一种便捷方法制备表面氨基化的超顺磁Fe_3O_4纳米粒子

提出了一种简便易行的对磁性纳米粒子表面进行氨基化的方法.首先使用化学共沉淀法合成了粒径为10 nm左右的Fe_3O_4纳米粒子,然后用阿仑膦酸钠对其表面进行修饰,使其表面具有了功能化的氨基.利用透射电子显微镜(TEM)、X射线衍射(XRD)、振动样品磁强计(VSM)、动态光散射(DLS)仪、热重分析(TGA)仪、傅里叶变换红外(FT-IR)光谱仪、X射线光电子能谱(XPS)仪等对其进行表征.结果显示磁性纳米粒子表面被成功地修饰了一层双膦酸分子.所制备的纳米粒子可在pH=6.3稳定存在4周以上.     

Influences of surfactant (PVA) concentration and pH on the preparation of copper nanoparticles by electron beam irradiation

Electron beam irradiation method was successfully applied to the preparation of Cu nanoparticles in aqueous solution under room temperature and ambient pressure using polyvinyl alcohol (PVA) as the surfactant. The influences of the pH on the products were studied by X-ray diffraction (XRD), and those of the surfactant PVA concentration on the particle size and agglomeration by ultraviolet–visible spectrophotometry (UV–vis) and laser scattering particle size distribution analysis (LSPSDA). The products were characterized by XRD and transmission electron microscopy (TEM). The results showed that the grain size of Cu nanoparticles, within a certain range, can decrease with increasing PVA concentration. Pure Cu nanoparticles with the grain size distribution of 5–50 nm were prepared when the pH was adjusted between 5.0 and 9.0, and the PVA concentration was 2.20 g/100 mL.     

Crystal Orientation Mapping Applied to the Y-TZP/WC Composite

 Crystal orientation measurements made by electron backscattered diffraction (EBSD) in the scanning electron microscope (SEM) and microscopic observations provided the basis for a quantitative investigation of microstructure in an yttria stabilised, tetragonal zirconia-based (Y-TZP) composite. Automatic crystal orientation mapping (ACOM) in a SEM can be preferable to transmission electron microscopy (TEM) for microstructural characterisation, since no sample thinning is required, extensive crystal data is already available, and the analysis area is greatly increased. A composite with a 20 vol.% tungsten carbide (WC) content was chosen since it revealed crystal relationships between the matrix and carbide phase already established by TEM analysis. However, this composite was difficult to investigate in the EBSD/ SEM since it is non-conductive, the Y-TZP grain size is of the order of the system resolution, and the sample surface, though carefully prepared, reveals a distinctive microtopography. In this paper, some useful solutions to these problems are discussed and the resulting data, which confirm crystal correlations previously established by TEM analysis, are presented.     

Conversion electron yield X-ray absorption fine structure measurements under atmospheric conditions

The detection of a sample current under atmospheric conditions was applied to XAFS measurements of a Ni foil and NiO powders, and the feasibility of the conversion electron yield (CEY) detection was examined. The obtained XAFS spectra were compared with those obtained using the conventional transmission method; it is concluded that fairly good statistics can be obtained using the CEY method and that the obtained spectra show an identical structure to those obtained using the transmission method.     

Homogeneous sample preparation for automated high throughput analysis with matrix-assisted laser desorption/ionisation time-of-flight mass spectrometry

This work presents a simple method for obtaining homogeneous sample surfaces in matrix-assisted laser desorption/ionisation time-of-flight mass spectrometry (MALDI-TOFMS) for the automated analysis of peptides and proteins. The sample preparation method is based on applying the sample/matrix mixture onto a pre-deposited highly diluted matrix spot. The pre-deposited crystals act as seeds for the new sample containing crystals which become much smaller in size and more evenly distributed than with conventional methods. This 'seed-layer' method was developed, optimised and compared with the dried-droplet method using peptides and proteins in the 1000-20,000 Da range. The seed-layer method increases the surface homogeneity, spot to spot reproducibility and sample washability as compared with the commonly used dried-droplet method. This methodology is applicable to alpha-cyanohydroxycinnamic acid, sinapinic acid and ferulic acid, which all form homogeneous crystal surfaces. Within-spot variation and between-spot variation was investigated using statistics at a 95% confidence level (n = 36). The statistical values were generated from more than 5000 data points collected from 500 spectra. More than 90% of the sample locations results in high intensity spectra with relatively low standard deviations (RSDs). Typically obtained data showed an RSD of 19-35% within a sample spot as well as in-between spots for proteins, and an RSD of < or = 50% for peptides. Linear calibration curves were obtained within one order of magnitude using internal calibration with a point-RSD of 3% (n = 10). The sample homogeneity allows mass spectra (average of 16 laser shots) to be obtained on each individual sample within 15 sec, whereby a 100 spot target plate can be run in 25 min. High density target plates using the seed-layer method were prepared by spotting approximately 100 picoliter droplets onto the target, resulting in sample spots < or = 500 microns in diameter using a flow-through piezo-electric micro-dispenser. By using this automated sample preparation step lower standard deviations are obtained in comparison to manually prepared samples.     

