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1.
The Ni0.75Co2.25O4 catalysts were prepared by a coprecipitation method and modified with cesium cations by impregnation with a solution of cesium nitrate or cesium nitrate with citric acid and ethylene glycol additives (the Pechini method). The catalysts obtained were investigated by X-ray diffraction analysis, the BET method, X-ray photoelectron spectroscopy, temperature-programmed reduction, and the temperatureprogrammed desorption of oxygen. The activity of the samples in a reaction of nitrous oxide decomposition was determined at temperatures of 200–300°C, in particular, in the presence of oxygen and water in the reaction mixture. It was found that the use of the Pechini method for supporting Cs makes it possible to obtain a more active catalyst, as compared with that prepared by impregnation with cesium nitrate, at the same cesium content (~2%) of the samples.  相似文献   

2.
KGd(WO4)2 (KGW) particles were synthesized at 3.5, 5.5 and 7.5 pH values by Pechini polymeric complex sol–gel method using potassium nitrate, gadolinium nitrate, ammonium paratungstate, citric acid and ethylene glycol as starting materials. Deionized water was used as solvent. Polymeric precursor gel was formed with citric acid as complexing agent and ethylene glycol as binder. Synthesized gel was analyzed by FT-IR spectroscopy. Prepared precursor gels were further annealed using resistive and microwave processes at 550 and 700 °C, respectively. The properties of heat treated samples were characterized by powder XRD, FT-IR, Raman and SEM analysis to understand the crystallinity, organic liberation, tungstate ribbon formation and surface morphology, respectively. The phase formation and different phases of intermediate oxides in pre-fired samples were investigated by powder XRD. Organic liberation in the samples in relation to temperature, and the carbon content in the pre-fired powder was analyzed using FT-IR spectrum. Raman spectrum reveals the formation of tungsten ribbons as well as the quality of the samples. The morphological changes at different synthesis conditions were observed with SEM micrographs.  相似文献   

3.
Solid solution phases of a formula Fe8V10W16–xMoxO85 where 0≤x≤4, have been obtained, possessing a structure of the compound Fe8V10W16O85. It was found on the base of XRD and DTA investigations that these solution phases melted incongruently, with increasing the value of x, in the temperature range from 1108 (x=0) to 1083 K (x=4) depositing Fe2WO6 and WO3. The increase of the Mo6+ ions content in the crystal lattice of Fe8V10W16O85 causes the lattice parameters a=b contraction with cbeing almost constant. IR spectra of the Fe8V10W16–xMoxO85 solid solution phases have been recorded.  相似文献   

4.
Pure tungstophosphoric acid, potassium tungstophosphate, and cesium tungstophosphate with varying extent of substitution of protons by Cs or K ions x (x = 1, 2, 2.5, and 3) have been prepared and are supported on silica by the wet impregnation method. The extent of loading was fixed at 20 wt %. For the sake of comparison, unloaded Cs x and K x (x = 1) salts of tungstophosphoric acid were prepared by the precipitation method. The supported catalysts were characterized by FT-IR, XRD, specific surface area measurements, and catalytic conversion of tert-butanol. The results revealed that the catalytic conversion of tert-butanol proceeds mainly via dehydration yielding isobutene. The Cs1PW/SiO2, HPW/SiO2, and K1PW/SiO2 catalysts were more active than their unsupported samples. The previous solids showed greater catalytic activity and stability. Unexpectedly, substitution of one proton of tungstophosphoric acid by a cesium or potassium ion exerted no measurable effect on the catalytic activity of the treated solids, in spite of decreasing the Brønsted acidity of Cs1PW/SiO2 and K1PW/SiO2 indicating that the acidity of HPW/SiO2 decrease may be due to the interaction between HPW and the SiO2 surface. On the other hand, significant decrease in the catalytic activity took place upon increasing the cation content (x) to x = 2, 2.5, and 3.  相似文献   

