Synthesis and structure analysis of La0.5SR0.5TiO3 nanoparticles prepared by thermal decomposition method

La0.5Sr0.5TiO3 (LSTO) nanoparticles were synthesized by thermal decomposition method using Cl3La, CI2Sr x 6H2O and C16H28O6Ti as starting materials. The obtained precursor in a powder form was calcined at 700, 900, 1100 and 1300 degrees C for 3, 6 and 9 h in air. The structures of all samples were analyzed by XRD and some of them were taken for SEM, TEM and VSM measurements. The results from SEM showed the parallelpipe like shape of the particles with sizes distributed between 80 and 180 nm and the sizes of these particles were increased with the increasing of calcination temperature and time. The XRD's results showed the perovskite structure with the lattice type of orthorhombic at the calcination temperature of 900, 1100 and 1300 degrees C for 3, 6 and 9 h. The TiO and others unknown phase were found at low calcination temperature and they were disappeared as the calcination temperature and time were increased. The results of TEM support the orthorhombic structure of LSTO nanoparticles with crystallite size less than 200 nm as revealed by SEM and XRD. The magnetic property of all samples was measured by VSM and revealed that those prepared at 700, 900, and 1100 degrees C exhibit diamagnetic behavior, whereas one at 1300 shows ferromagnetism at room temperature. In this work, it is found that the nano-LSTO of high crystalline phase and purity can be prepared by thermal decomposition method at calcination temperature of 900 to 1300 degrees C in air for 6-9 h.     

脉冲激光沉积Ba0.5Sr0.5TiO3、Pb0.5Ba0.5TiO3和Pb0.5Sr0.5TiO3薄膜及其介电性质

采用脉冲激光沉积法,在Pt／Ti／SiO2／Si基底上分剐制备厚度为350nm的Ba0.5Sr0.5TiO3(BST)、Pb0.5Ba0.5TiO3(PBT)和Pb0.5Sr0.5TiO3(PST)薄膜并研究了它们的介电性质。XRD显示,在相同的制备条件下三者具有不同的择优取向,PST具有(110)择优取向,PBT具有(111)择优取向,而BST则是混合取向。SEM显示三者样品表面均匀致密,颗粒尺寸大约在50nm至150nm之间。PST与BST、PBT相比有更高的介电常数,在频率为10kHz时,分别为874、334和355,而损耗都较低,分别为0．0378、0．0316和0．0423,同时PST漏电流也是最小的。测量薄膜的C-V特性扣铁电性能表明室温下BST呈现的是顺电相,PST和PBT则呈铁电相。本文也测量了薄膜在不同频率下的介电温度特性,BST、PBT和PST均表现出频率弥散现象,即随着频率的降低．居里温度降低而介电常数会升高。并测得BST和PST的居里温度分剐为-75和150℃。而PBT的居里温度在250℃以上。本文研究表明：与BST相比较,PBT的介电常数与之相近,漏电流较大;而PST具有高介电常数,较小的漏电流和较大的电容-电压调谐度,在相关半导体器件中的应用将有很大的潜力。     

Preparation of La0.5Li0.5TiO3 perovskite thin films by the sol–gel method

Perovskite La_0.5Li_0.5TiO₃ (LLT) thin films, 0.2–1 μm thick, were deposited on non-alkali aluminoborosilicate glass substrates (NA substrates) and glass substrates with ITO (indium tin oxide) coatings (ITO substrates) by the sol–gel method. Alkoxide-based solutions containing titanium alkoxide, lithium alkoxide and lanthanum alkoxide and acetate-based solutions containing titanium alkoxide, lithium acetate and lanthanum acetate, were used as coating solutions. Impurity phases tended to be precipitated on heat treatment in the films derived from the acetate-based solutions. Addition of acetylacetone or partial substitution of lead for lithium in the acetate-based solutions, however, was effective in suppressing the precipitation of impurity phases. Preferred orientation of the LLT (1 1 1/2) plane was observed in the films prepared from the acetate-based solutions when NA substrates were used, whereas the employment of the alkoxide-based solutions or ITO substrates and the partial substitution of lead for lithium, reduced the preferred orientation. The electrical conductivity of the films was much lower than the values reported for the sintered materials. This revised version was published online in November 2006 with corrections to the Cover Date.     

Optical properties of Ag nanoparticles embedded Ba0.5Sr0.5TiO3 films prepared by alternating pulsed laser deposition

Nanocomposite thin films consisting of nanometer-sized Ag particles embedded in amorphous Ba0.5Sr0.5TiO3 matrix were prepared on fused silica substrates by an alternating pulsed laser deposition method. Their optical nonlinearities have been studied using the Z-scan method. The surface plasmon resonance (SPR) peak shifts to red and increases with the increasing the volume fraction of Ag in the nanocomposite films. The magnitude of the third-order nonlinear susceptibility of the nanocomposite with an Ag volume fraction of 3.3% was calculated to be approximately 2 x 10(-8) esu at the SPR wavelength.     

