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1.
The SrFe12O19/poly (vinyl pyrrolidone) (PVP) composite fiber precursors were prepared by the sol-gel assisted electrospinning with ferric nitrate, strontium nitrate and PVP as starting reagents. Subsequently, the M-type strontium ferrite (SrFe12O19) nanofibers were derived from calcination of these precursors at 750–1,000 °C.The composite precursors and strontium ferrite nanofibers were characterized by Fourier transform infrared spectroscopy, X-ray diffraction, scanning electron microscopy and vibrating sample magnetometer. The structural evolution process of strontium ferrite consists of the thermal decomposition and M-type strontium ferrite formation. After calcined at 750 °C for 2 h the single M-type strontium ferrite phase is formed by reactions of iron oxide and strontium oxide produced during the precursor decomposition process. The nanofiber morphology, diameter, crystallite size and grain morphology are mainly influenced by the calcination temperature and holding time. The SrFe12O19 nanofibers characterized with diameters of around 100 nm and a necklace-like structure obtained at 900 °C for 2 h, which is fabricated by nanosized particles about 60 nm with the plate-like morphology elongated in the preferred direction perpendicular to the c-axis, show the optimized magnetic property with saturation magnetization 59 A m2 kg−1 and coercivity 521 kA m−1. It is found that the single domain critical size for these M-type strontium ferrite nanofibers is around 60 nm.  相似文献   

2.
This article demonstrates how important it is to find the optimal heating conditions when electrospun organic/inorganic composite fibers are annealed to get ceramic nanofibers in appropriate quality (crystal structure, composition, and morphology) and to avoid their disintegration. Polyvinylpyrrolidone [PVP, (C6H9NO) n ] and ammonium metatungstate [AMT, (NH4)6[H2W12O40nH2O] nanofibers were prepared by electrospinning aqueous solutions of PVP and AMT. The as-spun fibers and their annealing were characterized by TG/DTA-MS, XRD, SEM, Raman, and FTIR measurements. The 400–600 nm thick and tens of micrometer long PVP/AMT fibers decomposed thermally in air in four steps, and pure monoclinic WO3 nanofibers formed between 500 and 600 °C. When a too high heating rate and heating temperature (10 °C min−1, 600 °C) were used, the WO3 nanofibers completely disintegrated. At lower heating rate but too high temperature (1 °C min−1, 600 °C), the fibers broke into rods. If the heating rate was adequate, but the annealing temperature was too low (1 °C min−1, 500 °C), the nanofiber morphology was excellent, but the sample was less crystalline. When the optimal heating rate and temperature (1 °C min−1, 550 °C) were applied, WO3 nanofibers with excellent morphology (250 nm thick and tens of micrometer long nanofibers, which consisted of 20–80 nm particles) and crystallinity (monoclinic WO3) were obtained. The FTIR and Raman measurements confirmed that with these heating parameters the organic matter was effectively removed from the nanofibers and monoclinic WO3 was present in a highly crystalline and ordered form.  相似文献   

3.
The composite nanofibers of xSrSiO3/(100 − x)SrFe12O19 (x = 0–13 wt%) with diameters around 110 nm have been prepared by calcination of the electrospun SrSiO3/SrFe12O19/poly (vinyl pyrrolidone) (PVP) composite fibers at 800–900 °C. The composite nanofibers were characterized by Fourier transform infrared spectroscopy, X-ray diffraction, scanning electron microscopy and vibrating sample magnetometer. After calcined at 800° the M-type strontium ferrite is formed and the strontium silicate exists as an amorphous state when the calcination temperature below about 950 °C. The addition of SrSiO3 has an obvious suppression effect on the strontium ferrite grain growth and the ferrite grain size decreases from 66.9 to 33.5 nm corresponding SrSiO3 content from 0 to 9 wt% in the composite. The specific saturation magnetization (Ms) of the xSrSiO3/(100 − x)SrFe12O19 composite nanofibers exhibits a continuous reduction from 58.0 to 45.6 A m2 kg−1 with the increase of SrSiO3 content from 0 to 13 wt%. With addition of SrSiO3 from 0 to 13 wt%, the coercivity of the composite nanofibers obtained at 900 °C initially increases, reaching a maximum value 501.1 kA m−1 at the silicate content 7 wt%, and then shows a reduction tendency with the strontium silicate content increase further up to 13 wt%. This influence on the coercivity by strontium silicate can be attributed mainly to the ferrite grain growth suppression and the non-magnetic phase barrier for the domains misalignment.  相似文献   

