Facile synthesis of magnetic iron oxide nanoparticles and their characterization

Magnetic iron oxide nanoparticles are synthesized by suitable modification of the standard synthetic procedure without use of inert atmosphere and at room temperature. The facile synthesis procedure can be easily scaled up and is of important from industrial point of view for the commercial large scale production of magnetic iron oxide nanoparticles. The synthesized nanoparticles were characterized by thermal, dynamic light scattering, scanning electron microscopy and transmission electron microscopy analyses.     

络合沉淀法合成纳米Y2O3:Yb,Er及其上转换发光性能

以EDTA为螯合剂,采用络合沉淀法合成了纳米级Yb、Er共掺杂的Y2O3上转换发光粉.通过X射线衍射(XRD)、透射电子显微镜(TEM)、光致发光(PL)光谱和红外(IR)光谱对微晶进行了表征.结果表明,经980℃焙烧后的粒子为单一的立方晶相,其颗粒基本为球形,并且其粒径约为30nm.PL谱和IR谱分析结果表明:纳米粒子的表面效应使得表面原子更易吸附空气中的水和二氧化碳,从而增强了4S3/2→4F9/2的无辐射弛豫过程,使得样品所发红光与体材料相比具有更高的荧光分支比.另外,本文还对样品的发光性能作了详细的讨论.     

功能化CdS纳米晶的合成及CdS/聚苯乙烯纳米杂化材料的研究

以氯化镉和硫化钠为原料,采用巯基乙醇为有机配体,在H2O/DMF的溶剂中,制得分散均匀且表面富含羟基基团CdS纳米晶溶液.我们使用γ-甲基丙烯氧丙基三甲氧基硅烷(MPS)来修饰CdS纳米晶的表面,得到双键官能团化的CdS纳米晶.通过原位自由基聚合方法,成功地得到了聚苯乙烯基CdS纳米晶复合材料.利用傅里叶红外光谱仪(FT-IR)、透射电子显微镜(TEM)、紫外-可见光吸收光谱仪(UV-vis)、X射线衍射分析仪(XRD)、热重分析仪(TGA)、荧光光谱 (PL) 考察了CdS纳米晶及CdS/聚苯乙烯复合材料的结构和光学性能的关系规律.结果表明巯基乙醇表现出良好的光学性能,其配体不是简单的物理吸附于纳米晶表面,而是以化学键的形式和纳米晶表面镉原子相结合.相比于纯的聚苯乙烯材料,聚苯乙烯基CdS纳米晶材料表现出良好的光学和热学性能.     

片状氧化物粉体的合成与性能

片状粉体具有特殊的二维平面结构和较大的径厚比 ,应用于颜料、涂料、化妆品和汽车面漆等产品时 ,表现出了优异的性能。简要介绍几种重要的片状氧化粉体的合成与性能 ,对进一步开发利用具有参考价值     

Synthesis, structural and mechanical characterization of sputtered tungsten oxide coatings

Tungsten oxide coatings were deposited without substrate bias by DC reactive magnetron sputtering of a tungsten target using oxygen as reactive gas. By tuning the partial pressure of oxygen (p_O2/p_Ar) between 0 and 4, the oxygen content of the films was changed from 0 to 75 at.%. The structure of the films (investigated by X-ray diffraction) depends on their oxygen content. For low oxygen contents, the -W and β-W₃O phases were observed (< 30 at.%), and with the increase of oxygen content (30 at.% < O < 67 at.%) the structure became amorphous. A transition region was obtained for oxygen content between 67 at.% and 75 at.%, and when O > 75 at.%, a nanocrystalline (WO₃) structure was reached.

The hardness and Young's modulus were evaluated by depth sensing indentation. The decrease in hardness followed the four different ranges of chemical compositions accordingly, from ≈ 23 GPa for pure W down to ≈ 7 GPa for WO₃ films. A similar behaviour was observed for the Young's modulus, which ranged from 450 GPa to 150 GPa. The cohesion/adhesion of the films were investigated using a scratch-test apparatus. These coatings displayed a low adhesion (critical load, L_c < 15 N) to the steel substrate because the depositions were carried out intentionally without an adhesion interfacial layer.     

