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1.
Maghemite nano-particles were synthesized by a solid-state chemical reaction for its highly selective use as, cyclotron-produced, 109Cd (462.9 days) purification method of choice. 109Cd radiochemical separation starts with Ag activities precipitated with HCl 0.0015 M followed by, on a second step, 109Cd separation from Cu carrier and 65Zn (243.8 days) using Ca (NO3)2 0.01 M. Experimental parameters such, pH and sorbent concentration, on 109Cd extraction efficiency were investigated. Phase morphology, nanostructure and size of nano-particles were studied by X-ray diffraction (XRD) and scanning electron microscopy (SEM). A 10–20 nm average grain size was derived from XRD line broadening and SEM data. Heat treatment on Fe3+:Fe2+ ratios equal to 2:1, produced powders, resulting in tetragonal (maghemite) structure at 300 °C and rhombohedra (hematite) at 600 °C. 109Cd chemical and radionuclidic purity were determined by ICP-AES and HPGe detector gamma-ray spectrometry. The overall recovery and radionuclide purity were 80.0% from obtained 129.63 kBq/C MeV (70 kBq/μAh) initial activity and 91.4%, respectively.  相似文献   

2.
MgNb2O6 nanocrystalline powders have been synthesized at a low temperature by improved citrate sol–gel method in this paper. The high quality solution of Nb5+ was prepared using Nb2O5 as the starting material. The crystal structure and microstructure of MgNb2O6 powders were characterized by XRD and SEM techniques, and the effects of preparation craft including pH value and the proportion of citric acid to the niobium ions on the crystal structure and microstructure of powders were also investigated. XRD and TG/DTA results show that the single phase of MgNb2O6 for synthesized powders can be obtained by calcining the precursor at 700 °C. SEM results indicate that the average particle size of MgNb2O6 exhibits a significantly dependence on the pH values and the proportion of citric acid to the niobium ions, where it was found that particle size of a 20 nm can be obtained for the MgNb2O6 powders by sol–gel process.  相似文献   

3.
Titanium dioxide doped with iron (III) was prepared by sol–gel Spin Coating method. The phase structures, morphologies, particle size of the doped TiO2 have been characterized by X-ray diffraction (XRD), Raman spectroscopy, atomic force microscopy (AFM) and ultraviolet–visible (UV–Vis) spectrophotometer. The XRD and Raman results show that the 10% Fe3+-doped TiO2 thin films crystallize in anatase phase between 600 and 800 °C, and into the anatase–rutile phase at 1,000 °C, and further into the rutile phase when the content of Fe3+ increases (20%). The grain size calculated from XRD patterns shows that the crystallinity of the obtained anatase particles increased from 39.4 to 43.4 nm as the temperature of annealing increase, whereas the size of rutile crystallites increases, with increasing Fe3+ concentrations from 36.9 to 38.1 nm. The AFM surface morphology results confirmed that the particle size increases by increasing the annealing temperature and also with an increasing of Fe3+ content. The optical band gap (E g) of the films was determined by the UV–Vis spectrophotometer. We have found that the optical band gap decreased with an increasing of annealing temperatures and also with an increasing of Fe3+ content.  相似文献   

4.
We report herein a comprehensive study of the gas-phase Fe+-mediated oxidation of ethane by N2O on both the sextet and quartet potential energy surfaces (PESs) using density functional theory. The geometries and energies of all the relevant stationary points are located. Initial oxygen-atom transfer from N2O to iron yields FeO+. Then, ethane oxidation by the nascent oxide involves C–H activation forming the key intermediate of (C2H5)Fe+(OH), which can either undergo C–O coupling to Fe+ + ethanol or experience β-H shift giving the energetically favorable product of FeC2H4 + + H2O. Reaction of FeC2H4 + with another N2O constitutes the third step of the oxidation. N2O coordinates to FeC2H4 + and gets activated by the metal ion to yield (C2H4)Fe+O(N2). After releasing N2 through the direct H abstraction and/or cyclization pathways, the system would be oxidized to ethenol, acetaldehyde, and oxirane, regenerating Fe+. Oxidation to acetaldehyde along the cyclization –C–to–C hydrogen shift pathway is the most energetically favored channel.  相似文献   

