不同碳源和反应温度对原位合成SiC-TiC超细粉末的影响

以碳化硅(SiC)、二氧化钛(TiO2)和不同种类碳源为初始原料,采用碳热还原法在氩气气氛下原位合成SiC-TiC超细粉末.探讨了不同碳源和不同反应温度对所合成的SiC-TiC超细粉末的物相组成和显微形貌的影响.采用X-射线衍射仪(XRD)、激光粒度分析仪、扫描电镜(SEM)等手段对所合成的SiC-TiC超细粉末进行表征.实验结果表明,以蔗糖为碳源合成SiC-TiC超细粉末的适宜条件为1450 ℃保温2 h;以炭黑或葡萄糖为碳源合成超细粉末的适宜条件为1500 ℃保温2 h.三种碳源中以炭黑为碳源时所合成的SiC-TiC超细粉末粒度最小且合成出的粉末样品分散性好,大部分球状颗粒在0.5~1.0 μm 左右.在SiC粉末中原位合成的TiC颗粒,以粒径在0.1~0.2 μm左右的不规则的多样化结构颗粒存在.     

In‐situ TiC precipitation in molten Fe‐C and their characterisation

TiC particles were formed in liquid iron solution by the reaction between pure titanium and carbon available in molten iron. TiC particles have been precipitated in steels with four different carbon contents by in situ reactions during melting. The influence of titanium and carbon concentration on the precipitation of TiC was studied. The samples were studied by means of optical microscopy, scanning electron microscopy and X‐ray microanalysis. The morphology of the obtained crystals was studied and correlated with carbon and titanium. It was found that TiC crystallises as primary crystals at 1600°C during solidification of the Fe‐Ti‐C melt. The obtained crystals were of cubic, rectangle and had maximum size of 18.7 µm. The size and shape of the carbides increases with increasing carbon and titanium in molten iron. (© 2008 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

An estimation of the angular correlation curves being characteristic of positron annihilation in dislocations,vacancies, and vacancy clusters in Ni

Angular correlation curves are measured in Ni-0.1 at.% Sb; 90% cold-rolled during isochronal annealing. The behaviour of the parameters S, W, and R is interpreted by the formation of three-dimensional vacancy clusters nucleated at Sb atoms. Using results of positron lifetime measurement previously performed we estimate the angular correlation curves being characteristic of positron annihilation in bulk, dislocations, vacancies and vacancy cluster of different size (n = 5, 10, 20, and 50 vacancies per cluster).     

Influence of size on the supercooling in the crystallization of small particles in Bismuth island films

There has been measured the crystallization temperature of supercooled Bi particles versus their size in the 3–100 nm range in island films on amorphous carbon substrates. Crystallization temperature is found to decrease with particle size decreasing and the supercooling vanishes for particles of 2–3 nm in diameter. The results obtained are analyzed in the frame of the classic theory of crystallization.     

氩气退火时间对Fe(Se,Te)薄膜的性能影响研究

作为一种铁基超导薄膜,Fe(Se,Te)薄膜具有晶体结构简单、所包含的元素较少、易于合成的特点,不仅有利于超导机理研究而且有着潜在的技术应用价值。本文通过磁控溅射在温度为320 ℃的CaF₂单晶衬底上制备了Fe(Se,Te)薄膜,并在氩气氛围下进行了退火处理。研究了退火时间对Fe(Se,Te)薄膜的晶体结构、微观形貌、成分组成以及电输运特性的影响。结果表明:Fe(Se,Te)薄膜的结晶性较好,退火有助于消除薄膜样品中的FeSe相,薄膜的晶格常数c对退火不敏感,退火后薄膜晶粒尺寸变大;Fe(Se,Te)薄膜成分与靶材的名义组分存在一定的偏差,退火时间越长,Fe(Se,Te)薄膜表面的颗粒越密集;Fe(Se,Te)薄膜的电阻随温度升高而减小,呈现出半导体特性,退火3 h后电阻明显增大。     

多孔TiC陶瓷的制备、性能及机理研究

以TiO2和炭黑为反应物,TiC为添加物,通过反应烧结法制备出多孔TiC陶瓷.研究了TiC的添加量对晶粒大小、孔径尺寸、开气孔率及抗弯强度的影响.研究结果表明:随着TiC的添加量从0;增大到100;,反应生成TiC的粒径从0.17μm增大到0.71μm,孔径尺寸从0.15μm增大到1.51μm,开气孔率从78;持续降到38;,抗弯强度先增加后减小,添加量为80;时最高(86 MPa).TiC生长机理主要是由于添加的TiC使TiO2周围的碳含量减少,从而导致反应生成TiC的熔点降低,扩散能力提高,晶粒粒径增大.     