Plan-view preparation of TEM specimens from thin films using adhesive tape

A simple plan-view sample preparation technique for transmission electron microscopy (TEM) specimens is proposed for thin films by tearing-off the film with adhesive tape. The demand for very thin samples is highest for nanostructured materials where the structure of 2-5 nm sized features (grains) needs to be resolved; therefore, overlapping of nanometer-sized features should be avoided. The method provides thin areas at the fracture edges of plan-view specimens with thickness in the range of the grain size in the film allowing for artifact free high-resolution TEM imaging. Nanostructured materials typically fracture between the grains providing areas with the thickness of the grain size. Besides the swiftness of the method, the samples are free of surface amorphization artifacts, which can occur in ion beam milling up to 1 nm depth even at low energy ion bombardment. The thin film tear-off technique is demonstrated on a CuMn alloy thin film with grain size of 2 nm.     

溶剂热合成具有海绵状结构的介孔SnO2

采用溶剂热方法, 以SnCl4·5H2O/尿素/乙醇三元体系合成了具有特定结构的前驱体, 该前驱体经焙烧后得到了具有海绵状结构的介孔SnO2. 利用X射线粉末衍射(XRD)、傅立叶红外吸收光谱(FT-IR)、透射电镜(TEM)、热分析(TG-DTA)和氮气等温吸附鄄脱附等方法对产物的结构、形貌和热稳定性进行表征. 结果表明, 300 ℃焙烧处理后的样品由粒径约为5 nm的纳米粒子堆积而形成海绵状结构, 其中孔的尺寸范围在2-8 nm, 样品比表面积达到了134 m2·g-1.     

Influence of cobalt concentration on structural and optical properties of ZnS quantum dots

ZnS and Co-doped ZnS nanoparticles have been prepared by simple chemical precipitation method. Zinc acetate, sodium sulfide, and cobalt nitrate have been used as precursors for the preparation of Co-doped ZnS quantum dots. The X-ray diffraction results revealed that the undoped and Co-doped ZnS quantum dots exhibit hexagonal structure. The average grain size of quantum dot was found to lie in the range of 2.6–3.8 nm. The surface morphology has been studied using scanning electron microscope. The compositional analysis results confirm the presence of Co, Zn and S in the sample. The optical properties of undoped and Co-doped ZnS quantum dots have been studied using absorption spectra. TEM results show that undoped and Co-doped ZnS nanoparticles exhibit a uniform size distribution with average size of 2.5–3.4 nm.     

Synthesis and photocatalytic activity of nanocrystalline TiO2 co-doped with nitrogen and cobalt(II)

Nitrogen-modified cobalt-doped TiO₂ materials were successfully prepared via a modified sol–gel method. The structure and properties of the catalysts were characterized via X-ray diffraction (XRD), transmission electron microscopy (TEM), high-resolution TEM, ultraviolet–visible light diffuse reflectance spectra (UV–Vis DRS), N₂ adsorption–desorption isotherms, and energy-dispersive X-ray spectroscopy. The XRD patterns of the pure and co-doped TiO₂ samples indicate that the predominant phase was anatase. The average grain size obtained from TEM was approximately 10 nm. The Brunauer–Emmett–Teller analysis results indicate that the specific surface area was 77.7 m² g^?1. The UV–Vis DRS results for the co-doped sample reveal an absorption edge that had been red-shifted to 500 nm. The photocatalytic activities of the samples were evaluated through photodegradation of papermaking wastewater under UV and visible light irradiation. Compared with the cobalt-doped TiO₂ sample and Degussa P25, the 3 mol% N-doped mesoporous N/Co-TiO₂ photocatalyst exhibited the highest photocatalytic activity, which can be ascribed to the synergistic effect of the N and Co co-doping.     

