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1.
Novel complex nanospheres with core/shell structure for selective adsorption of Hg2+ have been prepared by a simple one-pot method. Scanning electron microscopy (SEM) and transmission electron microscope (TEM) images showed the nanospheres had perpendicularly thiol-functionalized mesoporous SiO2 hybrid shell and Fe3O4@SiO2 core (Fe3O4@nSiO2@mSiO2–SH). XRD patterns of as-synthesized nanospheres confirmed the observation of the SEM and TEM. The size of the nanospheres is about 100 nm. Based on the analysis of N2 sorption–desorption isotherm, the surface area and pore volume of the adsorbent are 861 m2/g and 0.48 cm3/g, respectively. The saturation magnetization value for Fe3O4@nSiO2@mSiO2–SH is as high as 6.87 emu g−1. The nanospheres showed more accessible active sites and high dispersibility in water, exhibited excellent performance for selective Hg2+ adsorption, had a stable structure, and could be recycled easily with magnet.  相似文献   

2.
Cu–Ni fcc alloy nanoparticles (NPs) of tunable atomic ratios were generated in SiO2 films. The films were prepared using the Cu(NO3)2 and Ni(NO3)2 co-doped inorganic–organic hybrid silica sols by single dipping. Transparent, crack-free, glassy SiO2 films of 310 ± 10 nm in thickness embedded with high mol percent of Cu–Ni alloy NPs were yielded after annealing at 750 °C in 10% H2-90% Ar atmosphere. Nominal compositions of the films were 20 mol% (Cu–Ni)-80 mol% SiO2. Optical spectral study of the heat-treated films showed disappearance of Cu plasmon bands due to Cu–Ni alloy formation. Grazing incidence X-ray diffraction (GIXRD) studies revealed the formation of Cu–Ni alloy (2:1, 1:1 and 1:2) NPs inside the SiO2 film. GIXRD showed a systematic shifting of the diffraction peaks with respect to the fcc Cu–Ni alloy composition, maintaining the nominal ratios. Transmission electron microscopy (TEM) studies of the representative Cu0.5Ni0.5-doped film showed existence of homogeneously dispersed Cu–Ni alloy NPs of average size 6.35 nm inside the SiO2 matrix. The energy dispersive X-ray scattering (EDX) analysis of the individual NPs using the nano-probe (scanning TEM mode) confirmed the presence of both the Cu and Ni with the desired atomic ratio.  相似文献   

3.
Silica aerogel (SiO2 aerogel) was prepared by sol–gel method from tetraethyl orthosilicate hydrolyzation and has been characterized by scanning electron microscopy and N2 adsorption for its surface structure, surface area, and pore-size distribution. Constant current charge–discharge technique, cyclic voltammetry, and electrochemical impedance spectrum were employed for its specific capacitance and equivalent series resistance. The results showed that the maximum specific capacitance of SiO2 aerogel electrode in 1 M Et4NBF4/PC electrolyte was 62.5 F g−1. In addition, the SiO2 aerogel capacitor exhibits excellent long-term stability with no significant degradation after 500 charging and discharging cycles. Therefore, the application of high surface area SiO2 aerogel as electrodes in supercapacitor devices is promising.  相似文献   

4.
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   

5.
Inorganic–organic hybrid membranes were prepared by sol–gel process with tetramethoxysilane/methyltrimethoxysilane/diisopropyl phosphite and 1-butyl-3-methylimidazolium tetrafluoroborate (BMIMBF4) ionic liquid as precursors. The Fourier transform infrared spectroscopy (FT-IR) and 31P, 29Si, 1H, 13C, and 19F nuclear magnetic resonance measurements have shown good chemical stability and complexation of (POH[(CH3)2CHO]2) with [BMIMBF4] ionic liquid in the fabricated hybrid membranes. The influence of the textural properties of all the prepared composite membranes could be interpreted from nitrogen adsorption–desorption measurements. The average pore size was increased proportionally with the ionic liquid weight percent ratio in the host phosphosilicate matrix from 2.59 to 11.71 nm, respectively. Thermogravimetric analysis and differential thermal analysis measurements confirmed that the hybrid membranes were thermally stable up to 260 °C. Thermal stability of the hybrid membranes was significantly enhanced by the presence of inorganic SiO2 framework and high stability of [BF4] anion. For all the composite membranes, the conductivities were measured within the temperature range (−30 °C) to 150 °C, and a maximum conductivity of 7 × 10−3 S/cm at 150 °C was achieved for 40 wt.% ionic liquid-based composite membrane under nonhumidified conditions.  相似文献   