4.
Sr0.8La0.2Zn0.2Fe11.8O19/poly(vinyl pyrrolidone) (PVP) composite fiber precursors were prepared by the sol–gel assisted electrospinning. Subsequently, the M-type ferrite Sr0.8La0.2Zn0.2Fe11.8O19 nanofibers with diameters about 120 nm were obtained by calcination of these precursors at different heat treatment conditions. The precursor and resultant Sr0.8La0.2Zn0.2Fe11.8O19 nanofibers were characterized by X-ray diffraction, scanning electron microscopy, transmission electron microscopy, energy-dispersive X-ray spectrometer and vibrating sample magnetometer. With the calcination temperature increased up to 1,000 °C for 2 h or the holding time prolonged to 12 h at 900 °C, the Sr0.8La0.2Zn0.2Fe11.8O19 particles gradually grow into a hexagonal elongated plate-like morphology due to the dimensional control along the nanofiber length. These elongated plate-like particles will be linked one by one to form the nanofiber with a necklace-like morphology. The magnetic properties of the Sr0.8La0.2Zn0.2Fe11.8O19 nanofibers are closely related to grain sizes, impurities and defects in the ferrite, which are influenced by the calcination temperature, holding time and heating rate. After calcined at 900 °C for 12 h with a heating rate of 3 °C/min, the optimized magnetic properties are achieved with the specific saturation magnetization 75.0 A m2 kg−1 and coercivity 426.3 kA m−1 for the Sr0.8La0.2Zn0.2Fe11.8O19 nanofibers.  相似文献   

5.
Nanocrystalline Mg–Cu–Zn ferrite powders were successfully synthesized through nitrate–citrate gel auto-combustion method. Characterization of the nitrate–citrate gel, as-burnt powder and calcined powders at different calcination conditions were investigated by using XRD, DTA/TG, IR spectra, EDX, VSM, SEM and TEM techniques. IR spectra and DTA/TGA studies revealed that the combustion process is an oxidation–reduction reaction in which the NO3 ion is oxidant and the carboxyl group is reductant. The results of XRD show that the decomposition of the gel indicated a gradual transition from an amorphous material to a crystalline phase. In addition, increasing the calcination temperature resulted in increasing the crystallite size of Mg–Cu–Zn ferrite powders. VSM measurement also indicated that the maximum saturation magnetization (64.1 emu/g) appears for sample calcined at 800 °C while there is not much further increase in M s at higher calcination temperature. The value of coercivity field (H c) presents a maximum value of 182.7 Oe at calcination temperature 700 °C. TEM micrograph of the sample calcined at 800 °C showed spherical nanocrystalline ferrite powders with mean size of 36 nm. The toroidal sample sintered at 900 °C for 4 h presents the initial permeability (μ i) of 405 at 1 MHz and electrical resistivity (ρ) of 1.02 × 108 Ω cm.  相似文献   

6.
Thermolysis of double complex salt [Pd(NH3)4][AuCl4]2 has been studied in helium atmosphere from ambient to 350 °C. The XAFS of Pd K and Au L3 edges and thermogravimetry measurements have been carried out to characterize the intermediates and the final product. In the temperature range 115–160 °C the complex is decomposed to form Pd(NH3)2Cl2 and AuCl4−x N x species with x ranging from 2 to 3. Subsequent heating of the intermediate up to 300 °C leads to the total loss of NH3. The Au–Cl and Au–Au bonds form the local environment of Au at the stage of decomposition while only four chlorine atoms are around Pd. At the temperature of 330 °C the Au and Pd nanoparticles as well as residues of palladium chloride are detected. The final product consists of separated Au and Pd nanoparticles.  相似文献   