Metal oxide/polyaniline nanocomposites: Cluster size and composition dependent structural and magnetic properties

Nanocomposites of iron oxide with conducting polymer in the form of powders of varying compositions have been studied to understand the effects of particle size, cluster size and magnetic inter-particle interactions. The sizes of the nanoparticles were estimated to be ∼ 10–20 nm from the X-ray diffraction (XRD) and the transmission electron micrographs (TEM). XRD shows a single crystalline phase for the γ-Fe₂O₃. The presence of conducting polymer was confirmed through Fourier transform infrared (FTIR) spectroscopy. The amount of polymer present in the composite, the transition temperature of iron oxide and the thermal stability of polymer was determined through thermogravimetric and differential thermal analysis (TGA-DTA). The room temperature magnetic hysteresis measurements show reduction in saturation magnetization with increasing polymer concentrations. A low value of coercivity was observed for low polymer composites. On increasing the polymer concentration, the coercivity and remanence become negligible indicating a superparamagnetic phase at room temperature. Beyond a certain composition, the system shows paramagnetic behaviour which is also confirmed through zero field cooled-field cooled (ZFC-FC) measurements. We also report preliminary results on the magnetic properties of self standing sheets prepared using γ-Fe₂O₃ and NiFe₂O₄ nanoparticles and conducting polymers.     

液-固-溶液法制备ZnSe:Fe纳米晶及其光学性能研究

采用液-固-溶液(LSS)法制备了ZnSe:Fe纳米晶,利用X射线粉末衍射(XRD)技术、透射电子显微镜(TEM)、光致发光(PL)谱、紫外-可见吸收(UV-vis)光谱以及傅里叶变换红外(FT-IR)光谱对所制备样品的结构和光学性质进行了表征,研究了掺杂Fe离子对ZnSe纳米晶光学性质的影响规律.实验结果表明所制备的...     

纳米NaYF4:Er3+,Yb3+上转换材料的合成及其性质研究

采用溶胶-凝胶法在水相合成了纳米NaYF_4:Er~(3 ),Yb~(3 )上转换材料,980nm红外激光照射下,肉眼可观察到明亮的上转换发光。实验研究了铒、镱掺杂浓度及焙烧温度对材料合成的影响。所合成的纳米材料呈圆球形、颗粒均匀、分散性好,平均粒径70nm,可应用于生物标记。     

Spindly cobalt ferrite nanocrystals: preparation, characterization and magnetic properties

In this paper we describe the preparation of homogeneously needle-shaped cobalt ferrite (CoFe(2)O(4)) nanocrystals on a large scale through the smooth decomposition of urea and the resulting co-precipitation of Co(2+) and Fe(3+) in oleic acid micelles. Furthermore, we found that other ferrite nanocrystals with a needle-like shape, such as zinc ferrite (ZnFe(2)O(4)) and nickel ferrite (NiFe(2)O(4)), can be prepared by the same process. Needle-shaped CoFe(2)O(4) nanocrystals dispersed in an aqueous solution containing oleic acid exhibit excellent stability and the formed colloid does not produce any precipitations after two months, which is of prime importance if these materials are applied in magnetic fluids. X-ray diffraction (XRD) measurements were used to characterize the phase and component of the co-precipitation products, and demonstrate that they are spinel ferrite with a cubic symmetry. Transmission electron microscopy (TEM) observation showed that all the nanocrystals present a needle-like shape with a 22?nm short axis and an aspect ratio of around?6. Varying the concentration of oleic acid did not bring about any obvious influence on the size distribution and shapes of CoFe(2)O(4). The magnetic properties of the needle-shaped CoFe(2)O(4) nanocrystals were evaluated by using a vibrating sample magnetometer (VSM), electron paramagnetic resonance (EPR), and a M?ssbauer spectrometer, and the results all demonstrated that CoFe(2)O(4) nanocrystals were superparamagnetic at room temperature.     

Nanostructured tungsten oxide with controlled properties: Synthesis and Raman characterization

Tungsten oxide thin films are interesting for their electrochromic and gas sensing properties. For technological applications, the control of morphology (effective surface, porosity) and structure (crystallinity, stoichiometry) at the nanoscale is of paramount interest to deliver distinctive properties.Nanostructured tungsten and tungsten oxide films have been synthesized by nanosecond pulsed laser deposition (PLD) starting from a W metallic target. Both inert and reactive buffer gases (He, Ar, dry air) have been exploited to induce cluster formation and/or oxidation and to vary the deposition energies of ablated species. A wide range of morphologies extending from compact and smooth, up to extremely porous and spongy-like structures have been obtained.The structure, the oxide phase and the degree of crystallinity of the films have been investigated by Raman spectroscopy. Films deposited in the presence of inert buffer gases reveal a spontaneous ex-situ oxidation, when exposed to ambient atmosphere, which is strongly related to the nanostructure. Instead, deposition in a varying pressure of dry air permits to grow tungsten oxide films and to tune their structure from amorphous to nano- and microcrystalline with different coexisting oxide phases.     