Comparative study of the synthesis of KReO<Subscript>4</Subscript> using acrylamide sol–gel and solid-state reaction methods

KReO₄ was synthesized by solid-state reaction and for the first time by sol–gel method via acrylamide polymerization. X-ray diffraction analysis showed that a single phase of KReO₄ was obtained by both methods at 500–505 °C having a tetragonal unit cell. The solid-state reaction samples had a grain size of 5 μm and the sol–gel samples had fibrous aspect, agglomerated between 10 and 100 μm. By TEM it was observed nanocrystals of 100 nm, it is suggested that the xerogel fibers are formed by nanocrystals. From the results obtained, we concluded that the morphology is strongly influenced by the method of synthesis used.     

纳米氧化锆的物相与尺寸效应

用溶胶凝胶法制得ＺｒＯ２粉体。通过控制晶体尺寸得到了室温下稳定的立方相、四方相和单斜相。用Ｘ射线衍射（ＸＲＤ）、透射电镜（ＴＥＭ）、激光拉曼谱（ＬＲＳ）、电子顺磁共振（ＥＳＲ）等技术研究了晶体结构和晶粒尺寸的相互关系。试验表明：单斜相、四方相、立方相ＺｒＯ２的比表面能依次递减。因而，当晶粒尺寸减小至纳米级时，四方相和立方相都可变为室温下的稳态或亚稳态。     

Synthesis of highly stable silver nanoparticles by photoreduction and their size fractionation by phase transfer method

In this report we demonstrate a green chemical approach for the synthesis of stable silver nanoparticles in aqueous medium using tyrosine as an efficient photoreducing agent. A narrow size distribution of silver nanoparticles can be achieved by this simple photoirradiation method without using any additional stabilizing agents or surfactants. Two different irradiation sources have been explored resulting in a different particle size distribution pattern in each case. Further, we show that starting from a polydisperse tyrosine synthesized silver nanoparticles sample, it is also possible to fractionate them into different size ranges. The size fractionation was achieved by a 2 stage phase transfer method employing different organic solvents. The nanoparticles synthesized were characterized using UV-vis spectroscopy, Transmission electron microscopy (TEM) and X-ray diffraction (XRD) techniques.     

超微粒CO3O4的合成与表征

本文用胶溶法合成了纳米级超微粒Co_3O_4,初步探讨了合成Co_3O_4超微粒的最佳实验条件,对产品的结构性能测试表明,所得超微粒子Co_3O_4粒度均匀,平均粒度为4.0nm.200℃热处理时,产品为无定形,在许多有机溶剂中具有良好的分散性和透明性;400℃热处理得到立方Co_3O_4纳米晶体,平均粒度为6.0nm,热稳定性好。     

Misorientation mapping for visualization of plastic deformation via electron back-scattered diffraction.

The ability to map plastic deformation around high strain gradient microstructural features is central in studying phenomena such as fatigue and stress corrosion cracking. A method for the visualization of plastic deformation in electron back-scattered diffraction (EBSD) data has been developed and is described in this article. This technique is based on mapping the intragrain misorientation in polycrystalline metals. The algorithm maps the scalar misorientation between a local minimum misorientation reference pixel and every other pixel within an individual grain. A map around the corner of a Vickers indentation in 304 stainless steel was used as a test case. Several algorithms for EBSD mapping were then applied to the deformation distributions around air fatigue and stress corrosion cracks in 304 stainless steel. Using this technique, clear visualization of a deformation zone around high strain gradient microstructural features (crack tips, indentations, etc.) is possible with standard EBSD data.     

Preparation and Magnetic Property of La_(0.7)Sr_(0.3)MnO_3 Nanorod by Combination Sol-Gel with Molten Salt

La0.7Sr0.3MnO3(LSMO) nanorods were synthesized by a method combining sol-gel with molten salts at 950 °C for 10 h, which employed KCl+NaCl(mass ratio 4:1) as eutectic molten salts. The morphologies and magnetic properties of the resulting LSMO nanorods were investigated by X-ray diffraction(XRD), scanning electron microscopy(SEM), transmission electron microscopy(TEM), and vibrating sample magnetometer(VSM) measurements. It was found that the obtained perovskite manganite LSMO was a uniform nanorod with a d...     

