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1.
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   

2.
以Nb2O5,K2CO3和CuO为原料经高温固相反应合成K4Nb6-xCuxO17催化剂,并通过层间离子交换反应,胺插入反应以及硫化反应制备CdS插层K4Nb6-xCuxO17复合催化剂(K4Nb6-xCuxO17/CdS)。利用X射线衍射(XRD),X射线光电子能谱(XPS),场发射扫描电镜(SEM),X射线能谱仪(EDX),紫外-可见漫反射(UV-Vis),分子荧光光谱(PL)等技术对催化剂进行表征。考察了催化剂的可见光催化制氢活性。结果表明,Cu离子掺杂进入K4Nb6O17晶格中,CdS位于K4Nb6O17层间。CdS插层K4Nb6-xCuxO17催化剂的最大吸收光波长约为550 nm。催化剂制氢活性有明显提高,紫外光和可见光下3 h产氢量分别达到279.83 mmol.gcat-1和7.11 mmol.gcat-1。最后讨论了复合催化剂光生电荷转移机理。  相似文献   

3.
A new pyrochlore-type Na0.32Bi1.68Ti2O6.46(OH)0.44 with the cubic cell of a=10.339(5) Å was prepared by hydrothermal reaction using TiO2 (anatase) and Bi2O3 in NaOH solution. This compound was obtained when the molar ratio of NaOH/TiO2 was above 2 and the reaction temperature was above 240 °C. The TG-curve of as-prepared sample showed a mass loss of 0.8 mass% which was caused by release of OH group. This compound decomposed to a pyrochlore-type compound and a layered-type Na0.5Bi4.5Ti4O15 above 800 °C. The optical band gap of Na0.32Bi1.68Ti2O6.46(OH)0.44 was estimated to be 2.5 eV.  相似文献   

4.
The structure, conductivity and water uptake of the oxygen-deficient perovskite-type compound Ba4Ca2Ta2O11 have been investigated. Ba4Ca2Ta2O11 crystallizes in the cryolite structure (cubic, Fm3m SG) with a = 8.4508(2) Å, under dry air. The compound can be partially hydrated up to a maximum water content of approximately 0.52 mol H2O per mol Ba4Ca2Ta2O11. In moist air, the structure symmetry becomes monoclinic (C2/m) and the temperature dependence of total conductivity shows a different behavior because of changes in transport mechanism. Three regions can be observed as a function of temperature. For the low temperature range 200–400 °C, the protonic conduction is prevailing with an activation energy EA = 0.85 eV. In the intermediate temperature range (400–600 °C), O2− anionic and protonic conductions are mixed with an activation energy EA = 0.45 eV and in the third region, for temperatures above 600 °C, O2−conduction is prevailing with an activation energy EA = 0.85 eV.  相似文献   

5.
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   

6.
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   

7.
Nanosized ZnNb2O6 photocatalysts (band gaps ~4.0 eV) were successfully synthesized via a citrate complex method. Their particle sizes ranged from 50 to 150 nm. The result of Mott–Schottky measurement revealed that the flat-band potential of ZnNb2O6 was ca. −1.3 V versus Ag/AgCl at pH 6.6. The photocatalytic activities of the samples for the degradation of methyl orange were evaluated under UV-light (λ = 254 nm). It was found that the sample obtained at 850 °C showed the highest photocatalytic activity due to its opportune crystallinity and surface area. Furthermore, ·OH radicals were detected as the major oxidation agents responsible for the decomposition of methyl orange.  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.
Microcrystalline ABi2Nb2O9 (A=Sr, Ba) photocatalysts were successfully synthesized by a citrate complex method. The as-prepared samples were characterized by the X-ray diffraction technique, BET surface area analysis, UV-vis diffuse reflectance spectrum, transmission electron microscopy, X-ray photoelectron spectroscopy and inductively coupled plasma-atomic emission spectrometry. The results indicated that single-phase orthorhombic SrBi2Nb2O9 could be obtained after being calcined above 650 °C, while BaBi2Nb2O9 was tetragonal. Based on the diffuse reflectance spectra, the band gaps of the obtained samples were calculated to be around 3.34-3.54 eV. For the photocatalytic redox reaction of methyl orange under UV-light irradiation, SrBi2Nb2O9 exhibited higher photocatalytic activity than that of BaBi2Nb2O9. The effects of the crystallinities, BET surface areas and crystal structures of the samples on the photocatalytic activities were discussed in detail.  相似文献   

