煅烧温度对La_(0.6)Sr_(0.4)MnO_3晶体结构及电磁性能的影响

采用传统固相反应法在不同烧结温度下制备了La_(0.6)Sr_(0.4)MnO_3样品,通过X射线衍射仪(XRD)和扫描电镜显微镜(SEM)对样品进行了物相结构和微观组织分析,比较了不同烧结温度下样品的烧结性、介电性和铁磁性能。研究结果表明,当烧结温度从1100℃增加到1200℃时,La_(0.6)Sr_(0.4)MnO_3样品的介电损耗呈降低趋势,介电常数数值呈增加趋势,并在测量频率范围内显示负值。随着烧结温度的增加,La_(0.6)Sr_(0.4)MnO_3样品的铁磁性呈现先上升后下降的趋势。当烧结温度为1150℃时,其饱和磁化强度达到最大,为37.80A·m~2·kg~(-1)。说明可以通过改变煅烧温度来有效调节晶粒尺寸,从而改进La_(0.6)Sr_(0.4)MnO_3样品的介电性能和铁磁性能。     

Preparation and characterization of polycrystalline La2Zr2O7 ultrafine fibres via electrospinning

Polyvinyl Pyrrolidone (PVP)/(Lanthanum nitrate and zirconium oxychloride) microfibres were fabricated by electrospinning. SEM micrographs indicated that the surface of the prepared composite microfibres was smooth, and the diameter of the microfibres was in the range of 2 microm-5 microm. X-ray diffractormetry (XRD) analysis revealed that the composite microfibres were amorphous in structure. La2Zr2O7 porous hollow ultrafine fibres (PHUF) were fabricated by calcination of the PVP/[La(NO3)3 + ZrOCl2] composite microfibres. The diameters of La2Zr2O7 PHUF were smaller than those of the PVP/[La(NO3)3 + ZrOCl2] composite microfibres. The surface of the ultrafine fibres became coarse with the increase of calcination temperatures. La2Zr2O7 PHUF formed by nanoparticles were acquired when calcination temperature was above 800 degrees C. Scanning electron microscope (SEM) analysis indicated that the diameter of the synthesized La2Zr2O7 PHUF was in the range of 500 nm-800 nm. XRD analysis revealed that the crystal structure of La2Zr2O7PHUF was found to be of the fluorite type when calcination temperature was 800 degrees C-900 degrees C, and of the pyrochlore type at 1000 degrees C. The latter is cubic in structure with space group Fd3m. The conductance of La2Zr2O7 PHUF is high to 5.19 S/cm2 and has no effect of frequency. Possible formation mechanism for La2Zr2O7 PHUF was preliminarily proposed.     

Decomposition of MEK and toluene over nanolayered TiO2 photocatalyts prepared from metallic titanium chip

The Nanolayered TiO2 photocatalysts were prepared by thermal treatment of metallic titanium chips. Photocatalytic activity for methyl ethyl ketone (MEK) and toluene was investigated using a closed circulating system. The photocatalysts were characterized by SEM and XRD. Surface of the Ti chips changed to be rough with increase of treatment temperature, and severe oxidation over 900 degrees C resulted in TiO2 powder. Uniform TiO2 nanolayer was formed as a rutile type on the metallic chip. Photocatalytic decomposition of MEK over the TiO2 photocatalysts occurred efficiently by UV-C irradiation. The maximum activity for MEK was obtained over Ti Chip treated at 700 degrees C. It was known that the prepared photocatalyts could be applied to remove various VOCs.     