5.
Ferromagnetic and superparamagnetic oxide nanoparticles are of particular attention because of their possible use in various fields ranging from bio-nanotechnology to spintronics. Detailed magnetic, dielectric and impedance investigations are crucial for the above-mentioned applications. This study deals with the exploration of various iron oxide phases under as-synthesized conditions by sol–gel method. pH of the sols is varied in the range of 1 to 11. X-ray diffraction (XRD) analysis indicate amorphous behavior for nanoparticles synthesized using pH 1 and 3. Nanoparticles synthesized using pH 2 and 4–6 exhibit hematite phase of iron oxide. Whereas structural transition to maghemite phase is observed for pH 7–8. Nanoparticles synthesized using high pH values, i.e. 9–11, exhibit structural transition towards magnetite phase of iron oxide. Hematite nanoparticles exhibit superparamagnetic and ferromagnetic hysteresis curves with saturation magnetization of ~ 24 emu/g and ~ 13–17 emu/g at pH 2 and pH 4–6, respectively. Maghemite nanoparticles exhibit superparamagnetic (pH 7) and ferromagnetic (pH 8) response with saturation magnetization of ~ 69 and ~ 42 emu/g, respectively. Fe3O4 nanoparticles exhibit superparamagnetic (pH 9–10) and ferromagnetic (pH 11) behavior with saturation magnetization of ~ 88, 87 and 52 emu/g, respectively. High grain boundary resistance contributed towards high dielectric constant of ~ 99, 109 and 154 (log f = 5.0) at pH 2, 7 and 9. Detailed impedance values indicate dominant role of grain boundaries in the conductivity of iron oxide nanoparticles. Superparamagnetic iron oxide (pH 9) exhibits strong antioxidant activity along with a very weak hemolytic response. The findings of cell lysis reveal that synthesized nanoparticles have a potential to combat dangerous cancer cells. Drug efficacy results show that after 120 min the encapsulation efficacy reaches a peak of ~ 83 % using curcumin, a naturally existing drug. In vivo biodistribution of nanoparticles was studied in Rabbit model. Synthesized nanoparticles are labelled using Technetium-99 m. Whereas, labeling efficacy and stability was examined using =nstant thin layer chromatography (ITLC) process. In vitro and in vivo results suggest potential anti-cancer applications of as-synthesized superparamagnetic nanoparticles.  相似文献   

6.
Direct synthesis of nanosheet Fe-ZSM-5 catalysts and their use for selective catalytic reduction (SCR) of NO x by ammonia were studied. XRD, BET, SEM, EPR, and NH3-TPD were used to understand the properties of catalysts with different iron loading. XRD confirmed the presence of the ZSM-5 crystal phase, and there was no Fe2O3 phase on the surface of the crystals. SEM showed the Fe-ZSM-5 catalysts comprised microspheres made up of nanosheets. EPR indicated that the iron was present as isolated Fe3+and FeO x oligomers uniformly dispersed throughout the crystals. NH3-TPD indicated that Fe-ZSM-5 (20,1:1) had maximum acid sites and density at approximately 250 and 450 °C, respectively. Fe-ZSM-5 (20,1:1) had the highest activity in the SCR reaction with NH3. It was also confirmed that Fe-ZSM-5 (20,1:1) had excellent resistance to SO2 and H2O under the SCR reaction conditions. The effects of water vapor and SO2, iron loading, and the Si/(Fe + Al) ratio were also investigated for these catalysts.  相似文献   

7.
Monodispersed nanostructured TiO2 spheres were obtained by the Sol–Gel method modified with ethylene glycol. The sample morphology and surface textural properties were characterized by X-ray diffraction (XRD), N2-physisorption, scanning electron microscopy (SEM), transmission electron microscopy (TEM), thermogravimetric analysis (TGA) and diffuse reflectance spectroscopy (DRS). The SEM image showed spheres with sizes ranging from 600 to 700 nm. In addition, HRTEM micrographs reveal hexagonal grains slightly elongated (20 nm). The powders present a BET surface area of 116 m2 g−1. Samples without thermal treatment and those treated at 400 °C both showed characteristic reflections of the anatase phase. The photocatalytic activity of the prepared TiO2 spheres was determined by degradation of 2,4-dichlorophenoxyacetic acid (2,4-D) in aqueous solution. Kinetics parameters have displayed than the nanostructured material present a reaction half-life time of 30 min and it was two times faster than commercial TiO2 (P25).  相似文献   

8.
N.M. Deraz  A. Alarifi 《Polyhedron》2009,28(18):4122-4130
Nanoparticles of zincl ferrite have been synthesized by the combustion method and the effect of lithia doping on their structural, morphological and magnetic properties have been studied in detail. The samples were characterized by IR, XRD, SEM, TEM and VEM. The powder XRD patterns confirm the single phase spinel structure for the synthesized materials. Transmission electron microscopy analysis revealed spherical Zn-ferrite particles with a narrow size distribution. 0.69 wt% Li2O-doping results in a decrease of the magnetization and increase of coercivity of the nanoparticles. This observation implies that, besides size, doping causes also significant structural rearrangements which in turn induce changes in the strength and the number of Fe3+(A)–O–Fe3+(B) superexchange interactions.  相似文献   