10.
LiFe0.5Ti1.5O4 was synthesized by solid-state reaction carried out at 900 °C in flowing argon atmosphere, followed by rapid quenching of the reaction product to room temperature. The compound has been characterized by X-ray powder diffraction (XRD) and 57Fe Mössbauer effect spectroscopy (MES). It crystallizes in the space group P4332, a = 8.4048(1) Å. Results from Rietveld structural refinement indicated 1:3 cation ordering on the octahedral sites: Li occupies the octahedral (4b) sites, Ti occupies the octahedral (12d) sites, while the tetrahedral (8c) sites have mixed (Fe/Li) occupancy. A small, about 5%, inversion of Fe on the (4b) sites has been detected. The MES data is consistent with cation distribution and oxidation state of Fe, determined from the structural data.The title compound is thermally unstable in air atmosphere. At 800 °C it transforms to a mixture of two Fe3+ containing phases – a face centred cubic spinel Li(1+y)/2Fe(5−3y)/2TiyO4 and a Li(z−1)/2Fe(7−3z)/2TizO5 – pseudobrookite. The major product of thermal treatment at 1000 °C is a ramsdellite type lithium titanium iron(III) oxide, accompanied by traces of rutile and pseudobrookite.  相似文献   

11.
采用简单沉积-沉淀法合成了Bi2WO6@Bi2MoO6-xF2x(BWO/BMO6-xF2x)异质结,借助XRD、XPS、TEM、SEM、EDS、UV-Vis-DRS、PC和EIS等测试技术对其组成、形貌、光吸收特性和光电化学性能等进行系统表征,并以模型污染物罗丹明B(RhB)的光催化降解作为探针反应来评价Bi2WO6@Bi2MoO6-xF2x异质结的光催化活性增强机制。形貌分析表明,所得Bi2MoO6微球由大量厚度为20~50 nm的纳米片组成;FE-SEM和HR-TEM分析表明,尺寸约为10 nm的Bi2WO6量子点均匀沉积在Bi2MoO6-xF2x微球表面,形成新颖的Bi2WO6@Bi2MoO6-xF2x异质结;与纯Bi2MoO6或者Bi2WO6相比,1∶1Bi2WO6@Bi2MoO6-xF2x异质结表现出更好的光催化活性和光电流性质,其对RhB光催化降解的表观速率常数分别为纯BMO和BWO的6.4和11.6倍。PC和EIS图谱分析表明,Bi2WO6量子点表面沉积显著提高Bi2MoO6-xF2x光生电子/空穴的分离效率和迁移速率;活性物种捕获实验证明了·O2-和h+是主要的活性物种。根据实验结果,探讨了F-掺杂和Bi2WO6量子点之间的协同效应对Bi2MoO6的光催化活性的影响机制。  相似文献   