6.
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   

7.
In this work, we report on laser ablation of thermally grown SiO2 layers from silicon wafer substrates, employing an 8–9 ps laser, at 1064 (IR), 532 (VIS) and 355 nm (UV) wavelengths. High-intensity short-pulse laser radiation allows direct absorption in materials with bandgaps higher than the photon energy. However, our experiments show that in the intensity range of our laser pulses (peak intensities of <2×1012 W/cm2) the removal of the SiO2 layer from silicon wafers does not occur by direct absorption in the SiO2 layer. Instead, we find that the layer is removed by a “lift off” mechanism, actuated by the melting and vaporisation of the absorbing silicon substrate. Furthermore, we find that exceeding the Si melting threshold is not sufficient to remove the SiO2 layer. A second threshold exists for breaking of the layer caused by sufficient vapour pressure. For SiO2 layer ablation, we determine layer thickness dependent minimum fluences of 0.7–1.2 J/cm2 for IR, 0.1–0.35 J/cm2 for VIS and 0.2–0.4 J/cm2 for UV wavelength. After correcting the fluences by the reflected laser power, we show that, in contrast to the melting threshold, the threshold for breaking the layer depends on the SiO2 thickness.  相似文献   

8.
Serge Zhuiykov 《Ionics》2009,15(4):507-512
In situ Fourier transform spectroscopy (FTIR) was used to study interactions of nanostructured ruthenium oxide (RuO2) thin-film sensing electrode with O2 at room temperature. RuO2 nanostructures were pretreated at 1,000 °C for 1 h in order to obtain good crystallinity of amorphous RuO2 nanoparticles. Morphology and properties of nanostructured RuO2 were characterized by X-ray diffraction, thermo-gravimetric/differential thermal analysis, scanning electron microscopy, and FTIR. It was shown that pretreated RuO2 is quite active for O2 , O2 2−, and O2− adsorption with clear 722 cm−1 band for superoxide ions (O2 ) adsorption for the different oxygen concentrations. The results of in situ FTIR measurements revealed that the active sites for oxygen adsorption are not limited to the triple boundaries, but extended to surfaces of RuO2 electrodes. Fundamental vibration frequencies of ruthenium–oxygen bond at a temperature of 23 °C as well as region above fundamental frequencies for the nanostructured RuO2 were identified.  相似文献   

9.
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   

10.
We analyzed the whole-body distribution of 14C–ADP-labeled silica nanoparticles (14C–ADP–SiO2 nanoparticles) and submicron particles (14C–ADP–SiO2 submicron particles) after intravenous injection into ICR mice. The 14C–ADP–SiO2 nanoparticles and submicron particles were synthesized before the injection and the particle size was 19.6 and 130 nm, respectively. Similarly, the shape was spherical and the crystallinity was amorphous. After the synthesis, we injected mice with the 14C–ADP–SiO2 nanoparticles or the 14C–ADP–SiO2 submicron particles and dissected tissues after 1, 2, 4, 8 and 24 h. The radioactivity in the tissues was measured with a liquid scintillation counter. As a result, the retention percentage in bone, skin, lymph nodes, and the digestive mixture was at least twofold higher in the 14C–ADP–SiO2 nanoparticles-exposed mice, whereas the retention percentage in the kidney was statistically higher in the 14C–ADP–SiO2 submicron particles-exposed mice. Both types of 14C–ADP–SiO2 particles mainly translocated to the muscle, bone, skin, and liver, but hardly translocated to the brain and olfactory bulb. Furthermore, the 14C–ADP–SiO2 nanoparticles had a higher retention percentage (62.4 %) in the entire body at 24-h post-injection than did the 14C–ADP–SiO2 submicron particles (50.7 %). Therefore, we suggested that the 14C–ADP–SiO2 nanoparticles might be more likely than the 14C–ADP–SiO2 submicron particles to be retained in the body, and consequently they might be gradually accumulated by chronic exposure.  相似文献   