甘氨酸燃烧法合成Sr2CeO4及其发光性质研究

为制备具有优良性能的蓝色荧光粉,首次采用甘氨酸-硝酸盐燃烧法合成了Sr2CeO4,利用热重-差热分析仪、X射线粉末衍射仪、扫描电镜等技术对其形成过程、物相结构、形貌粒度、发光性质进行了研究.结果表明:燃烧后的前驱物经800℃焙烧已有目标产物Sr2CeO4生成,1100℃时可得到较纯正交晶系的Sr2CeO4相.颗粒的形貌为不规则球形,平均粒径在80 nm左右.发光性质研究表明:Sr2CeO4荧光粉的激发光谱是宽带双峰结构,此宽带属于Ce4+的电荷迁移带,两个峰分别位于305 nm和348 nm,后者为主峰.用348 nm紫外光激发样品,发出明亮的蓝光,其发射光谱也是一个宽带,最大峰位于470 nm,此峰属于Ce4+的f→t1g跃迁.发光强度在800~1100℃随温度升高而增强.     

Nanostructured La(Sr)CrO3 through gel combustion: sintering and electrical behavior

Nanostructured La(Sr)CrO3 (LSC) powders was prepared through glycine-nitrate gel combustion process. It was shown for the first time that the use of relatively inexpensive CrO3 as a starting material for chromium has a potential for the bulk preparation of sinter-active LSC powder. As-prepared powder when calcined at 700 degrees C resulted in LSC along with a small amount of SrCrO4 as a secondary phase. The powder was found to be composed of soft agglomerates with a particle size of approximately 70-270 nm. The average agglomerate size was found to be 0.95 microm. The cold pressing and sintering of the LSC powder at 1450 degrees C resulted in mono-phasic La0.8Sr0.2CrO3 with 94% of its theoretical density. This is the lowest sintering temperature ever reported for La0.8Sr0.2CrO3. The conductivity of the sintered La0.8Sr0.2CrO3 at 1000 degrees C was found to be approximately 18 S cm(-1).     

Low temperature synthesis and visible light driven photocatalytic activity of highly crystalline mesoporous TiO2 particles

Mesoporous TiO2 powder materials with a high crystallinity have been prepared by evaporation induced self assembly (EISA) process using titanium tetraisopropoxide (TTIP) and pluronic P123 surfactant (EO20PO70EO20) as titanium source and structure-directing reagent, respectively. The prepared materials were characterized by low and wide-angle X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), optical absorption, and N2 adsorption-desorption experiments. The crystallinity of the materials was controlled by varying the calcination temperature. The resulting TiO2 materials showed highly crystalline structure with uniform particle size which increases from 11.8 to 23.8 nm with increasing the calcination temperature from 400 to 600 degrees C, respectively, whereas the specific surface area decreases from 125 to 40 m2/g. TEM and XRD results revealed that the calcination temperature of 600 degrees C is the best condition to obtain highly crystalline mesoporous TiO2. The photocatalytic activity of the TiO2 mesoporous materials with different crystallinity and textural parameters has been studied in the decomposition of methylene blue (MB) dye molecules under visible light irradiation. Among the mesoporous TiO2 materials studied, the material with the highest crystallinity, prepared at 600 degrees C, showed the best photocatalytic performance in the decomposition of MB under visible light in a short time.     

Structural study of Sr0.3Ba0.7Nb2O6 and La0.030Sr0.255Ba0.700Nb2O6 ceramic systems

Sr_0.3Ba_0.7Nb₂O₆ (SBN) and La_0.030Sr_0.255Ba_0.700Nb₂O₆ (LSBN) ceramic compounds have been prepared using the traditional ceramic method at two different calcination temperatures (900 and 1000 °C) and later sintered both at 1400 °C. A study of the effects of the calcination temperatures and La substitution on the morphological, compositional, and structural properties of SBN and LSBN is presented using scanning electronic microscopy (SEM), energy dispersive spectroscopy (EDS), and X-ray diffraction (XRD) analysis. From Rietveld refinement processes, the XRD patterns were interpreted to evaluate such effects in the structural parameters and the site occupation factors of the heavy metals and oxygen atoms. The effect of the incorporation of La resulted in a 0.25% cell contraction and turned out to be higher than the 0.08% dilation effect produced by the increase of calcination temperature. The La ion with similar effective ionic radius and higher electronegativity is incorporated into the structure occupying the A₁ site just like the Sr ions in the SBN compound. Differences in the site occupation factors between the SBN and LSBN samples lead to substantial changes in the physical properties such as temperature of relative dielectric constant maximum, relative dielectric constant, and dielectric loss, correlated with the distortion and the relative orientation of the oxygen octahedra.     

