Effect of substitution of K ions on the structural and electrical properties of nanocrystalline MgAl2O4 spinel oxide

Potassium substituted nanosized magnesium aluminates having a nominal composition Mg_1−xK_xAl₂O₄ where x=0.0, 0.25, 0.5, 0.75, 1.0 have been synthesized by the chemical co-precipitation method. The samples have been characterized by means of X-ray diffraction (XRD), scanning electron microscope (SEM), and dc electrical resistivity measurements. The XRD results reveal that the samples are spinel single phase cubic close packed crystalline materials. The calculated crystallite size ranges between 6 and 8 nm. The behaviour of the lattice constant seems to deviate from the Vegard's law. While X-ray density clearly increases, the bulk density and consequently, the percentage porosity do not exhibit a significant change on increasing the K⁺ content. The SEM micrographs suggest homogeneous distribution of the nanocrystallites in the samples. The dc electrical resistivity exhibits a typical semiconducting behaviour. Substitution of a Mg²⁺ ion by a K⁺ ion provides an extra hole to the system, which forms small polaron. Thermally activated hopping of these small polarons is believed to be the conduction mechanism in the Mg_1−xK_xAl₂O₄. The activation energy of hopping of small polarons has been calculated and found K⁺ ions content dependent.     

Preparation and magnetic properties of barium ferrites substituted with manganese, cobalt, and tin

Barium ferrites substituted by Mn-Sn, Co-Sn, and Mn-Co-Sn with general formulae BaFe_12−2xMn_xSn_xO₁₉ (x=0.2-1.0), BaFe_12−2xCo_xSn_xO₁₉ (x=0.2-0.8), and BaFe_12−2xCo_x/2Mn_x/2Sn_xO₁₉ (x=0.1-0.6), respectively, have been prepared by a previously reported co-precipitation method. The efficiency of the method was refined by lowering the reaction temperature and shortening the required reaction time, due to which crystallinity improved and the value of saturated magnetization increased as well. Low coercivity temperature coefficients, which are adjustable by doping, were achieved by Mn-Sn and Mn-Co-Sn doping. Synthesis efficiency and the effect of doping are discussed taking into account accumulated data concerning the synthesis and crystal structure of ferrites.     

Synthesis of nanocrystalline Co-Ni alloys by precursor approach and studies on their magnetic properties

Nanocrystalline Co-Ni alloys with different compositions were prepared by polyol reduction of mixed cobalt nickel hydroxides. The precursors (mixed cobalt nickel hydroxides) were prepared by co-precipitation. Powder X-ray diffraction analysis indicated the formation of fcc phase in the alloys and their crystallite size in the range 17-25 nm. Scanning electron microscopy and transmission electron microscopy studies revealed the morphology of the particles as being close to spherical, and the energy dispersive X-ray analysis showed the stoichiometry of the alloys. The magnetization as a function of field and temperature of the alloys, measured using a superconducting quantum interference device, showed superparamagnetic behavior with negligible coercivity and remanence values.     

Finite size effect on Gd doped CoGdxFe2−xO4 (0.0≤x≤0.5) particles

Nanoparticles of CoGd_xFe_2−xO₄ (where x=0.0, 0.1, 0.3, 0.5) series have been prepared by chemical co-precipitation. The effect of Gd³⁺ ion concentration on crystalline phase, crystallinity, crystallite size, molecular vibrations and magnetic resonance has been investigated in detail. The crystallinity decreases with an increase in Gd³⁺ ion concentration and changes the structural parameters. The spin lattice relaxation has been correlated with the doping ion concentration. Similarly, the superparamagnetic behavior of these particles has been observed with EPR spectroscopy.     

Cr3+ doped Al2O3 nanoparticles: Effect of Cr3+ content in intensifying red emission

Cr³⁺-doped α-Al₂O₃ nanoparticles (Al_2−xCr_xO₃, 0.005 ≤ x ≤ 0.05) were synthesized by co-precipitation method. X-ray diffraction (XRD) patterns of Cr³⁺:Al₂O₃ nanoparticles revealed the crystallite size of ∼53 nm and electron microscopy (SEM & TEM) confirmed the spherical nanoparticle formation. Diffuse reflectance spectra (DRS) displayed peaks at 406 and 558 nm corresponding to the Cr³⁺ transitions which became prominent with the increase in Cr³⁺ concentration which was also evidenced by the gradually increasing pink coloration of the samples. Photoluminescence (PL) studies showed the sharp red emission at 694 nm (ruby line) which was observed for all samples. The Dq/B value for all samples was found to be greater than 2.3 confirming the presence of Cr³⁺ ions in the octahedral sites. Chromaticity diagrams displayed the maximum red appearance for the sample with x = 0.01 and a lifetime of 4 ms. The synthesized Cr³⁺:Al₂O₃ nanoparticles with smaller crystallite sizes and narrow near monochromatic emission can be used in various applications including sensing, lasing, and bioimaging applications.     