7.
The calcination characteristics, sulfation conversion, and sulfation kinetics of a white mud from paper manufacture at fluidized bed combustion temperatures were investigated in a thermogravimetric analyzer. Also, the comparison between the white mud and the limestone in sulfation behavior and microstructure was made. Although the white mud and the limestone both contain lots of CaCO3, they are different in the alkali metal ions content and microstructure. It results in a marked difference in sulfation behavior between the white mud and the limestone. The CaO derived from white mud achieves the maximum sulfation conversion of 83% at about 940 °C which is 1.7 times higher than that derived from limestone at about 880 °C. The shrinking unreacted core model is appropriate to analyze the sulfation kinetics of the white mud. The chemical reaction activation energy E a and the activation energy for product layer diffusion E p for the sulfation of the white mud are 44.94 and 55.61 kJ mol−1, respectively. E p for the limestone is 2.8 times greater than that for the white mud. The calcined white mud possesses higher surface area than the calcined limestone. Moreover, the calcined white mud has more abundant pores in 4–24 nm range which is almost optimum pore size for sulfation. It indicates that the microstructure of the white mud is beneficial for SO2 removal.  相似文献   

8.
The main aim of this work was to synthesize the magnesium orthostannate doped by terbium cations and tested whether these materials can be used for colouring of the different materials, e.g. organic binder and ceramic glazes. Initial composition of pigments was counted according the general formula 2MgO(1 − x)SnO2xTbO2, where values of x varied from 0.1 to 0.5 in 0.1 steps. The simultaneous TG/DTA measurements of mixture containing tin oxide, magnesium carbonate hydroxide and terbium oxide showed that the formation of a new compound started at temperature 1,029 °C, but single-phase system was not prepared. Granulometric compositions of samples that were prepared by calcining at temperatures 1,300–1,400 °C are characterized by values of median (d 50) in range 4–8 μm. The calcining temperature 1,500 °C caused the increase of the particle sizes at around 12 μm. The composition of sample 2MgO–1.5SnO2–0.5TbO2 and heating temperature 1,500 °C are the most suitable conditions for preparation of colourfully interesting pigment that can be recommended also for colouring of ceramic glazes. Especially, for colouring of decorative lead containing glaze G 07091 containing 5 wt% of PbO and 8 wt% of Al2O3.  相似文献   

9.
Toward achieving selective catalytic reduction of NO x by hydrocarbons at low temperatures (especially lower than 200 °C), C2H2 selective reduction of NO x was explored on H-mordenite (H-MOR) catalysts in dielectric barrier discharge (DBD) plasma. This work reported significant synergistic effects of DBD plasmas and H-MOR catalysts for C2H2 selective reduction of NO x at low temperatures (100–200 °C ) and across a wide range of O2 content (0–15%). At 100 °C, NO x conversions were 3.3, 11.6 and 66.7% for the plasma alone, catalyst alone and in-plasma catalysis (IPC) cases (with a reactant gas mixture of 500 ppm NO, 500 ppm C2H2, 10% O2 in N2, GHSV = 12,000 h−1 and input energy density of 125 J L 1), respectively. At 200 °C, NO x conversions were 3.8, 54.0 and 91.4% for the above three cases, respectively. Also, strong signals of hydrogen cyanide (HCN) byproduct were observed in the catalyst alone system by an on-line mass spectrometer. By contrast, almost no HCN was detected in the IPC system.  相似文献   

