Synthesis and characterization of high purity hydroxyapatite nanorods by hydrothermal technique

High purity hydroxyapatite (HAp) nanorods were synthesized by hydrothermal technique using Ca(NO3)2 x 4H2O and (NH4)2HPO4 as starting materials in a hydrothermal reactor at 150-200 degrees C for 12-24 h with pH6 and pH9.5, respectively. The prepared HAp nanorods were characterized by XRD, FTIR, and TEM techniques. The XRD results confirmed the formation of pure phase of HAp at pH9.5. With increasing temperature and time, the crystallinity of the HAp was increased, showing the hexagonal structure of HAp with the lattice parameter a in a range of 1.144-1.148 nm and c of 0.723-0.724 nm. The crystalline sizes of the powders were found to be 44-85 nm as evaluated by the XRD line broadening technique. The chemical compositions of the HAp nanorods were characterized by FTIR spectroscopies. The peaks of the phosphate carbonate and hydroxyl vibration modes were observed in the FTIR spectra for all the samples. The morphology of the HAp was nanorods of diameter less than 100 nm, as revealed by TEM. Increasing the temperature and time resulted in the transition from polycrystalline to single crystalline phase of the HAp, as clearly confirmed by the analysis of TEM diffraction patterns.     

Refractory metal nanopowders: Synthesis and characterization

Refractory nanometals have been the subject of interest for the past two decades in order to manufacture compact materials with dramatically improved mechanical properties for aerospace, military, chemical and metallurgical applications. The interest in nanomaterials has led to the development of many synthetic methods for their fabrication. In this review the challenges, synthesis methods and the characteristics of refractory metal nanopowders of IV–VI sub-group of the periodic table are discussed. Special attention is paid to salt-assisted combustion reaction (SACR) as a promising technique for the large-scale production of refractory metal nanopowders.The current paper will: (1) focus on the synthesis methods, morphology and physical–chemical characteristics of metal nanopowders; (2) present the specific feature of the salt-assisted combustion reaction, combustion parameters and macro-kinetic aspects of chemical reactions in the powder bed; and (3) demonstrate the perceptiveness of the fabrication route for the mass production of nanosized powders.     

Preparation and characterization of single-crystalline gallium oxide nanobelts

Single-crystalline β-Ga₂O₃ nanobelts were synthesized by a simple physical evaporation method in argon atmosphere with the starting materials of Ga. The β-Ga₂O₃ nanobelts have a width of 50-100 nm and width-to-thickness ratios of 5-10, and length of up to a few millimeters, which may have potential applications in nanosize sensors or optoelectronic nanodevices.     

Template-free hydrothermal derived cobalt oxide nanopowders: Synthesis,characterization, and removal of organic dyes

Pure spinel cobalt oxide nanoparticles were prepared through hydrothermal approach using different counter ions. First, the pure and uniform cobalt carbonate (with particle size of 21.8–29.8 nm) were prepared in high yield (94%) in an autoclave in absence unfriendly organic surfactants or solvents by adjusting different experimental parameters such as: pH, reaction time, temperature, counter ions, and (Co²⁺:CO₃^2?) molar ratios. Thence, the spinel Co₃O₄ (with mean particle size of 30.5–47.35 nm) was produced by thermal decomposition of cobalt carbonate in air at 500 °C for 3 h. The products were characterized by powder X-ray diffraction (XRD), Fourier transform infrared (FTIR), transmission electron microscope (TEM), scanning electron microscope (SEM), and thermal analysis (TA). Also, the optical characteristics of the as-prepared Co₃O₄ nanoparticles revealed the presence of two band gaps (1.45–1.47, and 1.83–1.93 eV). Additionally, adsorption of methylene blue dye on Co₃O₄ nanoparticles was investigated and the uptake% was found to be >99% in 24 h.     