11.
Mesoporous γ-Fe2O3/SiO2 nanocomposite containing 30 mol% of γ-Fe2O3 was prepared by a template-free sol-gel method, and its removal ability for methyl orange (MO) was investigated. The nanocomposite was characterized using X-ray powder diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscope (SEM), Fourier transform infrared (FTIR) absorption measurements, nitrogen adsorption-desorption measurements, and magnetic measurements. The synthesized γ-Fe2O3/SiO2 nanocomposite has a mesoporous structure with an average pore size of 3.5 nm and a specific surface area of 245 m2/g, and it exhibits ferrimagnetic characteristics with the maximum saturation magnetization of 20.9 emu/g. The adsorption of MO on the nanocomposite reaches the maximum adsorbed percentage of ca. 80% within a few minutes, showing that most of MO can be removed in a short time. The MO adsorption data fit well with both Langmuir and Freundlich adsorption isotherms. The maximum adsorption capacity of MO is estimated to be 476 mg/g.  相似文献   

12.
Anatase is the low-temperature (300–550 °C) crystalline polymorph of TiO2 and it transforms to rutile upon heating. For applications utilizing the photocatalytic properties of nanoscale anatase at elevated temperatures (over 600 °C) the issue of phase stabilisation is of major interest. In this study, binary TiO2/SiO2 particles were synthesized by a flame aerosol process with TiCl4 and SiCl4 as precursors. The theoretical Si/Ti ratio was varied in the range of 0.7–1.3 mol/mol. The synthesized TiO2/SiO2 samples were heat treated at 900 and 1,000 °C for 3 h to determine the thermostability of anatase. Pyrogenic TiO2 P25 (from Evonik/Degussa, Germany) widely applied as photocatalyst was used as non-thermostabilized reference material for comparison of photocatalytic activity of powders. Both the non-calcinated and calcinated powders were characterized by means of XRD, TEM and BET. Photocatalytic activity was examined with dichloroacetic acid (DCA) chosen as a model compound. It was found that SiO2 stabilized the material retarding the collapse of catalyst surface area during calcination. The weighted anatase content of 85% remains completely unchanged even after calcination at 1,000 °C. The presence of SiO2 layer/bridge as spacer between TiO2 particles freezes the grain growth: the average crystallite size increased negligibly from 17 to 18 nm even during the calcination at 1,000 °C. Due to the stabilizing effect of SiO2 the titania nanoparticles calcinated at 900 and 1,000 °C show significant photocatalytic activity. Furthermore, the increase in photocatalytic activity with calcination temperature indicates that the titania surface becomes more accessible either due to intensified cracking of the SiO2 layer or due to enhanced transport of SiO2 into the necks thus releasing additional titania surface.  相似文献   

13.
The chaperonin protein GroEL was mixed with varying concentrations of K2PtCl4 followed by a 20-fold concentration of sodium borohydride to afford GroEL–platinum nanoparticle complexes in a ratio of between 1:25 and 1:2,000. Typical colour change, from colourless or pale yellow to brown, occurred that was dependent on the amount of platinum present. These complexes were characterised by UV/Vis, inductively coupled plasma optical emission spectroscopy, Fourier transform infra red, transmission electron microscopy (TEM) and energy dispersive X-ray spectroscopy. TEM analysis revealed that the size of nanoparticles increased as the molar ratio of platinum to GroEL increased with an average size diameter of 1.72–3.5 nm generated with GroEL–platinum molar ratios of 1:125–1:2,000. Fourier-transform infrared spectroscopy (FTIR) spectra showed no distinct changes in the structure of GroEL but confirmed that the nanoparticles were attached to the protein. The effect of platinum nanoparticles on the ATPase activity of GroEL showed an activity of 5.60 μmol min−1 ml−1 (87 % increase over a control) at the molar ratio of GroEL–platinum nanoparticles of 1:25.  相似文献   