5.
The Ru-Cs+/MgO and Ru-Cs+/γ-Al2O3 catalysts, which were prepared by an impregnation method using RuOHCl3 and Cs2CO3 as precursor compounds and reduced with H2 at 450°C, are characterized by X-ray diffraction, high-resolution transmission electron microscopy (with X-ray microanalysis), and X-ray photoelectron spectroscopy (XPS). The Cs+/MgO(Al2O3) systems, Ru-Cs+ black, and model systems prepared by cesium sputtering onto polycrystalline ruthenium foil are studied as reference samples. It is found that, in the Ru-Cs+/MgO sample, cesium is present as a Cs2 + xO cesium suboxide, which weakly interacts with the support, localized on the surface of Ru particles or near them. In the case of Ru-Cs+/γ-Al2O3, cesium occurs as a species that is tightly bound to the support; this is likely surface cesium aluminate, which prevents promoter migration to Ru particles. The Ru-Cs+/MgO sample exhibits a considerable shift of the Ru3d line in the XPS spectra toward lower binding energies, as compared to the bulk metal. It is hypothesized that this shift is due to a decrease in the electron work function from the surface of ruthenium because of the polarizing effect of Cs+ ions in contact with Ru particles. Based on the experimental results, the great difference between the catalytic activities of the Ru-Cs+/MgO and Ru-Cs+/γ-Al2O3 systems in ammonia synthesis at 250–400°C and atmospheric pressure is explained.  相似文献   

6.
Ni0.5Zn0.5Fe2O4 nanofibers with addition of 0–5 wt% Bi2O3 were synthesized by calcination of the electrospun polyvinylpyrrolidone/inorganic composite nanofibers at the temperature below the melting point of Bi2O3. The effects of Bi2O3 addition on the phase structure, morphology and magnetic properties of the nanofibers were investigated by means of X-ray diffraction, scanning electron microscopy, transmission electron microscopy, energy dispersive X-ray spectroscopy, selected area electron diffraction and vibrating sample magnetometer. It is found that the nanofiber diameter, crystallite size and magnetic parameters can be effectively tuned by simply adjusting the amount of Bi2O3 addition. The average diameter of Ni0.5Zn0.5Fe2O4 nanofibers doped with different contents of Bi2O3 ranges from 40 to 63 nm and gradually decreases with increasing Bi2O3 content. The addition of Bi2O3 does not induce the phase change and all the samples are a single-phase spinel structure. The amorphous Bi2O3 tends to concentrate on the nanoparticle surface and/or grain boundary and can retard the particles motion as well as the grain growth, resulting in a considerable reduction in grain size compared to the pristine sample. The specific saturation magnetization and coercivity of the nanofibers gradually decrease with the increase of Bi2O3 amount. Such behaviors are explained on the basis of chemical composition, surface effect, domain structure and crystal anisotropy.  相似文献   

7.
Li4Ti5O12/Li2TiO3 composite nanofibers with the mean diameter of ca. 60 nm have been synthesized via facile electrospinning. When the molar ratio of Li to Ti is 4.8:5, the Li4Ti5O12/Li2TiO3 composite nanofibers exhibit initial discharge capacity of 216.07 mAh g?1 at 0.1 C, rate capability of 151 mAh g?1 after being cycled at 20 C, and cycling stability of 122.93 mAh g?1 after 1000 cycles at 20 C. Compared with pure Li4Ti5O12 nanofibers and Li2TiO3 nanofibers, Li4Ti5O12/Li2TiO3 composite nanofibers show better performance when used as anode materials for lithium ion batteries. The enhanced electrochemical performances are explained by the incorporation of appropriate Li2TiO3 which could strengthen the structure stability of the hosted materials and has fast Li+-conductor characteristics, and the nanostructure of nanofibers which could offer high specific area between the active materials and electrolyte and shorten diffusion paths for ionic transport and electronic conduction. Our new findings provide an effective synthetic way to produce high-performance Li4Ti5O12 anodes for lithium rechargeable batteries.  相似文献   