State-of-the-art in analytical characterization of high purity solid samples by different spectroscopic methods

Facilities and some results of several spectroscopic methods which have potential applications in the field of analysis of solid high purity substances and which have been elaborated in Russia, will be discussed in this paper. Laser nondispersive atomic fluorescence method with glow discharge cathode sputtering atomiser, may be used for trace element determination as well as a tool for the investigation of technological processes, viz. deposition of thin films. Investigations on reduction of a background level in the new hollow cathode ion source for mass-spectrometry have been carried out. Laser mass spectrometry with tandem laser mass reflectron is successfully designed and applied for gaseous impurities determination in high pure silicon with limit of detection of 10⁻³–10⁻⁵ ppm wt. Several results of the layer-by-layer and bulk trace analysis of solids by high resolution mass spectrometry with radio frequency powered glow discharge ion source with the limits of detection at 10⁻¹–10⁻³ ppm wt will be presented here. The traditional arc and spark emission technique still finds considerable use. One of the examples considered in the paper is the analysis of metalfullerenes. To overcome the calibration problem the fluorination process inside the electrode crater using zinc fluoride has been investigated.     

聚1-萘胺纳米颗粒的合成及表征

采用界面聚合法合成了聚(1-萘胺)纳米颗粒.利用红外光谱(FT-IR),紫外可见吸收光谱(UV-vis),电子扫描显微镜(SEM),投射电镜(TEM),X射线衍射(XRD),循环伏安(cyclic voltammogram)等测试方法,对聚合物进行了表征并对聚合物形貌、结构及性能进行了初步探讨.结果表明,界面聚合法合成的聚(1-萘胺)呈现直径在100nm内的颗粒状分布;XRD结果显示,聚(1-萘胺)为半结晶态聚合物;界面聚合法合成的聚(1-萘胺)具有一定的电化学活性.     

溶剂热合成纳米钛酸钡及其表征

为满足钛酸钡纳米陶瓷的需求,本文用TiCl4和Ba(OH)2作前驱体,乙醇和乙二醇甲醚作混合溶剂,溶剂热合成了钛酸钡纳米粉体,并使用TEM、XRD和Raman光谱对产物进行了表征.结果表明,在本文条件下可以得到粒径为10~80 nm纳米粉体,通过控制反应条件可以达到控制颗粒尺寸的目的,反应时间和反应温度对颗粒尺寸有显著的影响.     

乙醇/水复合溶剂中纳米CaF2的沉淀制备及表征

用纯水溶剂和水/乙醇复合溶剂沉淀制备了不同粒径的CaF2纳米粉体.用FSEM和XRD对沉淀粉体的粒径和形貌进行了观测.研究发现,使用复合溶剂减小了产物纳米CaF2的粒径,从纯水溶液制备的51nm减小到1:4复合溶剂的20nm,并且沉淀粒径随复合溶剂中乙醇含量升高而减小.结果表明,复合溶剂是沉淀制备纳米粉体中控制粒径的有效手段.     

Synthesis, characterization and luminescence spectroscopy of oxide nanopowders activated with trivalent lanthanide ions: The garnet family

In this review, we deal with the preparation, structural investigation and especially optical spectroscopy of the garnet family of oxide materials activated with trivalent lanthanide ions, in the nanocrystalline form. In particular, attention is devoted here to the important garnet hosts; their synthesis, structure and luminescence spectroscopy are presented and discussed, with particular emphasis given to the possibility of obtaining efficient luminescence from trivalent lanthanide ions at the nanoscale, and to the potential and envisaged technological applications of this class of materials.     

Synthesis and characterization of vanadium oxide thin films on different substrates

In this study, the V₈O₁₅ derivative of vanadium oxide was produced on plain glass, indium tin oxide and silicon wafer substrate layers by taking advantage of wet chemical synthesis which is an easy and economical method. The structural properties of the produced films were examined by XRD and SEM analyses. Besides, Al/VO_x/p-Si metal-oxide-semiconductor (MOS) structure was obtained by the same synthesis method. Doping densities of these MOS structures were calculated from frequency dependent capacitance–voltage measurements. It was determined that the interface states which were assigned with the help of these parameters vary according to frequency.     