MOD法在种子层/Ni-W上制备La0.4Sr0.6TiO3薄膜的研究

采用金属有机沉积法(MOD)在双轴织构的Ni-5%(原子分数)W基带上制备了SrTiO3种子层,然后再在种子层上沉积La0.4Sr0.6TiO3薄膜.SEM图像显示种子层颗粒分布均匀,大小基本一致.通过XRD和SEM研究了不同热处理温度对La0.4Sr0.6TiO3薄膜取向和微观形貌的影响,结果显示,在Ar-4%H2气...     

One-dimensional SrFe12O19/Ni(0.5)Zn(0.5)Fe2O4 composite ferrite nanofibers and enhancement magnetic property

SrFe12O19/Ni(0.5)Zn(0.5)Fe2O4 composite ferrite nanofibers of diameters about 100 nm with mass ratio 1:1 have been prepared by the electrospinning and calcination process. The SrFe12O19/Ni(0.5)Zn(0.5)Fe2O4 composite ferrites are formed after calcined at 700 degrees C for 2 hours. The composite ferrite nanofibers are fabricated from nanosized Ni(0.5)Zn(0.5)Fe2O4 and SrFe12O19 ferrite grains with a uniform phase distribution. The ferrite grain size increases from about 11 to 36 nm for Ni(0.5)Zn(0.5)Fe12O4 and 24 to 56 nm for SrFe12O19 with the calcination temperature increasing from 700 to 1100 degrees C. With the ferrite grain size increasing, the coercivity (Hc) and remanence (Mr) for the SrFe12O19/Ni(0.5)Zn(0.5)Fe2O4 composite ferrite nanofibers initially increase, reaching a maximum value of 118.4 kA/m and 31.5 Am2/kg at the grain size about 40 nm (SrFe12O19) and 24 nm (Ni(0.5)Zn(0.5)Fe2O4) respectively, and then show a reduction tendency with a further increase of the ferrite grain size. The specific saturation magnetization (Msh) of 63.2 Am2/kg for the SrFe12O19/Ni(0.5)Zn(0.5)Fe2O4 composite ferrite nanofibers obtained at 900 degrees C for 2 hours locates between that for the single SrFe12O19 ferrite (48.5 Am2/kg) and the single Ni(0.5)Zn(0.5)Fe2O4 ferrite (69.3 Am2/kg). In particular, the Mr value 31.5 Am2/kg for the SrFe12O19/Ni(0.5)Zn(0.5)Fe2O4 composite ferrite nanofibers is much higher than that for the individual SrFe12O19 (25.9 Am2/kg) and Ni(0.5)Zn(0.5)Fe2O4 ferrite (11.2 Am2/kg). These enhanced magnetic properties for the composite ferrite nanofibers can be attributed to the exchange-coupling interaction in the composite.     

Mechanical properties and oxidation behaviors of carbon/carbon composites with C–TaC–C multi-interlayer

To improve the mechanical properties and oxidation-resistance properties, a C–TaC–C multi-interlayer structure was introduced in carbon/carbon (C/C) composites by chemical vapor infiltration. Compared with conventional C/C composites, a higher fracture toughness and strength have been achieved by using the C–TaC–C multi-interlayer. In addition, the composites also exhibit a higher preliminary oxidation temperature and a lower mass loss at high temperatures. The oxidation rate of the composites increases with temperature increasing in the range of 700–1300 °C, reaching a maximum value at 1300 °C, then decreases in 1300–1400 °C. A hexagonal structure of Ta₂O₅ phase is obtained when being oxidized at 700–800 °C, and it transforms to an orthorhombic phase at temperatures above 900 °C. The structures of C–TaC–C multi-interlayer are intact without cracks or porosities after being oxidized at 700–800 °C. In 900–1300 °C, the composites are oxidized uniformly with the formation of pores. At temperatures above 1300 °C, there are oxidation and non-oxidation regions with the oxidation process being controlled by diffusion.     

