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1.
A novel microwave dielectric powder with composition of Ca2Zn4Ti16O38 was synthesized through a citrate sol-gel process. The development of crystalline phases with heat-treating temperature for the gel derived powders was evaluated by using thermo-gravimetric analysis and X-ray powder diffraction analysis techniques. The pure phase of Ca2Zn4Ti16O38 with crichtonite crystal structure was obtained at relatively low temperature of 1000 °C. The synthesized powder has high reactivity and the dense ceramics with single crystalline phase were obtained at low sintering temperature of 1100 °C. Impedance spectroscopy and microwave dielectric measurements on sintered samples showed the present compound to be a modest dielectric insulator with excellent dielectric properties of εr∼47-49, Qf value ∼27,800-31,600 GHz and τf∼+45 to +50 ppm/°C. It shows comparable microwave dielectric properties to other moderate-permittivity microwave dielectrics, but much lower sintering temperature of 1100 °C.  相似文献   

2.
The NO catalytic direct decomposition was studied over La2CuO4 nanofibers, which were synthesized by using single walled carbon nanotubes (CNTs) as templates under hydrothermal condition. The composition and BET specific surface area of the La2CuO4 nanofiber were La2Cu0.882+Cu0.12+O3.94 and 105.0 m2/g, respectively. 100% NO conversion (turnover frequency-(TOF): 0.17 gNO/gcatalyst s) was obtained over such nanofiber catalyst at temperatures above 300 °C with the products being only N2 and O2. In 60 h on stream testing, either at 300 °C or at 800 °C, the nanofiber catalyst still showed high NO conversion efficiency (at 300 °C, 98%, TOF: 0.17 gNO/gcatalyst s; at 800 °C, 96%, TOF: 0.16 gNO/gcatalyst s). The O2 and NO temperature programmed desorption (TPD) results indicated that the desorption of oxygen over the nanofibers occurred at 80-190 and 720-900 °C; while NO desorption happened at temperatures of 210-330 °C. NO and O2 did not competitively adsorb on the nanofiber catalyst. For outstanding the advantage of the nanostate catalyst, the usual La2CuO4 bulk powder was also prepared and studied for comparison.  相似文献   

3.
Preparation of two novel mixed metal oxide ceramic materials, namely magnesium neodymium tantalum oxide (Mg2NdTaO6) and magnesium lanthanum tantalum oxide (Mg2LaTaO6) by conventional solid-state reaction method is reported in this paper. The crystal structure of these new compounds, were studied by indexing the X-ray diffraction patterns, powder pattern calculation and profile fitting. They were found to have a defective cubic pyrochlore structure, with the A site being randomly occupied by Mg and La/Nd, while, Ta and Mg are randomly distributed at the B site. The formula assigned were (MgNd)(MgTa)O6 and (MgLa)(MgTa)O6. The variation of dielectric constant, dielectric loss and conductivity of sintered pellets of these materials with applied frequencies in the range of 30 Hz-1 MHz were studied at room temperature. These room temperature studies at 1 MHz gave dielectric constant values of 24.8 and 25.35; conductivity values of 7.75×10−6 and 8.27×10−6 S/m as well as dielectric loss values of 0.0055 and 0.006 for Mg2NdTaO6 and Mg2LaTaO6, respectively. These new pyrochlore compounds were found to have dielectric constant, dielectric loss and conductivity values in the range suitable for possible electronic ceramic applications.  相似文献   