9.
Fe2O3/SiO2 nanocomposites based on fumed silica A-300 (SBET = 337 m2/g) with iron oxide deposits at different content were synthesized using Fe(III) acetylacetonate (Fe(acac)3) dissolved in isopropyl alcohol or carbon tetrachloride for impregnation of the nanosilica powder at different amounts of Fe(acac)3 then oxidized in air at 400–900 °C. Samples with Fe(acac)3 adsorbed onto nanosilica and samples with Fe2O3/SiO2 including 6–17 wt% of Fe2O3 were investigated using XRD, XPS, TG/DTA, TPD MS, FTIR, AFM, nitrogen adsorption, Mössbauer spectroscopy, and quantum chemistry methods. The structural characteristics and phase composition of Fe2O3 deposits depend on reaction conditions, solvent type, content of grafted iron oxide, and post-reaction treatments. The iron oxide deposits on A-300 (impregnated by the Fe(acac)3 solution in isopropanol) treated at 500–600 °C include several phases characterized by different nanoparticle size distributions; however, in the case of impregnation of A-300 by the Fe(acac)3 solution in carbon tetrachloride only α-Fe2O3 phase is formed in addition to amorphous Fe2O3. The Fe2O3/SiO2 materials remain loose (similar to the A-300 matrix) at the bulk density of 0.12–0.15 g/cm3 and SBET = 265–310 m2/g.  相似文献   

10.
Barium zirconate titanate, Ba(Zr0.20Ti0.80)O3 (BZT) powders were prepared by sol–gel method. These powders were characterized by thermogravimetric and differential thermogravimetric analyses (TG-DTA), X-ray diffraction (XRD) and microcopy electron transmission (TEM). The decomposition of the precursors was monitored by TG-DTA. XRD patterns reveal that BZT powders heat treated at 800 °C present single phase with perovskite-type cubic structure. TEM micrographs were employed to estimate the average particle size of the BZT powders (≈ 20 nm). The results indicate that the particle size of the BZT powders increases with the increasing of the holding time and aging temperature. The low aging temperature can reduce the agglomeration of the nanopowders. Three polyalcohols were employed as surfactants in sol–gel method: butanol (BTOL), polyethylene glycol (PEG) and polyvinyl alcohol (PVA). It is noted that PEG has a better effect on reducing agglomeration of BZT powders than that of the BTOL and PVA.  相似文献   

11.
Terbium-doped yttrium iron garnet (TbxY3−x Fe5O12; x = 0.0, 0.2, 0.4, 0.6 and 0.8) nanoparticles thin films have been prepared onto quartz substrate by sol–gel method followed by spin coating process. Annealing of the films was processed at 900 °C in air for 2 h. The structures were investigated by using an X-ray diffractometer (XRD) and a field emission scanning electron microscope (FE-SEM). The magnetic properties were studied by a vibrating sample magnetometer (VSM). The XRD patterns of the films were consistent with a single phase garnet structure. The lattice parameter was initially increased with Tb3+ concentration due to the larger size of the Tb3+ ion compared to Y3+ ion, but a decrease in lattice parameter was observed at higher Tb3+ concentration due to the effect of film’s thickness. FE-SEM micrographs reveal that the particles were highly agglomerated. The grain’s sizes for all films were in the range of 40–59 nm. The magnetic measurements at room temperature (25 °C) show that the saturation magnetization (Ms) of the films was reduced with the increase in Tb3+ ions, which due to the antiparallel alignment between Tb3+ ions and Fe3+ ions. The films illustrate normal shapes of hysteresis loops except Tb0.2Y2.8Fe5O12 and Tb0.4Y2.6Fe5O12 films exhibiting two steps increments before being saturated. The coercivity values (Hc) demonstrate non linear dependency with the terbium concentration (x).  相似文献   

12.
Iron nanoparticle deposition and stripping are observed from aqueous Fe2 + solution at pH 3 on stainless electrodes in the presence of focused microwave activation. The effects of Fe2 + concentration and microwave power are evaluated. It is shown that the resulting iron nanoparticle deposit (i) gives well-defined anodic stripping responses, (ii) is readily released into the solution phase, and (iii) is highly reactive towards chlorinated hydrocarbons such as trichloroacetate. The combined effects of increased mass transport and localized microwave heating improve pollutant degradation treatments.  相似文献   

