and promotes the ionic conductivity of the membranes. From the ionic conductivity results, 6 wt% of BaTiO3-incorporated composite polymer electrolyte (CPE) showed the highest ionic conductivity (6 × 10?3 Scm?1 at room temperature). It is found that the filler content above 6 wt% rendered the membranes less conducting. Morphological images reveal that the ceramic filler was embedded over the membrane. Thermogravimetric and differential thermal analysis (TG-DTA) of the CPE sample with 6 wt% of the BaTiO3 shows high thermal stability. Electrochemical performance of the composite polymer electrolyte was studied in LiFePO4/CPE/Li coin cell. Charge-discharge cycle has been performed for the film exhibiting higher conductivity. These properties of the nanocomposite electrolyte are suitable for Li-batteries.  相似文献   

12.
A proton-conducting nanocomposite gel polymer electrolyte (GPE) system, [35{(25 poly(methylmethacrylate) (PMMA) + 75 poly(vinylidenefluoride-co-hexafluoropropylene) (PVdF-HFP))?+?xSiO2}?+?65{1 M NH4SCN in ethylene carbonate (EC) + propylene carbonate (PC)}], where x?=?0, 1, 2, 4, 6, 8, 10, and 12, has been reported. The free standing films of the gel electrolyte are obtained by solution cast technique. Films exhibit an amorphous and porous structure as observed from X-ray diffractometry (XRD) and scanning electron microscopy (SEM) studies. Fourier transform infrared spectrophotometry (FTIR) studies indicate ion–filler–polymer interactions in the nanocomposite blend GPE. The room temperature ionic conductivity of the gel electrolyte has been measured with different silica concentrations. The maximum ionic conductivity at room temperature has been observed as 4.3?×?10?3?S?cm?1 with 2 wt.% of SiO2 dispersion. The temperature dependence of ionic conductivity shows a typical Vogel-Tamman-Fulcher (VTF) behavior. The electrochemical potential window of the nanocomposite GPE film has been observed between ?1.6 V and 1.6 V. The optimized composition of the gel electrolyte has been used to fabricate a proton battery with Zn/ZnSO4·7H2O anode and PbO2/V2O5 cathode. The open circuit voltage (OCV) of the battery has been obtained as 1.55 V. The highest energy density of the cell has been obtained as 6.11 Wh?kg?1 for low current drain. The battery shows rechargeability up to 3 cycles and thereafter, its discharge capacity fades away substantially.  相似文献   

13.
Ni0.04Zn0.96O and Fe0.03Zn0.97O with average diameter of 23 and 19 nm, respectively, have been synthesized by a modified sol–gel method to be used in the preparation of (100 − x)/x poly(vinyl alcohol)/oxide nanocomposite films, with x = 0, 1, 3 and 5 (in wt.%). A 125 W-Hg vapor lamp with emission above 254 nmwas used to irradiate PVA/Ni0.04Zn0.96O and PVA/Fe0.03Zn0.97O films. The effect on their structural, thermal, morphological and optical properties was studied by TG, DSC, DRX, AFM, UV–vis and PL spectrophotometry. The Ni0.04Zn0.96O addition on PVA films decreases the thermal stability of the polymer in inert and in oxidative atmosphere. In contrast, the Fe0.03Zn0.97O presence in the PVA films seems to increase the thermal stability of the polymer. The characteristic peak of the crystalline phase of PVA and wurtzite phase of the zinc oxide were identified through X-ray diffraction in both films. The crystallinity of the PVA film increases with UV irradiation and with the presence of Ni0.04Zn0.96O and Fe0.03Zn0.97O. The roughness of the PVA film was not modified by the addition of the doped oxides; however, it increases after UV irradiation, more significantly in the films containing the oxides. The PVA film exhibits absorption around 280 nm characteristic of π–π transitions related to carbonyl groups from residuals acetate, while the 95/05 PVA/Ni0.04Zn0.96O and 95/05 PVA/Fe0.03Zn0.97O nanocomposite films show absorption at the visible region which is characteristics of the band gap reduction of the doped oxides. The photoluminescence of PVA was modified by the presence of the oxides in the film. These nanocomposite films are interesting due to their thermal, mechanical (flexible) properties and low cost of production. In addition they are also able to exhibit peculiar optical properties showing potential to be used in photonic devices, gas sensors and organic solar cell applications.  相似文献   