4.
Garnet-structure related metal oxides with the nominal chemical composition of Li5La3Nb2O12, In-substituted Li5.5La3Nb1.75In0.25O12 and K-substituted Li5.5La2.75K0.25Nb2O12 were prepared by solid-state reactions at 900, 950, and 1000 °C using appropriate amounts of corresponding metal oxides, nitrates and carbonates. The powder XRD data reveal that the In- and K-doped compounds are isostructural with the parent compound Li5La3Nb2O12. The variation in the cubic lattice parameter was found to change with the size of the dopant ions, for example, substitution of larger In3+(rCN6: 0.79 Å) for smaller Nb5+ (rCN6: 0.64 Å) shows an increase in the lattice parameter from 12.8005(9) to 12.826(1) Å at 1000 °C. Samples prepared at higher temperatures (950, 1000 °C) show mainly bulk lithium ion conductivity in contrast to those synthesized at lower temperatures (900 °C). The activation energies for the ionic conductivities are comparable for all samples. Partial substitution of K+ for La3+ and In3+ for Nb5+ in Li5La3Nb2O12 exhibits slightly higher ionic conductivity than that of the parent compound over the investigated temperature regime 25-300 °C. Among the compounds investigated, the In-substituted Li5.5La3Nb1.75In0.25O12 exhibits the highest bulk lithium ion conductivity of 1.8×10−4 S/cm at 50 °C with an activation energy of 0.51 eV. The diffusivity (“component diffusion coefficient”) obtained from the AC conductivity and powder XRD data falls in the range 10−10-10−7 cm2/s over the temperature regime 50-200 °C, which is extraordinarily high and comparable with liquids. Substitution of Al, Co, and Ni for Nb in Li5La3Nb2O12 was found to be unsuccessful under the investigated conditions.  相似文献   

5.
CsAlSi5O12 crystals were synthesized at high temperature by slow cooling of a vanadium oxide flux. Single-crystal X-ray diffraction structure analysis and electron microprobe analyses yielded the microporous CAS zeolite framework structure of Cs0.85Al0.85Si5.15O12 composition. High-temperature single-crystal and powder X-ray diffraction studies were utilized to analyze anisotropic thermal expansion. Rietveld refined cell constants from powder diffraction data, measured in steps of 25 °C up to 700 °C, show a significant decrease in expansion above 500 °C. At 500 °C, a displacive, static disorder-dynamic disorder-type phase transition from the acentric low-temperature space group Ama2 to centrosymmetric Amam (Cmcm in standard setting) was found. Thermal expansion below the phase transition is governed by rigid-body TO4 rotations accompanied by stretching of T-O-T angles. Above the phase transition at 500 °C all atoms, except one oxygen (O6), are fixed on mirror planes. Temperature-dependent polarized Raman single-crystal spectra between −270 and 300 °C and unpolarized spectra between room temperature and 1000 °C become increasingly less resolved with rising temperature confirming the disordered static-disordered dynamic type of the phase transition.  相似文献   

6.
Formation of nano-sized Y2O3-doped CeO2 (YCO) was observed in the chemical reaction between proton conducting Y2O3-doped BaCeO3 (BCY) and CO2 in the temperature range 700-1000 °C, which is generally prepared by wet-chemical methods that include sol-gel, hydrothermal, polymerization, combustion, and precipitation reactions. BCY can capture CO2 of 0.13 g per ceramic gram at 700 °C, which is comparable to that of the well-known Li2ZrO3 (0.15 g per ceramic gram at 600 °C). Powder X-ray diffraction (PXRD), energy dispersive X-ray analysis (EDX), laser particle size analysis (LPSA), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and ac impedance spectroscopy were employed to characterize the reaction product obtained from reaction between BCY and CO2 and subsequent acid washing. PXRD study reveals presence of fluorite-like CeO2 (a=5.410 (1) Å) structure and BaCO3 in reaction products. TEM investigation of the acid washed product showed the formation of nano-sized material with particle sizes of about 50 nm. The electrical conductivity of acid washed product (YCO) in air was found to be about an order higher than the undoped CeO2 reported in the literature.  相似文献   