Analytical challenges in characterization of high purity materials

Available analytical literature reveals that it is possible to identify a lot of procedures to carry out any determination using a plethora of analytical techniques. The fundamental analytical requirements for realizing the desired and acceptable information from a chemical analysis are representative nature of the sample, precision, accuracy, selectivity and sensitivity. These decide, to a larger extent, the selection of the most appropriate methodology in order to obtain chemical information from a system. A number of analytical methodologies are being used in the author’s laboratory for carrying out trace elemental analysis as a part of chemical quality control. Quite a good number of analytical challenges with specific reference to the characterization of high purity materials of relevance to nuclear technology were addressed and methodologies were developed for trace elemental analysis of both metallic and non-metallic constituents. A brief review of these analytical challenges and the analytical methodologies developed and also the future needs of analytical chemist are presented in this paper.     

Synthesis, characterization and dielectric properties of europium-doped barium titanate nanopowders

Europium-doped cubic barium titanate (BT) nanocrystals with % [Eu/Ti] mol ratio varying from 0.05 to 0.25 were prepared through hydrothermal route. The nano nature of these powders was confirmed by XRD and TEM studies. Pellets were prepared after calcining the powders at 1000 °C for 2 h. These pellets were annealed at 200, 500, 700 and 1000 °C for 2 h at each temperature and used for dielectric measurements. Raman spectra of two typical pellets with %[Eu/Ti] Eu/Ti mol ratios of 0.15 and 0.25 showed all the peaks characteristic of tetragonal BaTiO₃. Pure BT showed a low dielectric constant (DC) with a value of 398. Doping with small amounts of Eu resulted in many fold increase of DC values. A maximum value of 10576 at 1 KHz frequency was observed for the sample with % [Eu/Ti] mol ratio of 0.15. Lowering of Curie temperature T_c (95 to 110 °C) was observed for pure as well as Eu-doped barium titanate.     

氧化钇纳米粉体材料的制备

以YCl3为原料 ,以Na2 CO3为添加剂 ,聚乙二醇 4 0 0为分散剂 ,首先制备出晶粒细小的碳酸钇前驱体。在 70 0℃焙烧 1h后制得Y2 O3纳米粉体材料 ,经XRD和TEM检测 ,粒径为 5 0nm ,粒度均匀     

高纯铝阳极氧化膜的电化学行为研究

为考察氧化膜状态对其电化学性能的影响,采用电化学方法研究了高纯铝阳极氧化膜在磷酸二氢钠缓冲溶液中的电化学性能.测试结果表明,高纯铝氧化膜的阴极极化过程分为3个阶段:1)电流密度变化较小而电位迅速负移,系克服氧化膜阻挡层电阻阶段;2)电流密度迅速增大而电位变化较小的析氢阶段;3)电流密度变化较小而电位迅速负移的氢离子扩散...     

Fe-C纳米粉体的制备及特性

在50%CH4 20%H2 30%Ar,总压为2×104Pa的混合气氛下,用直流电弧等离子体蒸发纯Fe制备了Fe-C纳米粉体.用XRD、TEM、HRTEM、XPS、VSM、化学分析和氧含量分析等测试手段对粉体进行了分析.结果表明,在50%CH4 20%H2 30%Ar的混合气氛下制备的粉体形貌接近类球形,平均粒度50nm,粒子具有核壳结构,核为Fe-C,壳为4nm左右的碳膜.在温度低于300℃时,在50%CH4 20%H2 30%Ar气氛下制备的纳米粉体抗氧化性比在50%H2 50%Ar气氛下制备的强,饱和磁化强度为151.8Am2/kg,比在纯CH4气氛下制备的106.3Am2/kg大.     

Synthesis and characterization of highly crystalline MgO nanopowders via a modified chemical-precipitation process

A modified chemical-precipitation method is proposed to synthesize MgO nanopowders with high crystallinity at a low temperature of 400 degrees C using acetic acid as a modifier. The as-obtained intermediates and final products were investigated by Fourier-transformed infrared spectroscopy, thermogravimetric analysis, X-ray diffraction and transmission electron microscopy, respectively. The influence of acetic acid in the MgO preparation process was also investigated by a comparison of the samples without acetic acid, and the mechanism of acetic acid modification is also proposed. The carboxyl group of acetic acid could coordinate with Mg atom in a monodentate mode to form a new organic ligand intermediate Mg(OH)(OCOCH3), which facilitates the thermal decomposition of the intermediate at low temperature and enhances the crystallization of MgO.