13.
In this work three alloys, Fe74Nb6B20, Fe64Ni10Nb6B20 and Fe54Ni20Nb6B20, were obtained by mechanical alloying to analyze the influence of Ni content on Fe–Nb–B alloy formation. Structural analysis by X-ray diffraction (XRD) confirms that partial substitution of Fe by Ni favours the formation during milling of a more disordered structure. Furthermore, thermal stability study was performed by differential scanning calorimetry (DSC) because thermally induced structural changes can affect soft magnetic behaviour. After 40 h of milling time, all DSC curves show several exothermic effects on heating associated to structural relaxation and crystallization. All alloys present a crystallization process with associated activation energy values ranged between 238 and 265 kJ mol–1 related to the crystalline growth of the bcc-Fe rich phase. In alloys with Ni, a second crystallization process appears at temperatures over 500°C with activation energies 397 (10% Ni alloy) and 385 kJ mol–1 (20% Ni alloy) probably associated to the nucleation and crystalline growth of a new phase.  相似文献   

14.
In this present work, the synthesis of nanocrystalline α-Al2O3 using pure aluminum (Al) and Fe2O3 (hematite) as the precursors by mechanical alloying technique has been studied. The formation of α-Al2O3 nanocrystallites occurs during the solid-state reaction and through the reduction treatment. Also in this paper, effects of milling time on particle size and the lattice strain nanocrystalline α-Al2O3 have been investigated. Obtained powders were evaluated by scanning electron microscopy (SEM), transmission electron microscopy (TEM), differential thermal analysis (DTA), thermal gravimetric analysis (TGA) and X-ray diffraction (XRD). The obtained results indicated that a reduction reaction was completed after 2 h milling in a planetary mill. The crystallite size of obtained α-alumina (α-Al2O3) was in general about 12 nm. Finally, the results showed appropriate homogeneity and dispersion of related nanocrystalline.  相似文献   

15.
In this study, superparamagnetic iron oxide nanoparticles (SPION) embedded by folic acid (SPION-folate) were prepared by a modified co-precipitation method. The structure, size, morphology, magnetic property and relaxivity of the SPION-folate were characterized systematically by means of XRD, VSM, HRSEM and TEM and the interaction between folate and iron oxide (Fe3O4) was characterized by FT-IR. The particle size was shown to be ≈5–10 nm. To ensure biocompatibility, the interaction of these SPION with mouse connective tissue cells (adhesive) was investigated using an MTT assay. Consequently, gallium-67 labeled nanoparticles ([67Ga]-SPION-folate) were prepared using 67Ga with a high labeling efficiency (over 96%, RTLC method) and they also showed an excellent stability at room temperature for at least 2 days and were evaluated for their biodistribution in normal rats up to 24 h compared with free Ga3+ cation and [67Ga]-SPION biodistribution. The biodistribution of the tracer among 3 other folate tracers were compared, showing lower liver uptake and higher blood circulation after 24 h leading to better bioavailability. The bone:muscle, kidney:muscle, lung:muscle, stomach:muscle ratios were 9.3, 9.32, 7.6 and 5.83 respectively. The developed folate-containing nano-system can be an interesting folate receptor tracer, capable of better cell membrane permeability while possessing paramagnetic properties for thermotherapy.  相似文献   

16.
The formation of CuII–Br–FeIII-type heterobimetallic complexes was observed spectrophotometrically, given the non-additivity of the spectra from the copper(II) and iron(III) complexes. The kinetics of the oxidation of promazine radical (ptz+•) to promazine 5-oxide, by iron(III) bromides, copper(II) bromides, and a mixture of these complexes in acidic aqueous solutions, have been studied using UV–Vis spectroscopy at I = 1.0 M (H+, Cu2+, Fe3+, Br) and T = 318 K. Copper(II) inhibits the oxidation of the promazine radical to promazine sulfoxide using iron(III) complexes. A rate retardation effect, characterized by the dependence of the pseudo second-order rate constant (k II) on the copper(II) concentration k II = a/(1 + b[CuII]), can be rationalized as a result of CuII–Br–FeIII-type heterobimetallic complex formation.  相似文献   