钛酸锶钡的自燃烧法合成、表征及电性能研究

以硝酸钡、硝酸锶、钛酸丁酯和柠檬酸为原料,采用自燃烧法合成了晶粒尺寸～20nm Ba0.5Sr0.5TiO3(BST)超细粉体。利用溶液中各种离子分布与溶液pH值的关系,研究了金属离子-柠檬酸水溶液体系中的络合pH条件,得到了自燃烧制备BST的最佳pH值范围。借助TG-DSC、IR、XRD和TEM研究了硝酸盐-柠檬酸盐干凝胶的自蔓延燃烧机理以及产物的物相结构和形貌特征。结果表明,自燃烧蔓延是在硝酸根离子和羧酸根离子之间进行的热诱导阴离子氧化还原反应,其中,硝酸根离子作氧化剂,羧酸根离子作还原剂。燃烧后得到了分散均匀,团聚少的BST纳米晶。将粉末压片在1100～1250℃烧结2h后,测试了烧结体样品的电容和介电损耗随频率变化的关系,并对变化的原因进行了详细分析。     

正交试验辅助分析溶胶-凝胶法制备Bi_(0.5)Na_(0.5)TiO_3粉体过程中的主导因素

以钛酸四丁酯、五水硝酸铋和无水乙酸钠为原料,用溶胶-凝胶法制备Bi0.5Na0.5TiO3(BNT)细粉,通过XRD和TEM表征粉体的结构和形貌。采用正交试验法,分析了反应温度、溶液pH值、加水量对最终BNT粉体粒径的影响。结果表明,各因素对粉体晶粒尺寸影响的显著性水平由大到小依次为加水量溶液pH值反应温度;反应温度为60℃、溶液pH值为4.5、加水量为7.2mL的条件下制得粉体的平均晶粒尺寸约为200～350nm。     

Synthesis of Ba0.5Sr0.5(Ti0.80Sn0.20)O3 prepared by the soft chemical method

Single-phase Ba_0.5Sr_0.5(Ti_0.80Sn_0.20)O₃ (BST:Sn) powders with perovskite structure were prepared by the soft chemical method. Infrared data indicates that the BST:Sn powder is carbonate free while Raman analysis has shown that the transversal (TO) and longitudinal (LO) optical modes tend to disappear with tin addition. The electron diffraction pattern of the BST:Sn powder showed an interplanar distance of 3.94 Å characteristic of the pseudo-cubic structure.     

Tuning the microwave dielectric properties of La(Mg0.4Sr0.1Sn0.5)O3 by introducing Ca0.8Sr0.2TiO3

The influence of sintering temperature on the microwave dielectric properties and microstructure of the (1 ? y)La(Mg_0.4Sr_0.1Sn_0.5)O₃–yCa_0.8Sr_0.2TiO₃ ceramic system were investigated with a view to their application in microwave devices. The (1 ? y)La(Mg_0.4Sr_0.1Sn_0.5)O₃–yCa_0.8Sr_0.2TiO₃ ceramic systems were prepared using the conventional solid-state method. The X-ray diffraction patterns of the (1 ? y)La(Mg_0.4Sr_0.1Sn_0.5)O₃–yCa_0.8Sr_0.2TiO₃ ceramic system shifted to higher angle as y increased. A dielectric constant of 41.2, a quality factor (Q × f) of 56,900 GHz, and a temperature coefficient of resonant frequency of ?6 ppm/ °C were obtained when the 0.4La(Mg_0.4Sr_0.1Sn_0.5)O₃–0.6Ca_0.8Sr_0.2TiO₃ ceramic system was sintered at 1,550 °C for 4 h.     

Effect of Y-doping on the transport and magnetic properties of La0.5Sr0.5CoO3 and La0.7Sr0.3CoO3

The temperature variation of magnetization, resistivity, and thermoelectric power of undoped and Y-doped La_0.7Sr_0.3CoO₃ and La_0.5Sr_0.5CoO₃ samples have been investigated. Y-doping decreases the magnetization possibly due to the spin-state transition of Co ions. The low temperature conduction in (La_1?y Y _y )_0.7Sr_0.3CoO₃ is consistent with the variable range hopping. With Y-doping, value of the Seebeck coefficient increases as Y-doping decreases bandwidth and increases distortion. Seebeck coefficient value also reflects that the orbital stability increases with Sr concentration.     

