Synthesis of lanthanum–strontium manganites by oxalate-precursor co-precipitation methods in solution and in reverse micellar microemulsion

Nanostructured lanthanum–strontium manganites were synthesized using two different co-precipitation approaches, one in bulk solution, and the other in reverse micelles of CTAB/1-hexanol/water microemulsion. In both cases, precursor cations were precipitated by using oxalic acid. The properties of the materials synthesized by using these two methods were compared in order to reveal potential advantages of the microemulsion-assisted approach. The influence of the annealing conditions on the properties of synthesized manganites was investigated by using X-ray diffraction, transmission electron microscopy, differential thermal analysis, thermogravimetric analysis and magnetic measurements.     

河口水体中痕量稀土元素的共沉淀预富集-电感耦合等离子体质谱法测定研究

建立了氢氧化铟共沉淀预富集 -电感耦合等离子体质谱法测定河口水体中痕量稀土元素的方法。实验结果表明 ,在80mg·L -1的In3 +和pH9.5的实验条件下 ,在1.0L水样中添加5.0～200.0ng的混合稀土标准溶液 ,均能定量回收 ,回收率在82.2 %～106.9 %之间。方法的分析流程空白为0.04(Tb)～10.17(La)ng·L -1,检出限在0.17(Yb)～1.46(La)ng·L-1之间 ,精密度 (RSD ,n=3)小于11.7 % ,可满足河口淡水和海水样品中的痕量稀土元素定量分析的要求     

Preparation of Ce-Zr-O solid solution

A single phase solid solution of Ce-Zr-O can be made by using NH₄HCO₃ solution as precipitating agent. The influence of preparation conditions, such as pH, Zr⁴⁺/(CO₃ ^2-+HCO₃ ^-) and Ce³⁺/Zr⁴⁺ ratio on the formation of the solid solution were investigated. The results show that a single phase Ce-Zr-O solid solution can be formed only under a narrow window of preparation conditions, indicating that some compounds are formed in the precipitating process. The compound may contain Ce³⁺, Zr⁴⁺, CO₃ ^2-, HCO^3-, and OH^-. The solid solution so prepared can be described as Ce_0.37Zr_0.63O₂. This revised version was published online in August 2006 with corrections to the Cover Date.     

The electrochemical evaluation of antipsychotic drug (promethazine) in biological and environmental samples through samarium cobalt oxide nanoparticles

In this work, we developed a perovskite structured samarium cobalt oxide nanoparticles (SmCoO₃ NPs) with the aid of the co-precipitation method. The rare earth metal (Sm) and cobalt oxide combined to form a perovskite lattice structure. One-pot route synthesized SmCoO₃ NPs were scrutinized successfully through various physicochemical techniques. Concerning its effective thermal stability and electrical properties, the synthesized SmCoO₃ NPs have been effectively implemented in the electrochemical evaluation of promethazine hydrochloride (PHY) using cyclic voltammetry. The electrochemical detection of PHY was performed through SmCoO₃ NPs-modified glassy carbon electrode (GCE) and unmodified GCE. The electron transfer kinetics, effect of scan rate, the influence of pH, electroactive surface area, selectivity, and sensitivity have been studied. The electron charge transfer rate (R_ct) and electrolyte resistance (R_s) were calculated to be 105.59 (Ω) and 150 (Ω) in the ferricyanide probe, indicating great facilitation of the electron transfer between PHY and SmCoO₃ NPs deposited on the electrode surface. Further, the optimized SmCoO₃-modified GCE exemplifies excellent selectivity, storage stability, reproducibility, repeatability, detection limit (5 nM), sensitivity (0.594 μA μM^?1 cm^?2), and wide consecutive linear ranges, respectively. Besides, the proposed method has been effectively employed for the detection of PHY in the various real samples which reveals good recoveries of 95.40–99.17%.     

Near-infrared quantum cutting in Yb3+ ion doped strontium vanadate

The materials Sr_3−x(VO₄)_2:xYb were successfully synthesized by co-precipitation method varying the concentration of Yb³⁺ ions from 0 to 0.06 mol. It was characterize by powder X-ray powder diffraction (XRD) and surface morphology was studied by scanning electronic microscope (SEM). The photoluminescence (PL) properties were studied by spectrophotometers in near infra red (NIR) and ultra violet visible (UV–VIS) region. The Yb³⁺ ion doped tristrontium vanadate (Sr₃(VO₄)₂) phosphors that can convert a photon of UV region (349 nm) into photons of NIR region (978, 996 and 1026 nm). Hence this phosphor could be used as a quantum cutting (QC) luminescent convertor in front of crystalline silicon solar cell (c-Si) panels to reduce thermalization loss due to spectral mismatch of the solar cells. The theoretical value of quantum efficiency (QE) was calculated from steady time decay measurement and the maximum efficiency approached up to 144.43%. The Sr_(3−x) (VO₄)_2:xYb can be potentiality used for betterment of photovoltaic (PV) technology.     