14.
Ultrathin carbon nanoparticle–poly(diallyldimethylammonium chloride) films (CNP‐PDDAC films) are formed on tin‐doped indium oxide (ITO) electrodes in a layer‐by‐layer electrostatic deposition process employing 9–18 nm diameter carbon particles. Transparent and strongly adhering films of high electrical conductivity are formed and characterized in terms of their electrochemical reactivity. When immersed in aqueous 0.1 M phosphate buffer pH 7, each layer of CNP‐PDDAC (of ca. 5–6 nm average thickness) is adding an interfacial capacitance of ca. 10 μF cm?2. Absorption into the CNP–PDDAC nanocomposite film is dominated by the sites in the PDDAC cationomer and therefore anionic molecules such as indigo carmine are strongly bound and retained within the film (cationic binding sites per layer ca. 150 pmol cm?2). In contrast, cationic redox systems such as ferrocenylmethyltrimethyl‐ammonium+ fail to bind. For solution phase redox systems such as hydroquinone, the rate of electron transfer is dramatically affected by the CNP‐PDDAC film and switched from completely irreversible to highly reversible even with a single layer of carbon nanoparticles. For the mixed redox system ascorbate–dopamine in 0.1 M phosphate buffer pH 7 cyclic voltammograms suggest a rapid and selective temporary poisoning process which causes the ascorbate oxidation to be suppressed in the second potential cycle. This effect is exploited for the detection of micromolar concentrations of dopamine in the presence of millimolar ascorbate.  相似文献   

15.
A titanium dioxide sol with narrow particle size distribution was synthesized using TiCl4 as the starting material. The sol was prepared by a process where HCl was added to a gel of hydrated titanium oxide to dissolve it. The resulting aqueous titanic acid solution was heated to form titanium dioxide sol. The effects of preparation parameters were investigated. TiCl4 was slowly added to distilled water at 5°C. Aqueous solution of sodium hydroxide was added to adjust the pH of the system to 8–12. After aging for a period of time, the peptized sol was filtered and sufficiently washed. The filtered cake was repulped in water. Hydrochloric acid was slowly added to the solution with stirring. After condensation reaction and crystallization, a transparent sol with suspended TiO2 was formed. XRD results show that the crystalline phase was anatase. The suspended TiO2 particles were rhombus primary particles with the major axis ca. 20 nm and the minor axis ca. 5 nm. The TiO2 particles prepared at pH 8 had the largest surface area of 141 cm3/g and it was microporous. The compositions of the solution which yielded the smallest suspended TiO2 particles were TiO2:HCl (35% HCl) = 1:1 (molar ratio), concentration of TiO2 = 10%. Hydroxypropyl cellulose with viscosity of 150–400 cps was added as a dispersant. The sol was excellent in dispersibility and long-term stability. Transparent thin films could be obtained through dip-coating glass substrate in the sol. The dip-coating on glass can be less than three times to have one monolayer TiO2. The transparent TiO2 thin film had strong hydrophilicity after being illuminated by UV light.  相似文献   

16.
Li2ZnTi3O8/C nanocomposite has been synthesized using phenolic resin as carbon source in this work. The structure, morphology, and electrochemical properties of the as-prepared Li2ZnTi3O8 samples were analyzed by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscope (TEM), Raman spectroscopy (RS), galvanostatic charge–discharge, and AC impedance spectroscopy. SEM images show that Li2ZnTi3O8/C was agglomerated with a primary particle size of ca. 40 nm. TEM images reveal that a homogeneous carbon layer (ca. 5 nm) formed on the surface of Li2ZnTi3O8 particles which is favorable to improve the electronic conductivity and inhibit the growth of Li2ZnTi3O8 during annealing process. The as-prepared Li2ZnTi3O8/C composite with 6.0 wt.% carbon exhibited a high initial discharge capacity of 425 and 159 mAh g?1 at 0.05 and 5 A g?1, respectively. At a high current density of 1 A g?1, 95.5 % of its initial value is obtained after 100 cycles.  相似文献   