Photocatalytic reduction of NO with NH3 using Si-doped TiO2 prepared by hydrothermal method

A series of Si-doped TiO2 (Si/TiO2) photocatalysts supported on woven glass fabric were prepared by hydrothermal method for photocatalytic reduction of NO with NH3. The photocatalytic activity tests were carried out in a continuous Pyrex reactor with the flow rate of 2000mL/min under UV irradiation (luminous flux: 1.1x10(4)lm, irradiated catalyst area: 160cm2). The photocatalysts were characterized by X-ray diffraction (XRD), BET, X-ray photoelectron spectroscopy (XPS), Fourier transform infrared (FT-IR) spectrophotometer, transmission electron microscopy (TEM), photoluminescence (PL) and temperature-programmed desorption (TPD). The experiment results showed that NO conversion on Si/TiO2 at 323K could exceed 60%, which was about 50% higher than that on Degussa P25 and pure TiO2. With the doping of Si, photocatalysts with smaller crystal size, larger surface area and larger pore volume were obtained. It was also found that Ti-O-Si bands were formed on the surface of Si/TiO2 and that the surface hydroxyl concentration was greatly increased. As a result, total acidity and NH3 chemisorption amount were enhanced for Si/TiO2 leading to its photocatalytic activity improvement.     

Enhanced large field-induced strain and energy storage properties of Sr0.6La0.2Ba0.1TiO3-modified Bi0.5Na0.5TiO3 relaxor ceramics

Dielectric materials especially relaxor ferroelectrics with giant strain and super-high energy density have received substantial attentions. Bi_0.5Na_0.5TiO₃ (BNT)-based ceramics as one of the typical relaxor ferroelectric materials have been extensively explored for their distinctive performance. Here, lead-free (1?x)Na_0.5Bi_0.5TiO₃–xSr_0.6La_0.2Ba_0.1TiO₃ (BNT–SLBT) ceramics were designed and prepared by the solid-state reaction method. A large strain response of 0.470% and huge piezoelectric strain coefficient of 600 pm/V were achieved in BNT–0.15SLBT relaxor, which were attributed to the relaxor-ferroelectric phase transition under stimulated electric field. The ε_r–T curve shows that with the increase of x content, the phase transition temperature moves to room temperature, which improves the energy storage performance. A super-high recoverable energy density W_rec of 3.18 J/cm³ and η of 82.8% under 250 kV/cm can be achieved in BNT–0.25SLBT ergodic relaxor. Moreover, the charge–discharge properties characterized by a high pulse discharge energy density (0.816 J/cm³), a rapid discharge duration (3 μs) and a power density (2.86 MW/cm³) are also observed in BNT–0.25SLBT ceramic. We provide a method for enhanced BNT-based ceramics with strain and energy storage in drive device or capacitor, facilitating the exploration of ceramic in the future.

     

Characterization of (Pb,La) TiO3 thin films prepared by the sol-gel method

Pb_(1–1.5x)La_xTiO₃ thin films were synthesized by the sol-gel spin-coating technique. The films became crystallized when the spin-coated films were annealed at 600 °C and at higher temperature, and became amorphous when annealed at 550 °C. The breakdown voltage, V _B, was recorded at around 30 V for 600–650 °C annealed films and varied only slightly with the composition. The V _B value of the amorphous films was observed to be higher than that of the crystalline films. The ferroelectric properties of both the amorphous and crystalline films were found to be similar. The dielectric constant, charge storage density and optical index of refraction of the films were _r =5–20, Q _c=0.12–0.54 C cm^–2 and n=1.6–2.3, respectively. They all increased moderately with La³⁺ content in the films. One possible reason why the ferroelectric properties are not modified as the amorphous films crystallize, may be that the octahedra are equilateral, whether the films are amorphous or crystalline. Additionally, a possible cause which lowers the breakdown voltage in crystalline film, is the formation of lead vacancies due to lead loss. The electrical properties of films coated on bare silicon become significantly lowered due to interdiffusion between films and substrate. The diffusion of Si⁴⁺ ions into-the films can be prevented by coating SrTiO₃ on the silicon substrate as a buffer layer. The charge storage capacity consequently becomes substantially enhanced.     

水热法制备稀土掺杂TiO_2薄膜及光催化降解性能研究

采用水热法,以载玻片为基片制备了稀土掺杂Ti O2薄膜。以紫外光区吸光度值为指标,确定最佳制备条件为:90℃保温2h,Ti(SO4)2溶液和尿素溶液摩尔比为10∶1,稀土掺杂量为1 mL0.5 mol/L稀土盐溶液,掺杂稀土镧Ti O2薄膜有较好的光吸收性能。利用X-射线粉末衍射法(XRD)、扫描电子显微镜(SEM)及电子能谱法(EDS)对Ti O2薄膜的结构及表面特性进行表征,结果表明制备的稀土掺杂Ti O2薄膜为锐钛矿型。以紫外灯为光源,降解率为指标,罗丹明B溶液降解为模型反应,考察稀土掺杂Ti O2薄膜光催化性能,结果表明,稀土掺杂Ti O2薄膜具有较高光催化活性且明显大于纯Ti O薄膜,该薄膜对罗丹明B的光催化降解率达87%以上。     