17.
Nanocrystalline Fe-doped TiO2 powders were prepared using TiOSO4, urea, and Fe(NO3)3 · 9H2O as precursors through a hydrothermal method. The as-synthesized yellowish-colored powders are composed of anatase TiO2, identified by X-ray diffraction (XRD). The grain size ranged from 9.7 to 12.1 nm, calculated by Scherrer’s method. The specific surface area ranged from 141 to 170 m2/g, obtained by the Brunauer–Emmett–Teller (BET) method. The transmission electron microscopy (TEM) micrograph of the sample shows that the diameter of the grains is uniformly distributed at about 10 nm, which is consistent with that calculated by Scherrer’s method. Fe3+ and Fe2+ have been detected on the surface of TiO2 powders by X-ray photoelectron spectroscopy (XPS). The UV–Vis diffuse reflection spectra indicate that the light absorption thresholds of the Fe-doped TiO2 powders have been red-shifted into the visible light region. The photocatalytic activity of the Fe-doped TiO2 was evaluated through the degradation of methylene blue (MB) under visible light irradiation. The Fe-doped TiO2 powders have shown good visible-light photocatalytic activities and the maximum degradation ratio is achieved within 4.5 h.  相似文献   

18.
An ion chromatographic method has been developed for the determination of traces of Li+, Na+, K+, Ca2+, Mg2+, Sr2+, Fe3+, Cu2+, Ni2+, Co2+, Zn2+, Cd2+, Mn2+ in UO2, ThO2 powders and sintered (Th,U)O2 pellets. This new method utilizes poly-(butadiene-maleic acid) (PBDMA) coated silica cation exchange column and mixed functionality column of anion and cation exchange to achieve the separation of alkali, alkaline earths and transition metal ions, respectively. It involves matrix separation after sample dissolution by solvent extraction with TBP (tri butyl phosphate)-TOPO (tri octyl phosphine oxide)/CCl4. Interference of transition metal ions in the determination of alkali, alkaline earth metal ions are removed by using pyridine 2,6-dicarboxylic acid (PDCA) in the tartaric acid mobile phase. Mobile phase composition is optimized for the base line separation of alkali, alkaline earth and transition metal ions. Linear calibration graphs in the range 0.01–20 μg mL−1 were obtained with regression coefficients better than 0.999. The respective relative standard deviations were also determined. Recoveries of the spiked samples are within ±10% of the expected value. The developed method is authenticated by comparison with certified standards of UO2 and ThO2 powders.  相似文献   

19.
The photocatalytic activity, of undoped and Europium‐doped LaSr2AlO5 powders, has been investigated by degrading methylene blue dye in water solutions. Those powders were fabricated by a combustion method and an annealing treatment in air. All samples showed a tetragonal single phase according to by X‐ray diffraction measurements (XRD). Scanning electron microscopy (SEM) revealed irregular semi‐oval grains with sizes in the range of 3.5–4.27 μm. Photoluminescence spectrum showed sharp emission peaks at 588 nm and at 617 nm which are associated with 7F1,7F25D0 Eu3+ ion forbidden transitions, respectively, under UV light excitation of 322 nm. The methylene blue (MB) degradation under UV light (254 nm) was studied by monitoring changes in the absorbance peak of MB at 665 nm. Finally, LaSr2AlO5:Eu powders were used three times and the efficiency for the degradation of MB decreased from 100 to 61% after the third cycle of use.  相似文献   

20.
《Arabian Journal of Chemistry》2020,13(11):8347-8360
FeN -co-doped TiO2 photocatalysts are prepared by sol–gel method using titanium tetraisopropoxide, urea and iron(II) acetylacetonate as precursors of titania, nitrogen and iron, respectively. The prepared samples are analysed from chemical-physical point of view by X-ray diffraction (XRD), Raman spectroscopy, UV–Vis diffuse reflectance spectroscopy (UV–Vis DRS), specific surface area measurements and scanning electron microscopy (FESEM). UV–Vis DRS spectra evidence that the co-doping of TiO2 with N and Fe leads to the narrowing of the band gap value (2.7 eV) with respect to Fe-doped TiO2 (2.8 eV) and N-doped TiO2 (2.9–3 eV). XRD patterns show that photocatalysts are mainly in anatase phase and Fe and N ions are successfully incorporated into the TiO2 lattice. The average crystallite size of Fe-N co-doped TiO2 is slightly lower than the other samples and equal to about 7 nm and the specific surface area of the co-doped sample results to be 117 m2 g−1. Photocatalytic performances of all prepared samples are evaluated by analysing the degradation of Acid Orange 7 azo dye under visible light irradiation. Photocatalytic efficiency obtained using FeN co-doped TiO2 strongly increases compared to undoped TiO2, N-doped TiO2 and Fe-doped TiO2 photocatalysts. In detail, using the co-doped photocatalyst, dye discoloration and mineralization result equal to about 90 and 83% after 60 min of LEDs visible light irradiation, underlining the best performances of the FeN co-doped TiO2 photocatalyst both in terms of treatment time and electric energy consumption.  相似文献   

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