7.
Nanosized-Ta2O5 powder photocatalyst was successfully synthesized by using sol-gel method via TaCl5 butanol solution as a precursor. Ta2O5 species can be formed under 500 °C via the decomposition of the precursor. The crystalline phase of Ta2O5 powder photocatalyst can be obtained after being calcined above 600 °C for 4 h. The crystal size and particle size of Ta2O5 powder photocatalyst was about 50 nm. A good photocatalytic performance for the degradation of gaseous formaldehyde was obtained for the nanosized-Ta2O5 powder. The Ta2O5 powder formed at 700 °C for 4 h and at 650 °C for 12 h showed the best performance. The calcination temperature and time play an important role in the crystallization and photocatalytical performance of nanosized-Ta2O5 powder.  相似文献   

8.
Bi2WO6 powder photocatalyst was prepared using Bi(NO3)3 and Na2WO4 as raw materials by a simple hydrothermal method at 150 °C for 24 h, and then calcined at 300, 400, 500, 600 and 700 °C for 2 h, respectively. The as-prepared samples were characterized with UV-visible diffuse reflectance spectra, fourier transform infrared spectra (FTIR), X-ray diffraction (XRD), scanning electron microscopy (SEM) and N2 adsorption-desorption measurement. The photocatalytic activity of the samples was evaluated using the photocatalytic oxidation of formaldehyde at room temperature under visible light irradiation. It was found that post-treatment temperature obviously influenced the visible-light photocatalytic activity and physical properties of Bi2WO6 powders. At 500 °C, Bi2WO6 powder photocatalyst showed the highest visible-light photocatalytic activity due to the samples with good crystallization and high BET surface area.  相似文献   

9.
To elucidate the phase transition at 115 K in the fresnoite-type compound K2V3O8, we undertook temperature-dependent neutron powder diffraction and single-crystal X-ray diffraction (XRD). For structure refinements in the nominal space group P4bm, the most dramatic change is evidenced by the a cell edge, which initially expands on cooling, then abruptly begins to contract at 115 K. The c cell edge contracts monotonically. The atomic displacement parameters (ADPs) also deviate from their expected temperature dependence at 115 K, where the oxygen atoms in the vanadium oxide plane exhibit an increase in apparent positional disorder. Similar changes in lattice parameters and ADPs are observed from the single-crystal XRD refinements. Below 115 K, weak superlattice reflections are clearly evident in XRD patterns recorded by a CCD detector, and these extra reflections can be indexed with the wave vector ±1/3〈110〉*+1/2c*. Possible space groups for the modulated structure are P42bc and P4nc.  相似文献   

10.
Li2CO3 and LiOH·H2O are widely used as Li-precursors to prepare LiFePO4 in solid-phase reactions. However, impurities are often found in the final product unless the sintering temperature is increased to 800 °C. Here, we report that lithium fluoride (LiF) can also be used as Li-precursor for solid-phase synthesis of LiFePO4 and very pure olivine phase was obtained even with sintering at a relatively low temperature (600 °C). Consequently, the product has smaller particle size (about 500 nm), which is beneficial for Li-extraction/insertion in view of kinetics. As for cathode material for Li-ion batteries, LiFePO4 obtained from LiF shows high Li-storage capacity of 151 mAh g−1 at small current density of 10 mA g−1 (1/15 C) and maintains capacity of 54.8 mAh g−1 at 1500 mA g−1 (10 C). The solid-state reaction mechanisms using LiF and Li2CO3 precursors are compared based on XRD and TG-DSC.  相似文献   