12.
Mn/Fe mixed oxide solids doped with Al2O3 (0.32-1.27 wt.%) were prepared by impregnation of manganese nitrate with finely powdered ferric oxide, then treated with different amounts of aluminum nitrate. The obtained samples were calcined in air at 700-1000 °C for 6 h. The specific surface area (SBET) and the catalytic activity of pure and doped precalcined at 700-1000 °C have been measured by using N2 adsorption isotherms and CO oxidation by O2. The structure and the phase changes were characterized by DTA and XRD techniques. The obtained results revealed that Mn2O3 interacted readily with Fe2O3 to produce well-crystallized manganese ferrite (MnFe2O4) at temperatures of 800 °C and above. The degree of propagation of this reaction increased by Al2O3-doping and also by increasing the heating temperature. The treatment with 1.27 wt.% Al2O3 followed by heating at 1000 °C resulted in complete conversion of Mn/Fe oxides into the corresponding ferrite phase. The catalytic activity and SBET of pure and doped solids were found to decrease, by increasing both the calcination temperature and the amount of Al2O3 added, due to the enhanced formation of MnFe2O4 phase which is less reactive than the free oxides (Mn2O3 and Fe2O3). The activation energy of formation (ΔE) of MnFe2O4 was determined for pure and doped solids. The promotion effect of aluminum in formation of MnFe2O4 was attributed to an effective increase in the mobility of reacting cations.  相似文献   

13.
The basic mercury(I) chromate(VI), Hg6Cr2O9 (=2Hg2CrO4·Hg2O), has been obtained under hydrothermal conditions (200 °C, 5 days) in the form of orange needles as a by-product from reacting elemental mercury and K2Cr2O7. Hydrothermal treatment of microcrystalline Hg6Cr2O9 in demineralised water at 200 °C for 3 days led to crystal growth of red crystals of the basic mercury(I, II) chromate(VI), Hg6Cr2O10 (=2Hg2CrO4·2HgO). The crystal structures were solved and refined from single crystal X-ray data sets. Hg6Cr2O9: space group P212121, Z=4, a=7.3573(12), b=8.0336(13), , 3492 structure factors, 109 parameters, R[F2>2σ(F2)]=0.0371, wR(F2 all)=0.0517; Hg6Cr2O10: space group Pca21, Z=4, a=11.4745(15), b=9.4359(12), , 3249 structure factors, 114 parameters, R[F2>2σ(F2)]=0.0398, wR(F2 all)=0.0625. Both crystal structures are made up of an intricate mercury-oxygen network, subdivided into single building blocks [O-Hg-Hg-O] for the mercurous compound, and [O-Hg-Hg-O] and [O-Hg-O] for the mixed-valent compound. Hg6Cr2O9 contains three different Hg22+ dumbbells, whereas Hg6Cr2O10 contains two different Hg22+ dumbbells and two Hg2+ cations. The HgI-HgI distances are characteristic and range between 2.5031(15) and 2.5286(9) Å. All Hg22+ groups exhibit an unsymmetrical oxygen environment. The oxygen coordination of the Hg2+ cations is nearly linear with two tightly bonded O atoms at distances around 2.07 Å. For both structures, the chromate(VI) anions reside in the vacancies of the Hg-O network and deviate only slightly from the ideal tetrahedral geometry with average Cr-O distances of ca. 1.66 Å. Upon heating at temperatures above 385 °C, Hg6Cr2O9 decomposes in a four-step mechanism with Cr2O3 as the end-product at temperatures above 620 °C.  相似文献   

14.
采用简单沉积-沉淀法合成了Bi_2WO_6@Bi_2MoO_(6-x)F_(2x)(BWO/BMO_(6-x)F_(2x))异质结,借助XRD、XPS、TEM、SEM、EDS、UV-Vis-DRS、PC和EIS等测试技术对其组成、形貌、光吸收特性和光电化学性能等进行系统表征,并以模型污染物罗丹明B(Rh B)的光催化降解作为探针反应来评价Bi_2WO_6@Bi_2MoO_(6-x)F_(2x)异质结的光催化活性增强机制。形貌分析表明,所得Bi_2MoO_6微球由大量厚度为20~50 nm的纳米片组成;FE-SEM和HR-TEM分析表明,尺寸约为10 nm的Bi_2WO_6量子点均匀沉积在Bi_2MoO_(6-x)F_(2x)微球表面,形成新颖的Bi_2WO_6@Bi_2MoO_(6-x)F_(2x)异质结;与纯Bi_2MoO_6或者Bi_2WO_6相比,1∶1Bi_2WO_6@Bi_2MoO_(6-x)F_(2x)异质结表现出更好的光催化活性和光电流性质,其对RhB光催化降解的表观速率常数分别为纯BMO和BWO的6.4和11.6倍。PC和EIS图谱分析表明,Bi_2WO_6量子点表面沉积显著提高Bi_2MoO_(6-x)F_(2x)光生电子/空穴的分离效率和迁移速率;活性物种捕获实验证明了·O_2~-和h~+是主要的活性物种。根据实验结果,探讨了F-掺杂和Bi_2WO_6量子点之间的协同效应对Bi_2MoO_6的光催化活性的影响机制。  相似文献   