Photocatalytic oxidation of nitric oxide with immobilized titanium dioxide films synthesized by hydrothermal method

Gas-phase photocatalytic oxidation (PCO) of nitric oxide (NO) with immobilized TiO2 films was studied in this paper. The immobilized TiO2 films were synthesized by hydrothermal method. The characterization for the physicochemical properties of catalysts prepared under different hydrothermal conditions were carried out by X-ray diffraction analysis (XRD), transmission electron microscopy (TEM), high resolution-transmission electron microscopy (HR-TEM), Brunauer-Emmett-Teller measurements (BET) and scanning electron micrograph (SEM). It was found that the PCO efficiency of the catalyst was mainly depended on the hydrothermal conditions. The optimal values of hydrothermal temperature and hydrothermal time were 200 degrees C and 24 h, respectively. Furthermore, it was also known that the photocatalytic efficiency would decrease remarkably when the calcination temperature was over than 450 degrees C. Under the optimal conditions (hydrothermal condition: 200 degrees C for 24 h; calcination temperature: 450 degrees C), the photocatalytic efficiency of catalyst could reach 60% higher than that of Degussa P25.     

Synthesis, characterization and photocatalytic H2 generation over ternary indium titanate nanoparticles

A low temperature surfactant-free solution-phase method has been successfully developed for the synthesis of ternary In2TiO5, nanoparticles using a solvothermal route. The mechanistic aspects of synthesis of In2TiO5 nanoparticles from precursors, In(acac)3 and Ti(IV) isopropoxide in benzyl alcohol at 220 degrees C under solvothermal conditions, were investigated by GC-MS and 13C{1H} NMR analysis. The N2-BET surface area of the 5-8 nm sized In2TiO5 nanoparticles was found to be 60 m2 g(-1), which decreased with increase in calcination temperature; 38 m2 g(-1) at 800 degrees C; 5 m2 g(-1) at 1200 degrees C. The High resolution transmission electron microscopy (HR-TEM) shows well-developed lattice fringes of the crystalline nanoparticles, and selected area electron diffraction (SAED), pattern was indexed to be orthorhombic In2TiO5. The nanoparticles show better photocatalytic hydrogen generation from water-methanol mixtures over bulk In2TiO5, anatase TiO2 nanoparticles prepared by identical route and commercial TiO2 photocatalyst (Degussa, P25) under UV-visible irradiation (16% UV + 84% visible). Photocatalytic properties as a function of crystallinity and surface area of indium titanate nanoparticles have also been investigated. The high photoactivity obtained is correlated with the electronic and crystal structure of In2TiO5.     

Direct formation of reusable TiO2/CoFe2O4 heterogeneous photocatalytic fibers via two-spinneret electrospinning

A reusable photocatalytic TiO2/CoFe2O4 composite nanofiber was directly formed by using a vertical two-spinneret electrospinning process and sol-gel method, followed by heat treatment at 550 degrees C for 2 h. The high photocatalytic activity of the composite nanofibers depends on the good morphology of the fibers and the appropriate calcination temperature. The crystal structure and magnetic properties of the fibers were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersion spectroscopy (EDS), transmission electron microscope (TEM) and vibrating sample magnetometer (VSM). The photocatalytic activity of the TiO2/CoFe2O4 fibers was investigated through ultraviolet-visible absorbance following the photo-oxidative decomposition of phenol. Meanwhile, the presence of CoFe2O4 not only broadens the response region of visible light, but also enhances the absorbance of UV light. Furthermore, these fibers displayed photocatalytic activity associated with magnetic activity of CoFe2O4 ferrites, allowing easy separated of the photocatalysts after the photo-oxidative process and effectively avoided the secondary pollution of the treated water.     