Synthesis temperature dependence of morphologies and properties of cobalt oxide and silicon nanocrystals

Cobalt and cobalt oxide nanocrystals were synthesized on Si substrates from aqueous cobalt nitrate [Co(NO₃)₂·6H₂O] powder via chemical vapor deposition method. Scanning electron microscope, field emission scanning electron microscope, and transmission electron microscope observations show different morphologies, such as continuous films, nano-bars, nano-dices, and nano-strings, depending on the synthesis temperature. The crystal structure characterization was conducted using X-ray diffraction methods. Furthermore, the properties of the samples were characterized using Raman spectroscopic analysis and vibrating sample magnetometer. The morpholo- gy change was discussed in terms of synthesis environments and chemical interactions between cobalt, oxygen, and silicon.     

壳聚糖修饰氧化铁磁性纳米颗粒的制备和性能研究

通过共沉淀法制备氧化铁磁性纳米颗粒,用壳聚糖对其表面进行修饰得到样品(CS@MNPS);表征其形貌结构、尺寸、表面基团、表面电荷、磁学性质和在不同介质中的稳定性等.实验结果表明,CS@ MNPs具有典型的立方反尖晶石晶体结构;粒径为16.5nm;在生理(pH值7.4)条件下拥有较高的正电荷(10mY);呈现超顺磁性,对驰豫时间T1、T2,尤其是T2*具有很强的响应;在双蒸馏水和含10％新生牛血清的RPMI 1640培养液中具有良好的稳定性,具有作为磁共振造影剂的潜力.     

Synthesis, characterization and humidity sensing properties of Cu-Sr-Al mixed metal oxide composites

Copper-strontium-aluminum mixed metal oxide composites prepared by sol-gel technique was investigated for humidity sensing properties. X-ray diffraction, scanning electron microscopy (SEM), FT-IR spectroscopy and nitrogen adsorption/desorption isotherm at 77 K was employed, respectively, to identify the structural phases, surface morphology, vibrational stretching frequencies and BET surface area of the composites. The composites were prepared with the mole ratios of Cu:Sr as (0.0:1.0, 0.2:0.8, 0.4:06, 0.6:0.4, 0.8:0.2 and 1.0:0.0) keeping the aluminium mole ratio as constant and were labeled as CuSA1, CuSA2, CuSA3, CuSA4, CuSA5 and CuSA6, respectively. The samples sintered at 900 °C for 5 h, were subjected to dc resistance measurements as a function of relative humidity (RH) in the range 5-98% and the results revealed that the sensitivity factor of CuSA5 possessed the highest humidity sensitivity of 42,000 while the pure composite copper aluminate (CuSA1) and strontium aluminate (CuSA6) possessed comparatively low sensitivities 10,000 and 20,000, respectively. The response and recovery characteristics of the composites CuSA1, CuSA5 and CuSA6 were studied.     

Synthesis and characterization of monodispersed orthorhombic manganese oxide nanoparticles produced by Bacillus sp. cells simultaneous to its bioremediation

A heavy metal resistant strain of Bacillus sp. (MTCC10650) is reported. The strain exhibited the property of bioaccumulating manganese, simultaneous to its remediation. The nanoparticles thus formed were characterized and identified using energy dispersive X-ray analysis (EDAX), high resolution transmission electron microscopy (HRTEM), X-ray photoelectron spectroscopy (XPS), powder X-ray diffraction (PXRD) and atomic force microscopy (AFM). When the cells were challenged with manganese, the cells effectively synthesized nanoparticles of average size 4.62 ± 0.14 nm. These were mostly spherical and monodispersed. The ex situ enzymatically synthesized nanoparticles exhibited an absorbance maximum at 329 nm. These were more discrete, small and uniform, than the manganese oxide nanoparticles recovered after cell sonication. The use of Bacillus sp. cells seems promising and advantageous approach. Since, it serves dual purposes of (i) remediation and (ii) nanoparticle synthesis. Considering the increasing demand of developing environmental friendly and cost effective technologies for nanoparticle synthesis, these cells can be exploited for the remediation of manganese from the environment in conjunction with development of a greener process for the controlled synthesis of manganese oxide nanoparticles.     

Effects of phosphorus doping on structural and optical properties of silicon nanocrystals in a SiO2 matrix

Promise of Si nanocrystals highly depends on tailoring their behaviour through doping. Phosphorus-doped silicon nanocrystals embedded in a silicon dioxide matrix have been realized by a co-sputtering process. The effects of phosphorus-doping on the properties of Si nanocrystals are investigated. Phosphorus diffuses from P-P and/or P-Si to P-O upon high temperature annealing. The dominant X-ray photoelectron spectroscopy P 2p signal attributable to Si-P and/or P-P (130 eV) at 1100 °C indicates that the phosphorus may exist inside Si nanocrystals. It is found that existence of phosphorus enhances phase separation of silicon rich oxide and thereby Si crystallization. In addition, phosphorus has a considerable effect on the optical absorption and photoluminescence properties as a function of annealing temperature.     