核壳结构CdS@C纳米复合材料的光催化性能研究

采用水热碳化法成功制备了不同碳含量的CdS@C纳米颗粒,同时对CdS@C的晶体结构、形貌、光学性能、光电化学和光催化性能进行了研究。实验结果表明本方法制备的碳包覆CdS纳米颗粒外壳为碳层,内核为六方纤锌矿结构CdS颗粒。CdS@C颗粒分散性良好,颗粒形貌主要为类球形,粒度均匀。X射线光电子能谱(XPS)证实CdS@C颗粒表面负载的碳主要以非晶碳形式存在。紫外-可见光光谱(UV-Vis)表明CdS@C纳米晶中表面碳的敏化作用提高了可见光响应范围,使得能隙变窄。光致发光光谱(PL)表明碳包覆CdS@C纳米颗粒的发光强度比纯CdS弱,有效抑制了光生载流子的复合。瞬态光电流响应和电化学阻抗谱(EIS)说明CdS@C纳米复合材料更有效促进电子-空穴对分离和提高转移效率。CdS@C纳米复合材料在可见光辐射下表现出良好的光催化活性和稳定性,其中·O₂^-和h⁺在光催化中起主要作用。     

微波水热法合成硅酸钇纳米晶

以硝酸钇、硅酸钠和氢氧化钠为主要原料,采用一种新方法-微波水热法可控合成了硅酸钇纳米晶.研究了起始溶液配比,合成温度及退火温度对硅酸钇的影响.采用X射线衍射仪(XRD)和透射电子显微镜(TEM)对粉体进行了表征.结果表明:随着合成温度的升高,Y_2SiO_5的含量增加.低温退火处理有助于提高硅酸钇微晶的结晶程度.选不同配比的溶液体系,经微波水热150 ℃作用10 min后,得到的前驱体于900 ℃下保温2 h,最终可获颗粒尺寸分别为400~600 nm、200~400 nm和400~600 nm的Y_2SiO_5、Y_(4.67)(SiO_4)_3O和Y_2Si_2O_7三种晶型的纳米晶,且其晶型最佳.     

On slow protein crystal nucleation: cluster‐cluster aggregation on diffusional encounters

With a view to experimental results on protein crystal nucleation the effects of cluster coalescence are probed semi‐quantitatively. The steric association restriction, which stems from the patchy surface of the protein molecules, explains both experimentally measured low crystal nucleation rate and coalescence limitations for crystalline clusters of protein molecules. The conclusion is that due to its action, and the impact of rotational diffusion, the coalescence of critical (and/or supercritical) clusters should be rejected as a conceivable alternative for explaining the slow nucleation of protein crystals. Besides, the analysis of cluster‐cluster aggregation on diffusional encounters may be of more general interest; it may be helpful by considering the coalescence of structured bio‐nano‐particles. (© 2009 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

The formation of tin oxides in thin-film Sn/C/KCl(100) structures

The formation of oxides upon the thermal annealing (both in air and vacuum) of island tin films grown on a KCl(100) substrate, which was coated by a thin layer of amorphous carbon, has been investigated by transmission electron microscopy. It is established that thermal annealing at temperatures below the tin melting point (T _m) does not lead to phase transitions with the formation of new crystalline oxide phases. At the same time, the films undergo structural changes: the average size of blocks in the substrate plane decreases compared to those in an as-deposited film. Thermal annealing in air at temperatures above the tin melting point leads to the formation of multiphase oxide structures and increases the average size of blocks and islands in the substrate plane. It is shown that preliminary thermal annealing in air at temperatures below T _m hinders oxidation upon subsequent heat treatment.     