煅烧温度对卤水-纯碱蒸氨汽法制备高纯氧化镁的影响

研究以卤水和纯碱工业蒸汽氨为原料制备高纯氧化镁的方法,实现纯碱工业蒸氨汽的高效循环利用。将较优实验条件下得到的斜方晶系的4MgCO_3·Mg(OH)2_·4H_2O单晶体作为前驱体,分别在600、700、800、900℃条件下进行煅烧,对在不同锻烧温度下前驱体的形貌及组成进行表征。结果表明,随着煅烧温度的升高,晶体的择优生长方向未发生变化,但结晶度提高,产品粒径增大,微观形貌发生变化;当煅烧温度超过700℃后,锻烧温度对产品纯度基本不产生影响。     

Sintering and electromagnetic properties of BaFe12O19 ferrite prepared by co-precipitation method

BaFe₁₂O₁₉ (BaM) was synthesized through the co-precipitation route. Pure phase BaM was formed after calcination of precipitated powder at 900 °C. BaM was sintered at three different temperatures; 1100, 1200, and 1300 °C to study the sintering kinetics by varying the sintering time from 1 to 4 h. Apparent porosity decreased, and bulk density increased with increasing sintering temperature and period. A bulk density of about 4.6 g/cm³ was achieved after sintering at 1300 °C/4 h. The rate-controlling mechanism of BaM densification was the diffusion of oxygen, and the activation energy for the sintering process was 274 kJ/mol. The grain size of BaM increased with rising sintering temperatures. Permittivity increased from about 11 to 17 and the permeability increased from about 10 to 16 with the increase in sintering temperature from 1100 to 1300 °C. Saturation magnetization was also enhanced to about 69 emu/g after sintering at 1300 °C/4 h. Therefore, BaM ferrite synthesized through the co-precipitation route can be effectively used for high-frequency applications after sintering at 1300 °C.

     

钙钛矿型La0.9Sr0.1NiO3催化剂的合成条件及其可见光催化活性的研究

采用溶胶-凝胶法制备了钙钛矿型La0.9Sr0.1NiO3复合氧化物光催化剂,通过TG-DTA、XRD、可见光催化性能等对合成产物的热分解过程、物相结构和可见光催化活性进行了研究;采用单因素实验探究了合成工艺条件(柠檬酸用量、pH值、煅烧温度、煅烧时间)对合成产物的物相结构和可见光催化性能的影响。结果表明,在柠檬酸用量与金属离子的总量比为1∶1,pH=1.5,400℃预处理4h,700℃煅烧4h时可制备出单一相的六方晶系的La0.9-Sr0.1NiO3晶体;在500 W氙灯的照射下,当La0.9Sr0.1NiO3催化剂用量为1.20g/500mL时,在180min内对13.2mg/L的甲基橙溶液的脱色率达到62.1%。     

Influence of structure parameters and crystalline phase on the photocatalytic activity of TiO2 nanotube arrays

Titanium oxide nanotube arrays (TiO2-NTAs) with different diameters and lengths are prepared by anodization of titanium foils in a water/ethylene glycol solution (5:95 V/V) containing 0.3 wt% NH4F. The effects of the diameters, lengths and crystalline phases of the NTAs on the photocatalytic (PC) activity are systematically evaluated. Larger pore diameter results in higher PC activity. The PC activity increases initially and then decreases with lengths for TiO2-NTAs and the optimal length that yields the highest PC activity is observed to be 6.2 microm. The crystalline phase and corresponding PC activity depend on the calcination temperature and their relationship is also investigated. The amorphous-to-anatase and anatase-to-rutile phase transitions initially occur at 300 and 500 degrees C, respectively. The PC activity of TiO2-NTAs initially increases with calcination temperature from 250 to 500 degrees C and then decreases at higher calcination temperature. The enhanced PC activity observed from the samples annealed at 250-450 degrees C is attributed to the better anatase crystalline structure at higher calcination temperature. The highest PC activity with regard to photodecomposition of methyl orange is observed from TiO2-NTAs calcined at 500 degrees C, which coincides with the anatse-to-rutile phase transformation. The synergistic effect of the anatase TiO2-NTAs and rutile barrier layers facilitate interfacial electron transfer consequently enhancing the PC activity. Further elevation of the calcination temperatures to 550 and 600 degrees C exhibits diminished PC activity because the NTs become shorter due to conversion of the bottom of anatase NTs into rutile film.     