Synthesis of EDTA-modified magnetic activated carbon nanocomposite for removal of permanganate from aqueous solutions

In this study, activated carbon particles were magnetized by different amounts of maghemite in different temperatures using co-precipitation method and the resultant nanocomposite were modified with ethylenediaminetetraacetic acid (EDTA) to increase the permanganate contaminants adsorption capacity and to prevent degradation and oxidation of maghemite nanoparticles. Various properties of nanocomposite were investigated using different techniques including, vibrating sample magnetometer, scanning electron microscopy, X-ray diffraction, and Fourier transform infrared spectrometer. Different kinetics, isotherms and thermodynamic models of adsorption process were investigated. Comparing data with kinetic models showed that the adsorption process complies with the pseudo-second-order kinetic model. The study of equilibrium isotherms data at different temperatures indicated that the adsorption process is more compatible with Langmuir model. Negative values of ΔG and positive values of ΔH revealed that adsorption process is spontaneous and endothermic. Response surface methodology was used to determine optimal parameters of an adsorbent dose of 1 g L⁻¹, pH = 2 and initial permanganate concentration of 50 mg L⁻¹, according to which, the maximum capacity of permanganate adsorption obtained under optimal conditions was 93.86 mg g⁻¹.     

TiO2ZrO2 composite: Synthesis,characterization and application as a facile,expeditious and recyclable catalyst for the synthesis of 2-aryl substituted benzoxazole derivatives

The activity of an efficient mesoporous TiO₂ZrO₂ composite catalyst for the synthesis of 2-aryl substituted benzoxazole derivatives using 2-aminophenol and substituted benzaldehydes/heterocyclic aldehydes at moderate temperature was studied. The catalyst was prepared by a co-precipitation method and characterized by X-ray diffraction, BET surface area and scanning electron microscopy. The effect of temperature, solvents and catalyst concentration on the synthesis of benzoxazole derivatives was systematically investigated. Short reaction times, green-reaction profiles, good to excellent yields, reliable cost efficiency, simple workup conditions and reusability of an eco-friendly catalyst are the noteworthy highlights of the reported method. The catalyst could be easily recovered and reused several times without any significant loss in the yield. The use of the present catalytic system to mediate the title chemical synthesis in a synthetic operation is important for the development of new atom-economic strategies and this is efficient in building complex structures from simple starting materials in an environmentally benign fashion.     

Catalytic properties of a (A=Ba, Ca, Sr and Y) modified lanthanum hexaaluminates for catalytic combustion of methane

A series of hexaaluminates, La_0.8A_0.2MnAl₁₁O_19−δ samples (A = Ba, Ca, Sr and Y) as new catalysts were prepared by carbonate precipitation and calcined at high temperature. The structure and properties of these samples were characterized by XRD, BET and XPS techniques. Upon calcination at 1200°C, the hexaaluminate structure was formed and it retained the specific surface area of 17∼20 m²g⁻¹. The La_0.8Ca_0.2MnAl₁₁O_19−δ catalyst has a surface area of 19.3 m²g⁻¹ and shows a good activity in CH₄ combustion.     

Tartaric acid-assisted co-precipitation synthesis of Er3+-doped Lu2O3 nanopowders

Erbium-doped lutetia nanopowders were synthesized by a novel co-precipitation method using tartaric acid as precipitant.The properties of the samples were investigated by Fourier transform infrared spectroscopy（FTIR）,X-ray diffraction（XRD）,TG-DSC, field emission scanning electron microscopy（FE-SEM）,and upconversion luminescence analysis.Pure cubic Lu₂O₃ nanopowders were directly obtained when the precursor was calcined at 800℃for 2 h,the samples showed strong upconversion luminescence under excitation of 980 nm laser diode.     

氢氧化锰共沉淀分离-催化极谱法测定土壤中有效钼

土壤样品中有效钼用草酸铵-草酸混合溶液(pH 3.3)振摇提取,所得悬浮液用干滤纸过滤,分取部分滤液蒸缩体积后加入10 g.L-1酸性高锰酸钾溶液并蒸发至近干,趁热加0.25 mol.L-1氢氧化钠溶液进行共沉淀分离。分取部分上清液,用硫酸(1+1)溶液酸化后加入混合底液(其中含有二苯基乙醇酸、二苯胍及氯酸钠)及少许钛铁试剂溶液作为与钼(Ⅵ)进行催化反应的试剂体系。用JP-303极谱仪进行测定。在-220 mV峰电位处测得的峰电流值与其相应的钼(Ⅵ)的质量浓度在0.8～20μg.L-1范围内呈线性关系。此方法的检出限(3s/k)为0.002 6μg.g-1。用此方法分析了5个土壤标准物质,所测得有效钼的含量与其认定值相符。