17.
Ion-conducting nanocomposite polymer electrolyte films based on poly(ethylene oxide)-NaPO3 3: 1 with up to 15 wt % of SiO2 have been prepared using recently developed hot-press technique instead of conventional solution cast method. With 7 wt % of SiO2, the film conductivity has been enhanced by an order of magnitude. The materials have been characterized by Fourier transform infrared spectrometry and thermogravimetric analysis. For the composition with the highest conductivity, the temperature dependences of ionic mobility, mobile ions concentration, ionic transference number, and ionic drift velocity have been determined. Dielectric constant and dielectric loss have been measured. The conductivity enhancement has been discussed on the basis of existing theories of dielectrics.  相似文献   

18.
A polymer film based on polymeric ionic liquid, which was poly(1‐vinyl‐3‐butylimidazolium chloride) (poly(ViBuIm+Cl?)for short), was firstly used as matrix to immobilize hemoglobin (Hb). FTIR and UV‐vis spectra demonstrated that the native structure of Hb was well preserved after entrapped into the polymer film. The Hb immobilized in the poly(ViBuIm+Cl?) film showed a fast direct electron transfer for the Hb‐FeIII/FeII redox couple. Based on the direct electron transfer of the immobilized Hb, polyvinyl alcohol (PVA)/Hb/poly(ViBuIm+Cl?)/GC electrode displayed good sensitivity and wide linear range for the detection of H2O2. The linear range of the PVA/Hb/poly(ViBuIm+Cl?)/GC electrode to H2O2 is from 3.5 to 224 μM with a limit of detection of 1.17 μM. Such an avenue, which integrated polymeric ionic liquid and redox protein via a simple method, may provide a novel and efficient platform for the fabrication of biosensors, biofuel cells and other bioelectrochemical devices.  相似文献   

19.
There has been an ongoing need to develop polymer materials with increased performance as proton exchange membranes (PEMs) for middle- and high-temperature fuel cells. Poly(vinyl alcohol) (PVA) is a highly hydrophilic and chemically stable polymer bearing hydroxyl groups, which can be further altered. Protic ionic liquids (proticILs) have been found to be an effective modifying polymer agent used as a proton carrier providing PEMs’ desirable proton conductivity at high temperatures and under anhydrous conditions. In this study, the novel synthesis route of PVA grafted with fluorinated protic ionic liquids bearing sulfo groups (–SO3H) was elaborated. The polymer functionalization with fluorinated proticILs was achieved by the following approaches: (i) the PVA acylation and subsequent reaction with fluorinated sultones and (ii) free-radical polymerization reaction of vinyl acetate derivatives modified with 1-methylimidazole and sultones. These modifications resulted in the PVA being chemically modified with ionic liquids of protic character. The successfully grafted PVA has been characterized using 1H, 19F, and 13C-NMR and FTIR-ATR. The presented synthesis route is a novel approach to PVA functionalization with imidazole-based fluorinated ionic liquids with sulfo groups.  相似文献   

20.
Poly(vinyl phosphonic acid) (PVPA)-Fe3O4 nanocomposite is synthesized by the precipitation of Fe3O4 in the presence of PVPA. Structural, surface, morphological, thermal properties and conductivity characterization/evaluation of the nanocomposite were performed by XRD, FT-IR, TEM, TGA and conductivity measurements respectively. The capping of PVPA around the Fe3O4 nanoparticles was confirmed by FT-IR spectroscopy, the interaction being via bridging oxygens of the phosphate and the nanoparticle surface. The crystallite and particle size were obtained as 6 ± 2 and 8.7 ± 0.1 nm from XRD line profile fitting and TEM image analysis respectively, which reveal nearly single crystalline nature of the Fe3O4 nanoparticles. Magnetic characterization of the bulk magnetite and (PVPA)-Fe3O4 nanocomposite reveals that both are in the superparamagnetic state at room temperature. The average magnetic domain size of the nanoparticles has been calculated using the Langevin function, which was fitted to the measured M-H hysteresis curves as 7.6 nm for the nanocomposite. In the nanocomposite, the reduction is due to the adsorption of PVPA onto the magnetite surface, which cancels some of the free spins at the surface causing a magnetically dead layer. Analysis of the conductivity and permittivity measurements revealed the coupling of ionic and polymer segmental motions and strong temperature dependency in the nanocomposite.  相似文献   

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