Lao.5Sro.5MnO3薄膜的输运特性和光诱导效应

用磁控溅射方法制备了La0.5Sro 5MnO3薄膜,研究了薄膜的输运特性和光诱导效应.La0.5Sr0 5MnO3薄膜具有温度相变特征:低温为铁磁金属相,高温则为顺磁非导体相,相变温度420 K.为铁磁金属相时,光诱导效应导致薄膜的电阻增大,在360 K电阻变化相对值的最大值约为9.62%.根据双交换作用模型,激光导致顺磁非导体相小极化子的浓度增加,使电阻减小.     

微波水热法制备纳米ZnO粉体的研究

以硝酸锌和氢氧化钠为原料,通过微波水热法制备了ZnO纳米粉体。采用X射线衍射、透射电镜、激光粒度分析、比表面测试等手段对微波水热产物进行表征,并探讨了溶液体系pH值、反应温度、反应时间对微波水热反应所得ZnO粉体性能的影响。结果表明,微波水热反应体系的pH值、反应温度对所制备粉体的粒度分布有重要影响。制备ZnO纳米粉体的最佳反应条件为:溶液体系pH值为5,反应温度为130℃,反应时间为10min,在此工艺条件下制备的ZnO粉体比表面积为18.53m2/g,平均粒度约为61nm,粒径分布狭窄,结晶完整。     

水基金属有机物分解法制备Ba0.5Sr0.5TiO3薄膜的研究

制备了水基Ｂａ＾２＋、Ｓｒ＾２＋、Ｔｉ＾４＋三元有机物溶液。根据红外光 谱测定及对比实验分析了溶液配制过程中化学反应机理。采用金属有机物分解法（ＭＯＤ）制备Ｂａ０．５Ｓｒ０．５ＴｉＯ３（ＢＳＴ）薄膜。通过ＸＲＤ、ＳＥ趱 阻抗分析仪等分析测试手段,薄膜的相结构、微观形态及电性能。结果表明,所制备ＢＳＴ薄 数矿晶相结构,结晶完整晶粒小（１０－５０ｎｍ）,显微结构均匀致密,并具有良好的电性能（电容密度为     

Photocatalytic ozonation of dimethyl phthalate with TiO2 prepared by a hydrothermal method

TiO(2) was prepared by a hydrothermal method at a low temperature and used to degrade and mineralize dimethyl phthalate (DMP). TiO(2) was characterized by XRD, TEM, BET and UV-vis techniques. The characteristics of TiO(2) prepared by a hydrothermal method (h-t TiO(2)) included a good crystalline anatase phase, greater surface area, stronger absorption to UV light wavelength and lower agglomeration than TiO(2) prepared by a classic sol-gel method (s-g TiO(2)). The photocatalytic activity of h-t TiO(2) prepared under optimal hydrothermal condition (180°C for 10h) was 2.5 times higher than that of s-g TiO(2) in degrading DMP. The process of photocatalysis combined with UV irradiation and ozonation (TiO(2)/UV/O(3)) considerably improved the mineralization and degradation of DMP compared to photocatalysis combined with UV irradiation (TiO(2)/UV), ozonation combined with UV irradiation (UV/O(3)), and ozonation alone (O(3)). A kinetic study showed the mineralization in TiO(2)/UV/O(3) followed the Langmuir-Hinshelwood model.     

Synthesis of Ni-doped LaSrMnO3 nanopowders by hydrothermal method for SOFC interconnect applications

Ni-doped lanthanum strontium manganite (LSMN) nanopowders, La_0.7Sr_0.3Mn_1?xNi_xO₃ (0.05?≤?x?≤?0.3) were synthesized at 150?°C for 8?h by hydrothermal reaction as a function of Ni doping concentration. The SEM analyses suggested that the calcination treatment influenced the morphology of the nanopowders. The calcined nanopowders at 1300?°C had agglomerated spherical structure of 44–77?nm. Meanwhile, the XRD studies revealed that the nanopowders have single crystalline phase over the range x?=?0.05–0.2. In addition, the LSMN nanopowders were sintered at elevated temperatures, 1250–1350?°C to examine their electrical conductivity for solid oxide fuel cell (SOFC) interconnect applications under actual SOFC working condition. Their electrical conductivity gradually increased to 90.05?S/cm with Ni doping concentration x?=?0.2, which were sintered at 1300?°C. These results suggest La_0.7Sr_0.3Mn_0.8Ni_0.2O₃ displays a good performance as an optimal composition of the LSMN.