Role of preparation parameters of Cu–Zn mixed oxide catalyst in solvent free glycerol carbonylation with urea

Solvent-free carbonylation of glycerol with urea to glycerol carbonate (GC) was achieved over heterogeneous Cu–Zn mixed oxide catalyst. Cu–Zn catalysts with different ratios of Cu:Zn were prepared using co-precipitation (CP) and oxalate gel (OG) methods. As compared to CuO–ZnO(2:1) catalyst prepared by oxalate gel (OG) method, much higher conversion of glycerol and highest selectivity towards glycerol carbonate (GC) was achieved with CuO–ZnO_CP(2:1) catalyst. Physicochemical properties of prepared catalysts were investigated by using XRD, FT-IR, BET, TPD of CO₂ and NH₃ and TEM techniques. The effect of stoichiometric ratio of Cu/Zn, calcination temperature of CuO–ZnO catalysts and effect of reaction parameters such as molar ratio of substrates, time and temperature on glycerol conversion to GC were critically studied. Cu/Zn of 2:1 ratio, glycerol–urea 1:1 molar ratio, 145 ​°C reaction temperatures were found to be optimized reaction conditions to achieve highest glycerol conversion of 86% and complete selectivity towards GC. The continuous expel of NH₃ from reaction the mixture avoided formation of ammonia complex with CuO–ZnO catalyst. As a result of this, CuO–ZnO catalyst could be recycled up to three times without losing its initial activity.     

新型复合共沉淀法制备高能量/高功率型锂离子二次电池用5V正极材料LiNi_(0.5)Mn_(1.5)O_4及其电化学性能

在传统的固相法的基础上开发了新型复合共沉淀法制备LiNi0.5Mn1.5O4材料.新型复合共沉淀法采用(NH4)2CO3和(NH4)2C2O4共同作为沉淀剂,通过控制共沉淀反应条件,得到了具有均匀球形形貌的沉淀物颗粒.再通过与饱和氢氧化锂溶液的水热反应及高温反应,最终制备出具有球形次级形貌和纯相尖晶石结构的LiNi0.5Mn1.5O4材料.电化学测试表明,制备的LiNi0.5Mn1.5O4具有优异的电化学性能,其初始容量达到了141.4mAh·g-1.在0.3C、1C和3C倍率下经过200次循环后的容量分别为136.0 mAh·g-1(96.3%)、128.6 mAh·g-1(94.4%)和113.9 mAh·g-1(91.1%).通过高温反应及特殊的冷却处理,LiNi0.5Mn1.5O4在4.0 V低压区平台的容量损失得到了有效抑制.更重要的是,通过控制合成过程中的关键步骤,可实现半定量化控制材料结构中的原子有序排布程度,进而得到具有高能量密度和高功率密度的两种LiNi0.5Mn1.5O4材料,其能量密度和功率密度分别达到了648.6 mWh·g-1和7000 mW·g-1以上.     

Effect of preparation methods on Co/ZrO2 catalysts in Fischer–Tropsch synthesis

Cobalt was incorporated into the zirconia support by different methods. The reducibility and activity of the catalysts was directly related to the preparation methods. Impregnated Co/ZrO₂ catalyst showed the highest reduction degree and the highest CO hydrogenation activity.     

Microwave-assisted synthesis and characterization of Bi-substituted yttrium garnet nanoparticles

Bi-substituted yttrium iron garnet (Bi-YIG, Bi_1.8Y_1.2Fe₅O₁₂) nanoparticles were prepared by microwave-assisted co-precipitation as well as conventional co-precipitation using ammonia aqueous solution as precipitant. The nanoparticles were characterized by thermal gravity-differential thermal analysis, X-ray powder diffraction, transmission electron microscopy, dynamic light scattering and vibrating sample magnetometer, respectively. The Faraday rotation of Bi-YIG modified PMMA slices was also investigated. Results demonstrate that the Bi-YIG nanoparticles prepared by microwave-assisted co-precipitation show smaller particle size and higher Faraday rotation than those prepared by conventional co-precipitation.     

Nano-sized Cu6Sn5 alloy prepared by a co-precipitation reductive route

Nano-sized Cu₆Sn₅ alloy powders were prepared by a co-precipitation reductive route using a hydrothermal method at 80 °C. The nano-size and morphology of the synthesized Cu₆Sn₅ alloy powders were evaluated by X-ray diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The obtained morphologies, chemical compositions are comparatively discussed. A variety of synthesis parameters, such as time, capping agent and sort of reductant, has an effect on the morphology of the obtained materials, and will be particularly highlighted.