11.
Thin crystals of La2O3, LaAlO3, La2/3TiO3, La2TiO5, and La2Ti2O7 have been irradiated in situ using 1 MeV Kr2+ ions at the Intermediate Voltage Electron Microscope-Tandem User Facility (IVEM-Tandem), Argonne National Laboratory (ANL). We observed that La2O3 remained crystalline to a fluence greater than 3.1×1016 ions cm−2 at a temperature of 50 K. The four binary oxide compounds in the two systems were observed through the crystalline-amorphous transition as a function of ion fluence and temperature. Results from the ion irradiations give critical temperatures for amorphisation (Tc) of 647 K for LaAlO3, 840 K for La2Ti2O7, 865 K for La2/3TiO3, and 1027 K for La2TiO5. The Tc values observed in this study, together with previous data for Al2O3 and TiO2, are discussed with reference to the melting points for the La2O3-Al2O3 and La2O3-TiO2 systems and the different local environments within the four crystal structures. Results suggest that there is an observable inverse correlation between Tc and melting temperature (Tm) in the two systems. More complex relationships exist between Tc and crystal structure, with the stoichiometric perovskite LaAlO3 being the most resistant to amorphisation.  相似文献   

12.
The complete Raman spectrum of arsenolite, cubic crystalline As4O6, is reported for the first time. The previously unseen Eg mode has been found at 443 cm−1. Further, there is additional support for the assignment of the 415 cm−1 mode as T2g.  相似文献   

13.
The La2CuO4 crystal nanofibers were prepared by using single-walled carbon nanotubes as templates under mild hydrothermal conditions. The steam reforming of methanol (SRM) to CO2 and H2 over such nanofiber catalysts was studied. At the low temperature of 150 °C and steam/methanol=1.3, methanol was completely (100%, 13.8 g/h g catalyst) converted to hydrogen and CO2 without the generation of CO. Within the 60 h catalyst lifespan test, methanol conversion was maintained at 98.6% (13.6 g/h g catalyst) and with 100% CO2 selectivity. In the meantime, for distinguishing the advantage of nanoscale catalyst, the La2CuO4 bulk powder was prepared and tested for the SRM reaction for comparison. Compared with the La2CuO4 nanofiber, the bulk powder La2CuO4 showed worse catalytic activity for the SRM reaction. The 100% conversion of methanol was achieved at the temperature of 400 °C, with the products being H2 and CO2 together with CO. The catalytic activity in terms of methanol conversion dropped to 88.7% (12.2 g/h g catalyst) in 60 h. The reduction temperature for nanofiber La2CuO4 was much lower than that for the La2CuO4 bulk powder. The nanofibers were of higher specific surface area (105.0 m2/g), metal copper area and copper dispersion. The in situ FTIR and EPR experiments were employed to study the catalysts and catalytic process. In the nanofiber catalyst, there were oxygen vacancies. H2-reduction resulted in the generation of trapped electrons [e] on the vacancy sites. Over the nanofiber catalyst, the intermediate H2CO/HCO was stable and was reformed to CO2 and H2 by steam rather than being decomposed directly to CO and H2. Over the bulk counterpart, apart from the direct decomposition of H2CO/HCO to CO and H2, the intermediate H2COO might go through two decomposition ways: H2COO=CO+H2O and H2COO=CO2+H2.  相似文献   

14.
Single crystals of CeAu4Si2 and CeAu2Si2 have been grown out of ternary fluxes rich in Au, and the former, also by sintering the stoichiometric composition at 750 °C. The single-crystal X-ray refinement result for CeAu4Si2 is orthorhombic, Cmmm (No. 65, Z=2), different from a tetragonal result found from an X-ray powder diffraction refinement [H. Nakashima, et al., J. Alloys Compds. 424 (2006) 7]. For CeAu2Si2, this is the first report of the stoichiometric crystalline phase, in the known tetragonal I4/mmm structure. The anisotropic field- and temperature-dependent magnetizations, as well as specific heat and resistivity data are compared. Although both compounds have related structural packing, they present unique magnetic features. CeAu2Si2 is a typical antiferromagnet with TN=8.8(1) K and CeAu4Si2 features a ferromagnetic component below Tc=3.3(1) K. Both phases have effective moments close in value to that of free Ce3+.  相似文献   