Synthesis and properties of LaNi<Subscript>1−<Emphasis Type="Italic">x</Emphasis></Subscript>Fe<Subscript><Emphasis Type="Italic">x</Emphasis></Subscript>O<Subscript>3−δ</Subscript> as cathode materials in SOFC

The synthesis of LaNi_{1− x} Fe _x O_3−δ (LNF) perovskites with x = 0.0–1.0, for use as cathode materials for an IT-SOFC, was investigated using four combustion methods, Water Citrate (WC), Modified Water Citrate (MWC), Nitric Citrate (NC), and Modified Nitric Citrate (MNC). The structures and homogeneities of the synthesized powders were examined using an XRD, and the particle sizes were examined using an SEM and a particle size analyzer. All four combustion methods gave the single phase perovskites with the same structure. The main difference was shown in a particle size that the smallest to the largest sizes were obtained from MNC, MWC, NC, and WC, respectively. In this LNF series, as x is 0–0.5, the crystal structure is cubic and rhombohedral at the calcination temperature of 700 and 900 °C, respectively. Further investigation indicated that the cubic structure changed to rhombohedral structure at 900 °C, and was stable up to 1200 °C. As x is 0.6–1.0, the crystal structure is in orthorhombic phase when calcined between 700 and 1000 °C. This orthorhombic phase decomposed above 1100 °C. From the XRD and SEM–EDX results, LaNi_0.6Fe_0.4O_3−δ (LNF64) has a good chemical compatibility with 8YSZ from room temperature up to 900 °C. In addition, its thermal expansion coefficient is 13.2 × 10⁻⁶ K⁻¹ close to that of 8 mol% Y₂O₃ (8YSZ). Therefore, LNF64 also has a good physical compatibility with 8YSZ.     

Effect of starting particle size on hot-pressing of magnesium oxide powder prepared by vapour-phase oxidation process

Effect of starting particle size on hot-pressing of magnesium oxide (MgO) powder was examined using seven kinds of MgO powders prepared by a vapour-phase oxidation process; the average primary particle sizes were 11, 25, 32, 44, 57, 107 and 261 nm. These compressed powders (compacts) were hot-pressed at a temperature between 900 and 1300°C. The densifications of these compacts during the hot-pressing proceeded via (i) the sintering of primary particles within secondary particles and the rearrangement of secondary particles/grains (900°C), (ii) the gradual grain growth controlled by the pore migration (900∼1100°C) and (iii) the rapid grain growth due to the active mass transfer (1300°C); the grain sizes of MgO compacts hot-pressed at and below 1100°C were <1 μm, while those at 1300°C attained 20∼30 μm. The transluscent compact with the relative density of 99.7% could be obtained when the compressed powder with the average primary particle size of 44 nm was hot-pressed at a temperature as low as 1100°C for 1 h. This revised version was published online in November 2006 with corrections to the Cover Date.     

Synthesis of Co2Z Ba-ferrites

Synthesis of Co₂Z (Ba₃Co₂Fe₂₄O₄₁) Ba-ferrites were studied in terms of process conditions. Co₂Z phase was synthesized by one-step calcination at 1350 °C. Single Co₂Z phase was obtained through calcining powders first at 900∼1100 °C and then postcalcination at 1350 °C, and other extra phases disappeared completely. Permeabilities of the Co₂Z ferrites synthesized by the two-step calcination at 900 and 1350 °C ranged between 3.5∼4.5, whereas the specimens including the intermediate products Co₂Y and M phases formed by the one-step calcination at 1300 °C showed smaller permeabilities about 2 to 2.5.