10.
Nanocomposites of ferrite and ferroelectric phases are attractive functional ceramic materials. In this work, the nanocomposite Ni1−x Co x Fe2O4–BaTiO3(x = 0.2, 0.3, 0.4, 0.5) fibers with fine diameters of 3 ~ 7 μm and high aspect ratios were synthesized by the organic gel-thermal decomposition process from the raw materials of citric acid and metal salts. The structure, thermal decomposition process and morphologies of the gel precursors and the resultant fibers derived from thermal decomposition of the gel precursors were characterized by Fourier transform infrared spectroscopy, thermogravimetric differential thermal analysis, X-ray diffraction and scanning electron microscopy. The magnetic properties of the nanocomposite fibers were measured by vibrating sample magnetometer. The nanocomposite fibers of ferrite Ni1−x Co x Fe2O4 and perovskite BaTiO3 are formed at the calcination temperature of 900 °C for 2 h. The average grain sizes of Ni1−x Co x Fe2O4 and BaTiO3 in the nanocomposite fibers increase from about 15 nm to approximately 67 nm with the increasing calcination temperatures from 900 to 1,180 °C. The saturation magnetization of the nanocomposite Ni1−x Co x Fe2O4–BaTiO3(x = 0.2, 0.3, 0.4, 0.5) fibers increases with the increase of grain sizes of Ni1−x Co x Fe2O4 and Co content, while the coercivity reaches a maximum value at the single-domain size of about 65 nm of Ni0.5Co0.5Fe2O4 obtained at the calcination temperature of 1,100 °C.  相似文献   

11.
In the present research, CO2 and SO2 binding ability of different oil shale ashes and the effect of pre-treatment (grinding, preceding calcination) of these ashes on their binding properties and kinetics was studied using thermogravimetric, SEM, X-ray, and energy dispersive X-ray analysis methods. It was shown that at 700 °C, 0.03–0.28 mmol of CO2 or 0.16–0.47 mmol of SO2 was bound by 100 mg of ash in 30 min. Pre-treatment conditions influenced remarkably binding parameters. Grinding decreased CO2 binding capacities, but enhanced SO2 binding in the case of fluidized bed ashes. Grinding of pulverized firing ashes increased binding parameters with both gases. Calcination at higher temperatures decreased binding parameters of both types of ashes with both gases studied. Clarification of this phenomenon was given. Kinetic analysis of the binding process was carried out, mechanism of the reactions and respective kinetic constants were determined. It was shown that the binding process with both gases was controlled by diffusion. Activation energies in the temperature interval of 500–700 °C for CO2 binding with circulating fluidized bed combustion ashes were in the range of 48–82 kJ mol−1, for SO2 binding 43–107 kJ mol−1. The effect of pre-treatment on the kinetic parameters was estimated.  相似文献   

12.
LiVPO4F/C composites with better electrochemical performance were prepared by calcination of LiF and amorphous vanadium phosphorus oxide (VPO) intermediate synthesized by a sol–gel method using H3PO4, V2O5 and citric acid as raw materials. The properties of LiVPO4F/C composites were investigated by X-ray diffraction (XRD), scanning electron microscopy (SEM) and electrochemical tests. The analysis of XRD patterns and Fourier transform infrared spectra (FTIR) reveal that VPO intermediate prepared by sol–gel method is amorphous and VPO4 may exist in VPO intermediate. The compositions of LiVPO4F/C composites are related to the calcination temperature for preparation of amorphous VPO/C intermediate and LiVPO4F/C composite prepared by VPO/C synthesized at 700°C consists of a single crystal phase of LiVPO4F. The electrochemical tests show that LiVPO4F/C composite prepared by VPO/C synthesized at 700°C exhibits higher discharge capacity and excellent cycle performance. This LiVPO4F/C composite displays discharge capacity of 133 mAh g−1 at 0.5 C (78 mA g−1) and remains capacity retention of 96.8% after 30 cycles, even at a high rate of 5 C, the composite exhibits high discharge capacity of 115 mAh g−1 and capacity retention of 97% after 100 cycles.  相似文献   

13.
Olivine-structured LiCoPO4 is synthesized by a Pechini-type polymer precursor method. The structure and the morphology of the compounds are studied by the Rietveld-refined X-ray diffraction, scanning electron microscopy, Brunauer, Emmett, and Teller surface area technique, infrared spectroscopy, and Raman spectroscopy techniques, respectively. The ionic conductivity (σ ionic), dielectric, and electric modulus properties of LiCoPO4 are investigated on sintered pellets by impedance spectroscopy in the temperature range, 27–50 °C. The σ (ionic) values at 27 and 50 °C are 8.8 × 10−8 and 49 × 10−8 S cm−1, respectively with an energy of activation (E a) = 0.43 eV. The electric modulus studies suggest the presence of non-Debye type of relaxation. Preliminary charge–discharge cycling data are presented.  相似文献   