15.
Li4Ti5O12 nanoparticles were precipitated from ethylene glycol solution of titanium tetra isopropoxide (Ti(O-iPr)4) and Li2O2 by refluxing at 197 °C for 12 h. The obtained particles were filtered and dried at 100 °C for 12 h, and the dried powder samples were heated at 320, 500 and 800 °C for 3 h. The X-ray diffraction patterns of the obtained samples exhibited a good fit with the spinel phase. The field emission-SEM images of the dried powder sample and the samples heated at 320, 500 and 800 °C for 3 h showed a uniform spherical morphology with a particle size of 5, 8, 10 and 400 nm, respectively. According to the results of electrochemical testing, the dried powder sample and the samples heated at 320, 500, and 800 °C for 3 h showed initial capacities of 200, 310, 320, and 260 mA h/g, respectively, at a current density of 0.05 mA/cm2. Nanosized (6–8 nm) particles with good crystallinity were obtained by controlling the synthesis conditions. The sample heated at 500 °C for 3 h exhibited a high capacity and an excellent rate capability over 60 cycles.  相似文献   

16.
The compound previously reported as Ba2Ti2B2O9 has been reformulated as Ba3Ti3B2O12, or Ba3Ti3O6(BO3)2, a new barium titanium oxoborate. Small single crystals have been recovered from a melt with a composition of BaTiO3:BaTiB2O6 (molar ratio) cooled between 1100°C and 850°C. The crystal structure has been determined by X-ray diffraction: hexagonal system, non-centrosymmetric space group, a=8.7377(11) Å, c=3.9147(8) Å, Z=1, wR(F2)=0.039 for 504 unique reflections. Ba3Ti3O6(BO3)2 is isostructural with K3Ta3O6(BO3)2. Preliminary measurements of nonlinear optical properties on microcrystalline samples show that the second harmonic generation efficiency of Ba3Ti3O6(BO3)2 is equal to 95% of that of LiNbO3.  相似文献   

17.
新铌酸盐化合物K6Zr2Nb14O42的合成   总被引:1,自引:1,他引:0  
一些铌酸盐晶体具有优良的非线性光学性质,它们在激光倍频、电光调制、参量振荡、实时全息存贮等领域均具有潜在的广泛的应用前景,因此新铌酸盐晶体的人工合成、结构及性能研究工作受到了重视[1-3],吴伯麟等曾报道了在K2O-Cr2O3-Nb2O5体系中存在一...  相似文献   

18.
对沉淀法合成的p区金属氧化物Ga2O3和Sb2O3紫外光光催化降解盐酸四环素的性能进行了研究,讨论了制备条件对光催化性能的影响。最佳制备条件下得到的Ga2O3-900和Sb2O3-500样品光催化性能存在巨大差异,通过X射线粉末衍射、傅里叶红外光谱、N2吸附-脱附测试、荧光光谱、拉曼光谱、电化学分析及活性物种捕获实验等对样品进行分析,研究二者光催化降解盐酸四环素的机理,揭示影响光催化性能差异的本质因素。结果表明,Ga2O3和Sb2O3光催化性能差异主要归结于二者不同的电子和晶体结构、表面所含羟基数量及光催化降解机理。  相似文献   

19.
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   

20.
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   

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