15.
ZnO/TiO2/SnO2 mixture was prepared by mixing its component solid oxides ZnO, TiO2 and SnO2 in the molar ratio of 4?1?1, followed by calcining the solid mixture at 200-1300 °C. The products and solid-state reaction process during the calcinations were characterized with powder X-ray diffraction (XRD), thermogravimetric and differential thermal analysis (TG-DTA), UV-Vis diffuse reflectance spectroscopy (UV-Vis DRS) and Brunauer-Emmett-Teller measurement of specific surface area. Neither solid-state reaction nor change of crystal phase composition took place among the ZnO, TiO2 and SnO2 powders on the calcinations up to 600 °C. However, formation of the inverse spinel Zn2TiO4 and Zn2SnO4 was detected at 700-900 and 1100-1200 °C, respectively. Further increase of the calcination temperature enabled the mixture to form a single-phase solid solution Zn2Ti0.5Sn0.5O4 with an inverse spinel structure in the space group of . The ZnO/TiO2/SnO2 mixture was photocatalytically active for the degradation of methyl orange in water; its photocatalytic mass activity was 16.4 times that of SnO2, 2.0 times that of TiO2, and 0.92 times that of ZnO after calcination at 500 °C for 2 h. But, the mass activity of the mixture decreased with increasing the calcination temperature at above 700 °C because of the formation of the photoinactive Zn2TiO4, Zn2SnO4 and Zn2Ti0.5Sn0.5O4. The sample became completely inert for the photocatalysis after prolonged calcination at 1300 °C (42 h), since all of the active component oxides were reacted to form the solid solution Zn2Ti0.5Sn0.5O4 with no photocatalytic activity.  相似文献   

16.
By means of powder X-ray diffraction, powder neutron diffraction and transmission electron microscopy (TEM), we determined the crystal structures of a metal-ordered manganite YBaMn2O6 which undergoes successive phase transitions. A high-temperature metallic phase (Tc1=520 K<T) crystallizes in a triclinic P1 with the following unit cell: Z=2, a=5.4948(15) Å, b=5.4920(14) Å, c=7.7174(4) Å, α=89.804(20)°, β=90.173(20)°, γ=91.160(4)°. The MnO6 octahedral tilting is approximately written as a0bc, leading to a significant structural anisotropy within the ab plane. The structure for Tc2<T<Tc1 is a monoclinic P2 (Z=2, a=5.5181(4) Å, b=5.5142(4) Å, c=7.6443(3) Å, β=90.267(4)°) with an abc tilting. The structural features suggest a dx2y2 orbital ordering (OO). Below Tc2=480 K, crystallographically inequivalent two octahedra show distinct volume difference, due to the Mn3+/Mn4+ charge ordering. The TEM study furthermore revealed a unique d3x2r2/d3y2r2 OO with a modified CE structure. It was found that the obtained crystal structures are strongly correlated to the unusual physical properties. In particular, the extremely high temperature at which charge degree of freedom freezes, Tc2, should be caused by the absence of the structural disorder and by heavily distorted MnO6 octahedra.  相似文献   

17.
Highly crystalline phenyl 2,5-dichlorobenzenesulfonate (PDBS, Tmelt = 86-87 °C) and pentafluorophenyl 2,5-dichlorobenzenesulfonate (FPDBS, Tmelt = 120-122 °C) were synthesized. Single-crystal X-ray molecular structure determinations show that both compounds have similar three-dimensional molecular structures; however, PDBS crystals are thin platelets and FPDBS crystals form hexagonal tube-like structures that are predominately hollow at one end. PDBS crystals exhibit offset π-stacking of the phenoxy-rings that form complete two-dimensional layers each two molecules thick. Hydrogen-bonding interactions are calculated at ∼3.2 Å between the C6-hydrogen and the sulfonyl-oxygen of a neighboring molecule. On the other hand, for FPDBS, π-stacking of the dichloro-substituted ring as well as dipole-dipole interactions of the fluorinated-phenoxy rings appears to be the predominate intermolecular interactions. Neither structure exhibits any kind of side-on interaction of the phenyl rings. PDBS and FPDBS exhibit melting point depressions of 26 and 40 °C, respectively, in the presence of supercritical CO2. Although both sulfonates exhibit high solubility in CO2, much lower pressures are needed to dissolve FPDBS compared to PDBS. For example, at 100 °C FPDBS dissolves at 4750 psia and PDBS dissolves at 11,000 psia. The solubility data reinforce the observation that fluorinating a compound can significantly lower the conditions needed to dissolve that compound in CO2.  相似文献   