14.
Electrical conductivity in the monoclinic Li2TiO3, cubic Li1.33Ti1.67O4, and in their mixture has been studied by impedance spectroscopy in the temperature range 20–730 °C. Li2TiO3 shows low lithium ion conductivity, σ300≈10–6 S/cm at 300 °C, whereas Li1.33Ti1.67O4 has 3×10–8 at 20 °C and 3×10–4 S/cm at 300 °C. Structural properties are used to discuss the observed conductivity features. The conductivity dependences on temperature in the coordinates of 1000/T versus logeT) are not linear, as the conductivity mechanism changes. Extrinsic and intrinsic conductivity regions are observed. The change in the conductivity mechanism in Li2TiO3 at around 500–600 °C is observed and considered as an effect of the first-order phase transition, not reported before. Formation of solid solutions of Li2– x Ti1+ x O3 above 900 °C significantly increases the conductivity. Irradiation by high-energy (5 MeV) electrons causes defects and the conductivity in Li2TiO3 increases exponentially. A dose of 144 MGy yields an increase in conductivity of about 100 times at room temperature. Electronic Publication  相似文献   

15.
Electrochromic titanium oxide (TiO2) films were deposited on ITO/glass substrates by chemical solution deposition (CSD). The stock solutions were spin-coated onto substrates and then heated at various temperatures (200–500 °C) in various oxygen concentrations (0–80%) for 10 min. The effects of the processing parameters on the electrochromic properties of TiO2 films were investigated. X-ray diffraction measurements demonstrated that the amorphous TiO2 films were crystallized to form anatase films above 400 °C. The electrochromic properties and transmittance of TiO2 films were measured in 1 M LiClO4–propylene carbonate (PC) non-aqueous electrolyte. An amorphous 350 nm-thick TiO2 film that was heated at 300°C in 60% ambient oxygen exhibited the maximum transmittance variation (ΔT%), 14.2%, between the bleached state and the colored state, with a ΔOD of 0.087, Q of 10.9 mC/cm2, η of 7.98 cm2/C and x in Li x ClO4 of 0.076 at a wavelength (λ) of 550 nm.  相似文献   

16.
Compositionally graded Ba1−x Sr x TiO3 (BST) (0 ≤ x ≤ 0.4) thin films were fabricated on Pt/Ti/SiO2/Si and YSZ/Pt/Ti/SiO2/Si substrates by a modified sol–gel technique. The YSZ buffer layer was prepared by RF magnetron sputtering. The microstructure of the graded BST films was investigated by X-ray diffraction (XRD), scanning electron microscopy (SEM), and atomic force microscopy (AFM). The results showed that all the films have uniform and crack-free surface with a perovskite structure. The graded BST film with an YSZ buffer layer has larger dielectric constant and lower dielectric loss. The leakage current density of the graded BST film with an YSZ buffer layer lowers two orders than the film without buffer layer. The improved electric properties of the graded films with an YSZ buffer layer was attributed to the YSZ buffer layer act as an excellent seeding layer to enhance the graded BST film growth.  相似文献   

17.
This paper describes the synthesis of ZrW2O8 by the use of an aqueous citrate-gel method in order to prepare a fine, pure and homogeneous oxide mixture suitable for ceramic processing. The thermal expansion coefficient thus obtained for α-ZrW2O8 is −10.6 × 10−6 °C−1 (50–125 °C) whereas for the β-ZrW2O8 a value of −3.2 × 10−6 °C−1 (200–300 °C) is obtained. The advantages of the use of a sol–gel method is expressed in the very homogeneous end-products. The paper describes crystallographic data, morphological structure and the thermal expansion properties of the ZrW2O8 material. Moreover, photoluminescence and photochromic properties specific to the precursor gel are described and analyzed. These effects support our views that the precursors show homogeneity up to nanometer level.  相似文献   