8.
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   

9.
SiO2/TiO2 hybrid nanofibers were prepared by electrospinning and applied for photocatalytic degradation of methylene blue (MB). The phase structure, specific surface area, and surface morphologies of the SiO2/TiO2 hybrid nanofibers were characterized through thermogravimetry (TG), X-ray diffraction (XRD) analysis, Brunauer–Emmett–Teller (BET) analysis, scanning electron microscopy (SEM), etc. XRD measurements indicated that doping of silica into TiO2 nanofibers can delay the phase transition from anatase to rutile and decrease the grain size. SEM and BET characterization proved that silica doping can remarkably enhance the porosity of the SiO2/TiO2 hybrid nanofibers. The MB adsorption capacity and photocatalytic activity of the SiO2/TiO2 hybrid nanofibers were distinguished experimentally. It was found that, although increased silica doping content could enhance the MB adsorption capacity, the intrinsic photocatalytic activity gradually dropped. The SiO2 (10 %)/TiO2 composite nanofibers exhibited the highest MB degradation rate, being superior to SiO2 (20 %)/TiO2 or pure TiO2.  相似文献   

10.
Trimetallic NiMoW/Al2O3 catalyst was prepared using mixed H4SiMo3W9O40 heteropoly acid of Keggin structure and nickel citrate. Bimetallic NiMo/Al2O3 and NiW/Al2O3 catalysts based on H4SiMo12O40 and H4SiW12O40, respectively, were synthesized as reference samples. The use of mixed H4SiMo3W9O40 heteropoly acid as an oxide precursor allows the tungsten sulfidation degree and the degree of promotion of active phase particles to be increased. The hydrodesulfurization activity is enhanced as compared to NiW/Al2O3 catalyst. The synergistic enhancement of the activity of the NiMo3W9/Al2O3 catalyst relative to the bimetallic analogs is probably caused by formation of new mixed promoted active sites for direct desulfurization.  相似文献   

11.
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   

12.
TiO2 nanofibers were prepared from tetrabutyl titanate sol precursors by using electrospun method. X-ray diffraction (XRD) and atomic force microscope (AFM) were used to characterize their crystal structure and morphology feature. The results demonstrated that TiO2 nanofibers possessed anatase phase and the average diameter of TiO2 nanofibers was about 150 nm. The photocatalytic property of TiO2 nanofibers was evaluated for the photodecomposition of methyl orange solution. And TiO2 nanofibers exhibited high photocatalytic activities with transfer efficiency about 100% after 20 min.  相似文献   

13.
Mn3O4 powders have been produced from Electrolytic Manganese Residue (EMR). After leaching of EMR in sulfuric acid, MnSO4 solution containing various ions was obtained. Purifying the solution obtained and then adding aqueous alkali to the purified MnSO4 solution, Mn(OH)2 was prepared. Two methods were employed to produce Mn3O4. One way was oxidation of Mn(OH)2 in aqueous phase under atmosphere pressure to obtain Mn3O4. The other way was roasting Mn(OH)2 precursors in the range of 500°C to 700°C. The prepared samples were investigated by using several techniques including X-ray powder diffraction (XRD), Fourier Transformation Infra-Red (FTIR) spectra, and Brunauer-Emmett-Teller (BET) specific surface area instrument. Particle distribution and magnetic measurements were carried out on laser particle size analyzer, vibrating sample magnetometer (VSM). Through XRD, FTIR and determination of total Mn content (TMC), the products prepared were confirmed to be a single phase Mn3O4. BET specific surface areas can reach to 32 m2 g−1. The results indicated that products synthesized by aqueous solution oxidation method had higher specific surface areas and smaller particle size than those prepared by means of roasting. However the products prepared using the above two methods showed no obvious differences in magnetic property.   相似文献   

14.
Heterostructured SnO2/CuO nanofibers with a hollow morphology were successfully fabricated by a one-step electrospinning method. The electrospun nanofibers were transformed into hollow nanostructures in the presence of camphene after a calcination process, and the obtained samples were characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), UV-vis diffuse reflection spectroscopy (DRS), photoluminescence spectra (PL), and photodegradation measurements. The scanning electron microscopy (SEM) images displayed a rough and hollow structure for the obtained nanofibers. X-ray photoelectron spectroscopy (XPS) and energy-dispersive X-ray spectroscopy (EDX) identified the molecular composition and chemical interactions of the nanofibers. Photoluminescent (PL) measurements indicated that a recombination of the photoinduced electrons and holes was further inhibited due to the hollow nanostructure. Furthermore, the photodegradation of methylene blue suggested that the heterostructured SnO2/CuO hollow nanofibers possessed higher charge separation and photodegradation abilities than those of the other samples under visible light irradiation. This work can be potentially applied to the fabrication of other inorganic oxide photocatalysts with enhanced photodegradation activity in the field of environmental remediation.  相似文献   