Murraya Koenigii leaf-assisted rapid green synthesis of silver and gold nanoparticles

A facile bottom-up 'green' and rapid synthetic route using Murraya Koenigii leaf extract as reducing and stabilizing agent produced silver nanoparticles at ambient conditions and gold nanoparticles at 373 K. The nanoparticles were characterized using UV-vis, transmission electron microscopy (TEM), X-ray diffraction (XRD) and FTIR analysis. This method allows the synthesis of well-dispersed silver and gold nanoparticles having size ～10 nm and ～20 nm, respectively. Silver nanoparticles with size ～10 nm having symmetric SPR band centered at 411 nm is obtained within 5 min of addition of the extract to the solution of AgNO3 at room temperature. Nearly spherical gold nanoparticles having size ～20 nm with SPR at 532 nm is obtained on adding the leaf extract to the boiling solution of HAuCl4. Crystallinity of the nanoparticles is confirmed from the high-resolution TEM images, selected area electron diffraction (SAED) and XRD patterns. From the FTIR spectra it is found that the biomolecules responsible for capping are different in gold and silver nanoparticles. A comparison of the present work with the author's earlier reports on biosynthesis is also included.     

NdFeO3纳米晶的合成及气敏性能

以Nd2O3,Fe(NO3)3·9H2O,硝酸(1∶1)为原料,在柠檬酸体系中用溶胶凝胶法合成了具有钙钛矿结构的稀土复合氧化物NdFeO3;用XRD和TEM对产物的组成、颗粒大小、形貌进行了表征;结果表明:产物为纳米颗粒,平均粒径为28nm左右,且颗粒均匀。还采用静态配气法测试了材料的气敏性能,发现NdFeO3对H2S有很高的灵敏度,且抗干扰能力强,有较好的工业应用前景。     

Synthesis and Analysis of Tm3+ Doped YF3 Upconversion Luminescent Nano-materials

<正>Upconversion(UC)phosphor Tm~(3+)doped YF_3 nano-crystals were prepared by hydrothermal method under different conditions and characterized by Field Transmission electron microscopy(TEM),Scanning electron microscopy(SEM)and X-ray diffraction(XRD).Their UC luminescence properties were studied by fluorescence spectrophotometer with 980 nm diode laser excitation,and impact of different grain sizes and morphology on the UC luminescence intensity was discussed.The fluorescence decay lifetime was calculated by Multi-exponential function fitting method.Results show that UC emission intensity was enhanced with the reduction of grain size,and the decay lifetime is 0.60 us.     

一种便捷方法制备表面氨基化的超顺磁Fe3O4纳米粒子

提出了一种简便易行的对磁性纳米粒子表面进行氨基化的方法. 首先使用化学共沉淀法合成了粒径为10 nm左右的Fe3O4纳米粒子, 然后用阿仑膦酸钠对其表面进行修饰, 使其表面具有了功能化的氨基. 利用透射电子显微镜(TEM)、X射线衍射(XRD)、振动样品磁强计(VSM)、动态光散射(DLS)仪、热重分析(TGA)仪、傅里叶变换红外(FT-IR)光谱仪、X射线光电子能谱(XPS)仪等对其进行表征. 结果显示磁性纳米粒子表面被成功地修饰了一层双膦酸分子. 所制备的纳米粒子可在pH=6.3稳定存在4周以上.     

Structural and thermal properties of chemically synthesized Bi2Te3 nanoparticles

Bi₂Te₃ nanoparticles (NPs) have been synthesized at 50?°C by a low-cost wet chemical route. The structural properties of product sample were characterized by powder X-ray diffraction (XRD), transmission electron microscopy (TEM), and scanning electron microscopy. Thermal properties of product sample were investigated by differential scanning calorimetry (DSC), thermogravimetric (TG), and transient plane source techniques. The XRD and selected area electron diffraction of Bi₂Te₃ NPs result showed the polycrystalline nature with a rhombohedral (R3m) structure of the nanocrystallites. The average grain size of Bi₂Te₃ NPs was found to be about 30?nm by XRD and TEM measurements. DSC result shows one endothermic peak and one exothermic peak. TG result shows that only 48?% mass loss has occurred in Bi₂Te₃ sample. The obtained lower thermal conductivity of Bi₂Te₃ NPs is about 0.3?W m^?1 K^?1 at room temperature, which is caused by considering the crystalline nature of this material.