18.
Nano-composites of SnO(V2O3) x (x = 0, 0.25, and 0.5) and SnO(VO)0.5 are prepared from SnO and V2O3/VO by high-energy ball milling (HEB) and are characterized by X-ray diffraction (XRD), scanning electron microscopy, and high-resolution transmission electron microscopy techniques. Interestingly, SnO and SnO(VO)0.5 are unstable to HEB and disproportionate to Sn and SnO2, whereas HEB of SnO(V2O3) x gives rise to SnO2.VO x . Galvanostatic cycling of the phases is carried out at 60 mA g−1 (0.12 C) in the voltage range 0.005–0.8 V vs. Li. The nano-SnO(V2O3)0.5 showed a first-charge capacity of 435 (±5) mAh g−1 which stabilized to 380 (±5) mAh g−1 with no noticeable fading in the range of 10–60 cycles. Under similar cycling conditions, nano-SnO (x = 0), nano-SnO(V2O3)0.25, and nano-SnO(VO)0.5 showed initial reversible capacities between 630 and 390 (±5) mAh g−1. Between 10 and 50 cycles, nano-SnO showed a capacity fade as high as 59%, whereas the above two VO x -containing composites showed capacity fade ranging from 10% to 28%. In all the nano-composites, the average discharge potential is 0.2–0.3 V and average charge potential is 0.5–0.6 V vs. Li, and the coulombic efficiency is 96–98% after 10 cycles. The observed galvanostatic cycling, cyclic voltammetry, and ex situ XRD data are interpreted in terms of the alloying–de-alloying reaction of Sn in the nano-composite “Sn-VO x -Li2O” with VO x acting as an electronically conducting matrix.  相似文献   

19.
This paper describes a procedure of preparing sodium tantalite nanofibers for the first time. Sodium tantalite nanofibers were synthesised by electrospinning a sol–gel precursor solution of poly(vinyl pyrrolidone)/sodium tantalite, followed by careful sintering of the as-electrospun composite fibers at 550 °C for 3 h. The morphology, microstructure and crystal phase were investigated by transmission electron microcopy and X-ray diffraction. The optical property was characterized by ultraviolet–visible (UV–vis) spectrometer. Typical nanofibers were with diameter between 70 and 90 nm and length exceeding 0.1 mm. An unusual phenomenon, the red-shift of optical absorption band edge happened, indicated the fabricated NaTaO3 nanofibers were potential good candidates for photocatalytic application. The experiment photodegradation of methylene blue by NaTaO3 nanofibers under UV light irradiation was performed.  相似文献   

20.
Tetragonal copper ferrite (CuFe2O4) nanofibers were fabricated by electrospinning method using a solution that contained poly(vinyl pyrrolidone) (PVP) and Cu and Fe nitrates as alternative metal sources. The as-spun and calcined CuFe2O4/PVP composite samples were characterized by TG-DTA, X-ray diffraction, FT-IR, and SEM, respectively. After calcination of the as-spun CuFe2O4/PVP composite nanofibers (fiber size of 89 ± 12 nm in diameter) at 500 °C in air for 2 h, CuFe2O4 nanofibers of 66 ± 13 nm in diameter having well-developed tetragonal structure were successfully obtained. The crystal structure and morphology of the nanofibers were influenced by the calcination temperature. After calcination at 600 and 700 °C, the nature of nanofibers changed which was possibly due to the reorganization of the CuFe2O4 structure at high temperature, and a fiber structure of packed particles or crystallites was prominent. Crystallite size of the nanoparticles contained in nanofibers increases from 7.9 to 23.98 nm with increasing calcination temperature between 500 and 700 °C. Room temperature magnetization results showed a ferromagnetic behavior of the calcined CuFe2O4 samples, having their specific saturation magnetization (Ms) values of 17.73, 20.52, and 23.98 emu/g for the samples calcined at 500, 600, and 700 °C, respectively.  相似文献   

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