14.
Polyvinylidenefluoride–hexafluoropropylene-based (PVdF–HFP-based) gel and composite microporous membranes (GPMs and CPMs) were prepared by phase-inversion technique in the presence 10 wt% of AlO(OH) n nanoparticles. The prepared membranes were gelled with 0.5-M LiPF3(CF2CF3)3 (lithium fluoroalkylphosphate, LiFAP) in EC:DEC (1:1 v/v) and subjected to various characterizations; the AC impedance study shows that CPMs exhibit higher conductivity than GPMs. Mechanical stability measurements on these systems reveal that CPMs exhibit Young’s modulus higher than that of bare and GPMs and addition of nanoparticles drastically improves the elongation break was also noted. Transition of the host from α to β phase after the loading of nanosized filler was confirmed by XRD and Raman studies. Physico-chemical properties, like liquid uptake, porosity, surface area, and activation energy, of the membranes were calculated and results are summarized. Cycling performance of Li/CPM/LiFePO4 coin cell was fabricated and evaluated at C/10 rate and delivered a discharge capacity of 157 and 148 mAh g−1 respectively for first and tenth cycles.  相似文献   

15.
Nanoporous SiO2 thin films with ultra-low dielectric constants were synthesized using a molecular template method. Uniform films with pore size between 10 and 20 nm were obtained as observed by N2 adsorption/desorption isotherms and transmission electron microscopy. Fourier transform infrared spectroscopy (FTIR) and differential thermal analysis were carried out to investigate the effect of n-hexane washing on structural properties before and after the surface modification process. The results showed that –OH bonds were substituted with –CH3 bonds in the films as a result of modification of trimethylchlorosilane (TMCS)/n-hexane solution. Four kinds of model were used to analyze the relationship between porosity and dielectric constant of the films, where the dielectric constant was determined from capacitance-voltage measurements. The investigation indicated that the corresponding relationship was in accord with that estimated by the Rayleigh model.  相似文献   

16.
The application of resonance Raman (RR) and surface‐enhanced resonance Raman (SERR) spectroscopies to the qualitative and semiquantitative analysis of the artificial dye indigo carmine has been examined using sodium‐citrate‐reduced silver colloid and island films with various roughnesses. Additional, the Raman spectrum of the solid state and density functional theory (DFT) calculations helped to a better understanding of the fully optimized geometry and of the vibrational wavenumbers of the dye. A strong chemical interaction of indigo carmine with the silver colloidal particles was observed mainly at very low concentration of 0.03 × 10−9 M and with silver film surfaces at a concentration of 10−4 M . The indigo carmine orientation possibilities while going to different metallic substrates are discussed. Copyright © 2007 John Wiley & Sons, Ltd.  相似文献   

17.
Water and methanol transport behavior, morphology, and solvent adsorption of filler-free Nafion membrane, Nafion–SiO2, Nafion–TiO2, and two Nafion–Zr(HPO4)2 composites were investigated using nuclear magnetic resonance methods, including spin-lattice relaxation and pulsed-field-gradient spin-echo diffusion conducted under both variable temperature and variable hydrostatic pressure conditions and scanning electron microscopy analysis. A comparison between water and methanol self-diffusion coefficients reveals that the water mobility is higher than the methanol mobility in all the membranes. Additionally, the inclusion of inorganic fillers improves both the solvent uptakes and the transport properties of the composite membranes relative to filler-free Nafion, with the exception of one of the Nafion–Zr(HPO4)2 composite. Nafion–Zr(HPO4)2 composites were prepared by two different procedures, in situ and ex situ. Although phosphorus-31 magic-angle spinning nuclear magnetic resonance spectra show the same structures of the particles in both kinds of membranes, the morphology, solvent absorption properties, and solvent mobilities are very different. Paper presented at the 11th EuroConference on the Science and Technology of Ionics, Batz-sur Mer, Sept. 9–15, 2007.  相似文献   