Facile fabrication of porous ZnO by a template free method

In this paper, a template free method has been employed to fabricate porous ZnO. Brick shaped precursor was first synthesized by a mild hydrothermal process. Accompanied with the decomposition of the precursor during the subsequent annealing treatment, porous ZnO with the inherited morphology of the precursor was obtained. The as‐prepared products were characterized by X‐ray diffraction (XRD) and scanning electron microscopy (SEM). It exhibited that the porous hierarchical frame consists of nano‐sheets with wurtzite‐type. The size of the pores as well as the size of the particles varied with the annealing temperature. Mechanism speculation showed that the crystal‐aggregation in the growth process of the precursor is the key to the establishment of pore structure. (© 2011 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Parallel simulation of random fractal growth using dynamic lattice liquid (DLL) model

The dynamic lattice liquid (DLL) model is proposed as a universal tool for investigating various aggregation processes. This model allows to perform simulations in systems with constant number of particles and explicit presence of a solvent. The fractals growth is investigated in the systems with different initial concentration of cluster forming particles. It is shown that fractal dimension increases with increasing initial concentration of particles which build up the cluster. The presented results show that DLL algorithm properly reflects structural and dynamic properties of such process.     

Investigation of defects in low-temperature-grown GaAs using optical transient spectroscopy

Optical transient current spectroscopy (OTCS) has been used to investigate defects in the low-temperature-grown GaAs after postgrowth rapid thermal annealing (RTA). Two samples A and B were grown at 220°C and 360°C on (0 0 1) GaAs substrates, respectively. After growth, samples were subjected to 30 s RTA in the range of 500–800°C. Before annealing, X-ray diffraction measurements show that the concentrations of the excess arsenic for samples A and B are 2.5×10¹⁹ and 1×10¹⁹ cm⁻³, respectively. It is found that there are strong negative decay signals in the optical transient current (OTC) for the annealed sample A. Due to the influence of OTC strong negative decay signals, it is impossible to identify deep levels clearly from OTCS. For a comparison, three deep levels can be identified for sample B before annealing. They are two shallower deep levels and the so-called As_Ga antisite defect. At the annealing temperature of 600°C, there are still three deep levels. However, their structures are different from those in the as-grown sample. OTC strong negative decay signals are also observed for the annealed sample B. It is argued that OTC negative decay signals are related to arsenic clusters.     

Nanometre resolution of silica hydrogel formation using time-resolved fluorescence anisotropy

We report a new approach to particle size measurement in sol–gels which is based on fluorescence anisotropy decay. The effect of siloxane polymerisation on silica particle size and microviscosity as a function pH and sodium silicate concentration is described from initial mixing with sulphuric acid to beyond the time to the macroscopic gel point, t_g. The decay of near infra-red fluorescence anisotropy of a dye probe molecule is interpreted in terms of two rotational correlation times corresponding to solvated unbound dye and dye bound to silica particles. As polymerisation proceeds, increasing take-up of the dye from the liquid phase onto silica particles occurs. Silica primary particles of maximum mean hydrodynamic radius ≈1.5 nm are found to be present within the first 20 min of mixing. At pH between 1 and 0.8, irrespective of t_g, the particle size increases to a maximum radius of ≈4.5 nm after ≈2000 min. Lowering the pH in the range 0.8–0.15 produces a maximum radius of ≈3.5 nm. For all the sols studied, intra-particle syneresis then reduces the final particle radius by ≈0.5 nm within ≈6000 min. Although the bulk properties of the sol–gel change drastically at t_g, the probe detects little change in the microviscosity.     

A position study on the effect of C,Cu, Ni and Sb on the defect annealing in cold-rolled iron

Positron lifetime and angular correlation measurements are used to study the formation of defects and their annealing behaviour in cold-rolled pure Fe and dilute Fe alloys with C, Cu, Ni, and Sb. The results show that positrons are trapped by dislocations and vacancy clusters. The effect of foreign atoms on the cluster formation and the annealing properties are discussed.     