无Co混合导电型陶瓷透氧膜的制备和性质研究

首次合成了Ｓｒ１０－ｎ／２ＢｉｎＦｅ２０Ｏｍ（ｎ＝２，４，６，８，１０等）系列氧化物透氧膜，它们具有较高的透氧能力，其中，样品ｎ＝１０在１１００Ｋ时的透氧率为０．９０ｍｌ（ＳＴＤ）／（ｃｍ２·ｍｉｎ），比Ｓｒ１－ｘＢｉｘＦｅＯ３高约两倍．Ｓｒ１－ｘＢｉｘＦｅＯ３（ｘ＝０．１，０．３，０．５）系列的透氧率随Ｂｉ含量增加而增大．通过两个系列氧化物的ＸＲＤ和化学组成的对比，发现Ｂｉ离子含量和晶格空位浓度对透氧能力大小起决定性作用．     

Pebax/SAPO-34混合基质膜的制备及性能研究

选用Pebax1657和SAPO-34为膜材料,分别采用醋酸和1-丁醇为溶剂,通过流延法制备Pebax/SAPO-34混合基质膜(MMMs).研究发现,溶剂能显著地影响膜的结构形态以及渗透性能.纯Pebax膜的气体渗透系数受溶剂的影响较大,而选择性受溶剂影响不大.对于分子筛含量较高(质量分数33%)的MMMs,以1-丁醇为溶剂时,分子筛的分散均匀程度更高,但就材料的成膜性而言,醋酸为溶剂时更好.MMMs中气体渗透系数的变化是结晶度、扩散曲度、链段运动能力和膜形态等因素的共同作用的结果.醋酸为溶剂时,由于相分离的发生,气体的渗透系数出现突跃,最大提高到纯Pebax膜的3倍.1-丁醇为溶剂时,除H2外,气体渗透系数先出现一定程度的提高,而后由于受到链段僵化以及扩散曲度的影响而降低.     

Urchin-like Co2P nanocrystals: Synthesis, characterization, influencing factors and photocatalytic degradation property

In this paper, cobalt phosphides (Co₂P) nanocrystals with urchin-like structures have been successfully synthesized via a water-ethanol mixed-solvothermal route, employing white phosphorus (WP) and cobalt dichloride as starting reactants, sodium acetate as the pH adjustor, and sodium dodecyl benzene sulfonate (SDBS) as the surfactant. The as-obtained product was characterized by X-ray powder diffraction (XRD), energy dispersive spectrometry (EDS), (high resolution) transmission electron microscopy (TEM/HRTEM), selected area electron diffraction (SAED) and field emission scanning electron microscopy (FESEM). It was found that sodium acetate played an important role in the formation of Co₂P nanocrystals with urchin-like structures. Some factors influencing the morphology of the product, including the reaction temperature, time, amounts of WP and SDBS and so on, were investigated. The photocatalytic property of the product for the degradation of organic dyes was studied. A possible formation mechanism of urchin-like Co₂P nanocrystals was suggested based on the experiment results.     

Biferroic LuCrO3: Structural characterization,magnetic and dielectric properties

Multiferroic LuCrO₃ perovskite-type structure (Pbnm) obtained via auto-ignition synthesis was characterized by a combination of X-ray diffraction (XRD) and thermogravimetric (TG) techniques, and through magnetization and permittivity measurements. Results showed that amorphous combustion powders were fully transformed to orthorhombic LuCrO₃ structure at 1200 K after the first LuCrO₄ crystallization at 700 K. The magnetic response displays thermal irreversibility between zero-field-cooling and field-cooling condition which is due to spin canted AF switching at 116 K. Accordingly, a hysteresis loop in the M(H) data confirms weak ferromagnetism in LuCrO₃. On the other hand, the permittivity measurement shows a broad peak transition typical of relaxor-type ferroelectrics transition at ∼450 K. Electrical conductivity increases as temperature increases showing an anomaly around the diffuse phase transition. The diffuse phase transition and the formation of the charge carriers are discussed in terms of a local distortion around the Lu Site.     

Vanadium oxide nanodisks: Synthesis,characterization, and electrochemical properties

Highly crystallined VO_1.6·H₂O nanodisks assembled from nanoparticles have been successfully fabricated under hydrothermal conditions by using bulk V₂O₅ and Na₂S₂O₃ as the starting materials in the presence of surfactant polyethylene glycol 4000 (PEG-4000). The nanodisks have a diameter of 200 nm and thickness of 40 nm. Hollow nanodisks are occasionally observed, which is similar to Chinese ancient copper coins. The formation of nanodisks can be ascribed to a novel solid-solution-solid growth mechanism. Compared with other methods, the solid state transformation method is simple and economic. In addition, the nanodisks exhibit good electrochemical behavior and promising to be used in lithium-ion battery.