18.
Previous studies in our laboratory have reported that the chemical etch rate of a commercial photosensitive glass ceramic (FoturanTM, Schott Corp., Germany) in dilute hydrofluoric acid is strongly dependent on the incident laser irradiance during patterning at λ=266 nm and λ=355 nm. To help elucidate the underlying chemical and physical processes associated with the laser-induced variations in the chemical etch rate, several complimentary techniques were employed at various stages of the UV laser exposure and thermal treatment. X-ray diffraction (XRD) was used to identify the crystalline phases that are formed in Foturan following laser irradiation and annealing, and monitor the crystalline content as a function of laser irradiance at λ=266 nm and λ=355 nm. The XRD results indicate the nucleation of lithium metasilicate (Li2SiO3) crystals as the exclusive phase following laser irradiation and thermal treatment at temperatures not exceeding 605 °C. The XRD studies also show that the Li2SiO3 density increases with increasing laser irradiance and saturates at high laser irradiance. For our thermal treatment protocol, the average Li2SiO3 crystal diameters are 117.0±10.0 nm and 91.2±5.8 nm for λ=266 nm and λ=355 nm, respectively. Transmission electron microscopy (TEM) was utilized to examine the microscopic structural features of the lithium metasilicate crystals. The TEM results reveal that the growth of lithium metasilicate crystals proceeds dendritically, and produces Li2SiO3 crystals that are ∼700–1000 nm in length for saturation exposures. Optical transmission spectroscopy (OTS) was used to study the growth of metallic silver clusters that act as nucleation sites for the Li2SiO3 crystalline phase. The OTS results show that the (Ag0)x cluster concentration has a dependence on incident laser irradiance that is similar to the etch rate ratios and Li2SiO3 concentration. A comparison between the XRD and optical transmission results and our prior etch rate results show that the etch rate contrast and absolute etch rates are dictated by the Li2SiO3 concentration, which is in turn governed by the (Ag0)x cluster concentration. These results characterize the relationship between the laser exposure and chemical etch rate for Foturan, and permit a more detailed understanding of the photophysical processes that occur in the general class of photostructurable glass ceramic materials. Consequently, these results may also influence the laser processing of other photoactive materials. PACS  42.62.-b; 61.43.Fs; 81.05.Kf; 81.10.-h; 83.80.Ab  相似文献   

19.
Using low-pressure chemical vapour deposition (LPCVD), multi-walled carbon nanotubes (MWNTs) are grown on nanocrystalline Fe70Pt30 film. The Fe70Pt30 nanocrystalline film is deposited by vapour condensation technique. The size of the nanoparticles varies from 5–10 nm, as inferred from SEM micrographs of Fe70Pt30 film. SEM and TEM observations of as-grown CNTs film reveal that these are multi-walled and their diameter varies from 30–80 nm and length is of the order of several micrometers respectively. There is a structural change from ordinary geometry of CNTs to bamboo shaped as suggested by TEM image. Raman spectra shows sharp G and D bands with a higher intensity of G band showing the presence of graphitic nature of the nanotubes. An experimental study of the temperature dependence of electrical conductivity of MWNTs film is done over a wide temperature range from (293–4 K). The measured data gives a good fit to variable-range hopping (VRH) and the results are interpreted using Mott's (VRH) model. The conduction mechanism of the MWNTs film shows a crossover from the exp[ -(To/T)1/4] law in the temperature range (293–110 K) to exp[ -(Tm/T)1/3] in the low temperature range (110–4 K). This behaviour is attributed to temperature-induced transition from three-dimension (3D) to two-dimension (2D) VRH. Various Mott's parameters like characteristic temperature (Tm), density of states at Fermi level N(EF), localization length (ξ), hopping distance (R), hopping energy (W) have also been calculated using above-mentioned model.  相似文献   

20.
In this study, amino-modified titanate nanotubes (NH2-TNs) were prepared and used to adsorb duplex DNA. Macroscopic complexes between DNA and NH2-TNs were observed. The uptake of DNA by NH2-TNs was very fast; equilibrium was reached within 10 min at pH 3.6–5.0. The equilibrium capacity in the adsorption isotherm of NH2-TNs was 240 mg g−1, and further increase of the adsorption capacity was obtained with the addition of Ca2+ in solution. The adsorbed DNA could be released with phosphate buffer saline (PBS) solution without damage of the DNA strands. NH2-TNs could protect DNA from cleavage efficiently in the presence of DNase I.  相似文献   

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