Deposition of thick silica-titania sol-gel films on Si substrates

A process for production of thick (>10 μm) titania-doped silica films on Si substrates by repetitive spin-coating of sol-gel material and rapid thermal annealing for 10 s in the range 800–1200°C is described. The dependence of overall thickness and etch rate in buffered HF on annealing temperature is described, and it is shown that films annealed at low (< 1175°C) temperatures have a relatively large thickness and etch rate. However, films having the properties of fully densified material (minimum thickness and etch rate) can be produced by subsequent consolidation. The film stress characteristics are similar to those phosphosilicate glass formed by the same process: films annealed below a critical temperature (< 1075°C) are under tensile stress at the annealing temperature, and crack before a thick film can be built up. Refractive index data are given; these show that only fully consolidated films have the refractive index expected from their SiO₂ and TiO₂ compositions. Finally, discrepancies in results for thickness of unconsolidated single-layer and multilayer films are explained using a simple model that accounts for the effect of cumulative densification.     

Crystallization of silicon thin films by current‐induced joule heating using a tungsten overcoat

A modified crystallization process using current‐induced joule heating under vacuum is presented. A thin layer of high temperature resistant tungsten was sputtered on the amorphous silicon as the conducting and annealing medium. The thin film thickness was measured by α‐stepper. The high current density provided effective means in crystallizing the amorphous silicon layer. The crystalline morphology was studied by scanning electron microscopy (SEM) after Secco‐etch, transmission electron microscopy (TEM), and x‐ray diffraction (XRD), under different annealing conditions. The grain size was controlled in the range of 0.1‐0.5 μm and could be increased with annealing time. No tungsten silicide was found. Some defects were formed due to electron‐migration effect near the electrodes. (© 2007 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Effect of annealing and composition on crystal structure,surface morphology and optical absorption of chemically deposited Cd1‐xSnxS films

Cd_1‐xSn_xS thin films were successfully deposited on suitably cleaned glass substrate by chemical bath deposition method at 74 °C. Hydrated Stannous Chloride (SnCl₂.2H₂O) in aqueous solution was added to the CdS growing solution in different proportions. The experimental results indicate, a successful doping for lower concentration of Sn, saturation for intermediate doping levels, and a degradation of the doping process for higher concentration of Sn. Indirect (X‐ray diffraction) and Direct (Scanning electron microscopy) measurements were performed to characterize the growth and the nature of crystallinity of the different Cd_1‐xSn_xS films. The effect of annealing on the crystal structure and morphology of the deposited films has also been discussed. The X‐ray diffraction spectra show that the thin films are polycrystalline and have both cubic and hexagonal structure. The Interplanar spacing, lattice constant, grain size, strain, and dislocation density were calculated for as‐deposited and annealed films. The grain size was found to decrease from 5 nm to 0.89 nm with doping concentration of Sn. The grain size further decreased due to annealing at 400 °C. SEM studies show layered growth and long needle like structures along with some voids. After annealing the densification and smaller size of the particles was also observed. The optical absorption spectra show shifting of absorption peaks towards lower wavelength side (© 2010 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

A model of the effect of R.T. preageing on the nucleation of η′-precipitation in Al-Zn-Mg alloys

The effect of R.T. preageing on the precipitation of the η′ particles was investigated in two Al-Zn-Mg alloys. The results are explained by a model according to which during or immediately after the quench to RT vacancy, or vacancy-zinc clusters (nuclei) are formed. The heterogeneous formation of η′ particles during the artificial ageing takes place at the nuclei or at over-critical size GPZ in the more concentrated alloy or at solute-rich regions left behind after the complete reversion of GPZ in the alloy with lower Zn concentration.     

Small-angle neutron scattering data on C60 clusters in weakly polar solutions of fullerenes

Solutions of fullerence C₆₀ in carbon disulfide CS₂ have been investigated by small-angle neutron scattering. Combination of solubility, contrast, and incoherent scattering make it possible to measure and analyze the relatively small scattering cross section of this system. Along with single fullerene molecules, a small amount of large fullerene clusters (more than 100 Å in size) is found in these solutions. The formation of these clusters depends on the procedure of solution preparation. The size distribution functions of clusters are compared with the results of the phenomenological cluster model of fullerene solubility.