18.
SiO2/TiO2 composite microspheres with microporous SiO2 core/mesoporous TiO2 shell structures were prepared by hydrolysis of titanium tetrabutylorthotitanate (TTBT) in the presence of microporous silica microspheres using hydroxypropyl cellulose (HPC) as a surface esterification agent and porous template, and then dried and calcined at different temperatures. The as-prepared products were characterized with differential thermal analysis and thermogravimetric (DTA/TG), scanning electron microscopy (SEM), X-ray diffraction (XRD), nitrogen adsorption. The results showed that composite particles were about 1.8 μm in diameter, and had a spherical morphology and a narrow size distribution. Uniform mesoporous titania coatings on the surfaces of microporous silica microspheres could be obtained by adjusting the HPC concentration to an optimal concentration of about 3.2 mmol L−1. The anatase and rutile phase in the SiO2/TiO2 composite microspheres began to form at 700 and 900 °C, respectively. At 700 °C, the specific surface area and pore volume of the SiO2/TiO2 composite microspheres were 552 and 0.652 mL g−1, respectively. However, at 900 °C, the specific surface area and pore volume significantly decreased due to the phase transformation from anatase to rutile.  相似文献   

19.
The magnetic properties and the magnetocaloric effect are presented for the perovskite-related oxide SrFe0.5Co0.5O3 prepared using electrochemical oxidation. SrFe0.5Co0.5O3 exhibits a second order paramagnetic-ferromagnetic transition close to room temperature (TC=330 K). The maximal magnetic entropy change ΔSMMax , the maximal adiabatic temperature change ΔTad and the refrigerant capacity are found to be equal to respectively 4.0 J/kgK, 1.8 K and 258 J/kg while raising the B-field change from 0 to 5 T.  相似文献   

20.
Phase transitions in MgAl2O4 were examined at 21-27 GPa and 1400-2500 °C using a multianvil apparatus. A mixture of MgO and Al2O3 corundum that are high-pressure dissociation products of MgAl2O4 spinel combines into calcium-ferrite type MgAl2O4 at 26-27 GPa and 1400-2000 °C. At temperature above 2000 °C at pressure below 25.5 GPa, a mixture of Al2O3 corundum and a new phase with Mg2Al2O5 composition is stable. The transition boundary between the two fields has a strongly negative pressure-temperature slope. Structure analysis and Rietveld refinement on the basis of the powder X-ray diffraction profile of the Mg2Al2O5 phase indicated that the phase represented a new structure type with orthorhombic symmetry (Pbam), and the lattice parameters were determined as a=9.3710(6) Å, b=12.1952(6) Å, c=2.7916(2) Å, V=319.03(3) Å3, Z=4. The structure consists of edge-sharing and corner-sharing (Mg, Al)O6 octahedra, and contains chains of edge-sharing octahedra running along the c-axis. A part of Mg atoms are accommodated in six-coordinated trigonal prism sites in tunnels surrounded by the chains of edge-sharing (Mg, Al)O6 octahedra. The structure is related with that of ludwigite (Mg, Fe2+)2(Fe3+, Al)(BO3)O2. The molar volume of the Mg2Al2O5 phase is smaller by 0.18% than sum of molar volumes of 2MgO and Al2O3 corundum. High-pressure dissociation to the mixture of corundum-type phase and the phase with ludwigite-related structure has been found only in MgAl2O4 among various A2+B3+2O4 compounds.  相似文献   

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