15.
It has been shown that cesium hydrogen phosphotungstate Cs2.5H0.5PW12O40 is a promising catalyst of the gas-phase carbonylation of dimethoxymethane (DMM) to methyl methoxyacetate (MMA). This catalyst provided the MMA selectivity and yield of 54% and 40%, respectively, under mild experimental conditions: T = 110°C, P = 10 bar, and GHSV = 6000 h–1 for DMM/CO/Ar = 4/76/20 mol/mol/mol. The carbonylation of DMM to MMA is accompanied by side reactions of DMM disproportionation into dimethyl ether (DME) and methyl formate (MF), as well as by secondary side reactions of MF decomposition into methanol and CO and methanol dehydration into DME.  相似文献   

16.
(1.2–8.3)%FeOх/Al2O3 monolith catalysts have been prepared by impregnating alumina with aqueous solutions of iron(III) nitrate and oxalate and have been tested in NH3 oxidation and in the selective decomposition of N2O in mixtures resulting from ammonia oxidation over a Pt–Rh gauze pack under conditions of nitric acid synthesis (800–900°C). In the case of the support calcined at 1200°C, the catalyst is dominated by bulk Fe2O3 particles localized on the Al2O3 surface. The activity of these samples in both reactions decreases with a decreasing active component content, thus limiting the potential of Fe2(C2O4)3 · 5H2O, an environmentally friendlier but poorly soluble compound, as a substitute for Fe(NO3)3 · 9H2O. Decreasing the support calcination temperature to 1000°C or below leads to the formation of a highly defective Fe–Al–O solid solution in the (1.2–2.7)%FeOх/Al2O3 catalysts. The surface layers of the solid solution are enriched with iron ions or stabilize ultrafine FeOх particles. The catalytic activity of these samples in both reactions is close to the activities measured for ~8%FeOх/Al2O3 samples prepared using iron nitrate.  相似文献   

17.
Spinel LiMn2−x Ni x O4 compounds doped with a range of Ni (x=0–0.06) were synthesized by a spray-drying method. The structure and morphology characteristics of the powders were studied in detail by means of X-ray diffraction (XRD), scanning electron microscopy, and transmission electron microscopy. The XRD data reveal that all the samples have well-defined spinel structure, but, with the increase in Ni content, the doped lithium manganese spinels have smaller lattice constant. The undoped and doped spinel LiMn2O4 particles are fine, narrowly distributed, and well crystallized. The electrochemical characteristics of the samples are measured in the coin-type cells in a potential range of 3.2–4.35 V vs Li/Li+. All cyclic voltammogram curves exhibit two pairs of redox reaction peaks, but, among them, there are some differences about the peak split. With the increase in the Ni content, the specific capacities of the samples decrease slightly, but their cyclic ability increases.  相似文献   

18.
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   

19.
Polymolybdates of the composition Cs2Mo4O13 (1) and Cs4Mo8O26 · 4H2O (2) are synthesized under hydrothermal conditions from a mixture containing (NH4)6Mo7O24 · 4H2O and CsCl at pH 2.5 and 3.6, respectively.  相似文献   

20.
Solid solutions based on cesium monogallate CsGaO2 are synthesized in the Ga2O3-TiO2-Cs2O system. Their crystalline structure and also temperature and concentration conductivity dependences are studied. The cesium cation character of conductivity is confirmed. The most conducting samples contain an excess of cesium oxide and have the structure of high-temperature γ-modification of KAlO2. Their specific conductivity is (5.0–6.7) × 10?3 S cm?1 at 400 °C, (2.5–5.0) × 10?2 S cm?1 at 700°C at the activation energy of 33–35 kJ/mol?1.  相似文献   

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