超细球形铜粉的制备工艺研究

以水合肼为还原剂,采用液相化学法对超细铜粉的制备工艺进行了研究。结果表明,直接还原Cu2O获得的铜粉粒度分布很不均匀,抗氧化性能差。在添加微量亚铁氰化钾和2,2’-联吡啶后,铜粉的形貌、粒度分布以及抗氧化性能得到很大改善。经两步还原硫酸铜可制备平均粒度0.5μm以下且分布范围窄的近球形铜粉,热分析表明,该粉末在空气中120℃以下无氧化。     

前驱物颗粒形貌对钨钴合金粉形貌的影响

研究了不同前驱物(草酸钴粉末、氧化钴粉末)颗粒形貌对钨钴合金粉形貌的影响.采用粉末共还原的方法制备钨钴合金粉末,通过SEM观察制备前后各种粉末形貌,讨论了钨钴合金粉形貌与不同前驱物(草酸钴粉末、氧化钴粉末)颗粒形貌之间的关系.     

脉冲电磁场对草酸钴粒度的控制

在脉冲电磁场(PEMF)作用下,以氯化钴为母液、草酸铵为沉淀剂,采用草酸盐沉淀法制备了尺度较小且粒度分布均匀的草酸钴粉体.初步分析了PEMF与草酸钴制备体系的交互作用机理.同时,利用FTIR争电导率实验为机理模型提供了强有力的实验证据.结果表明,施加PEMF条件下获得的沉淀产物为β-CoC2O4·2H2O,其平均粒径为3.5403μm,与未施加PEMF条件下制备的样品相比降低了60.13%.PEMF作用下,反应体系中稳定晶核数量的增加以及形核率的提高是草酸钴粒度减小及粒度分布得到改善的原因所在.     

次亚磷酸钠还原法制备纳米铜颗粒

利用液相还原两步法,油酸为萃取荆和保护剂,葡萄糖和次亚磷酸钠将五水硫酸铜分别还原为氧化亚铜和单质铜,制备得到了粒度为50～100nm左右分散均匀的球形纳米铜颗粒,并用XRD、SEM和TEM对其进行了表征.结果表明,在油酸的保护下,采用液相还原两步法可制得分散性好、具有抗氧化性能的球形纳米铜颗粒.     

松油醇包覆Cu-Ag复合纳米粉的氧化特性

用气-液两相稳定法制备了Cu-Ag复合纳米粉。并用XRD、 HRTEM、 DSC-TG、 红外光谱、 化学分析和氧含量分析等手段研究了粉体的相结构、 表面组成、 形貌、 粒度分布和氧化特性。结果表明, Cu-Ag复合纳米颗粒具有壳核结构, 核为纳米Cu-Ag, 壳为厚度10nm左右的松油醇(C₁₀H₁₈O)分子层和氧化层双层结构, 粉体的粒度分布为20~150nm。在空气中, 220℃包覆在Cu-Ag复合纳米粒子表面的松油醇分子开始氧化, 进而导致Cu-Ag复合纳米粒子在340℃左右迅速氧化, 680℃左右Cu-Ag复合纳米粒子完全氧化。 温度低于220℃时, 气-液两相稳定法制备的Cu-Ag复合纳米粉的抗氧化能力比气相稳定法制备的Cu-Ag复合纳米粉的抗氧化能力好。      

液相还原法制备超细球形银粉的生长机理

以抗坏血酸为还原剂,硝酸银为反应前驱体,通过对液相体系分时间段取样研究液相还原法制备超细球形银粉的生长机理。借助扫描电子显微镜(SEM)、透射电子显微镜(TEM)、能谱(EDS)仪、X射线衍射(XRD)仪、紫外吸收光谱(UV-Vis)仪和颗粒图像分析仪对银粉进行表征和分析。结果表明,以抗坏血酸还原硝酸银制得了平均粒度为0.543μm,球形度为0.926,分散良好的超细球形银粉;该氧化还原反应可自发进行,使被还原的银原子达到过饱浓度形成银原子团簇和细小的银晶核,银晶核主要以原子扩散控制生长和晶核聚集两种方式长大,最终获得表面自由能较小、粒度分布均匀的球形银粉。     

还原氧化石墨烯-贵金属纳米复合物的制备及表征

以氧化石墨和氯铂酸为前驱体,在油胺中简便地合成了还原氧化石墨烯-铂(Reduced graphene oxide-platinum,rGOPt)纳米复合物,并对其进行了表征。透射电子显微镜和光谱测试结果表明,铂纳米颗粒均匀分布在石墨烯表面,尺寸约为30nm,铂纳米粒子为多孔隙结构,结晶性能良好,氧化石墨在高温下转变为还原氧化石墨烯。用此方法也可以制备还原氧化石墨烯-金(rGO-Au)或还原氧化石墨烯-银(rGO-Ag)的纳米复合物,金、银纳米颗粒呈球状,对可见光具有明显的表面等离子吸收。同时,油胺作为溶剂、贵金属盐的还原剂和表面活性剂,使制备过程简单、快捷。     

氧化钨厚膜气敏传感器的气氛改性研究

采用丝网印刷法将钨酸分解得到的氧化钨粉末制备成氧化钨厚膜气敏传感器,并先后在氢气和空气气氛中进行还原和氧化处理,系统研究了氢气浓度和氧化时的升温速率对敏感膜的形貌、结构和CO气敏性能的影响.结果表明,经氢气还原-空气氧化后,敏感膜表面形貌由近似球形的颗粒转化为表面光滑两端开口的集束棒状或规则的四方柱状,而晶体结构则没有发生改变.敏感膜对CO的灵敏度(Rair/RCO)随CO浓度的增加和测试温度的升高而增大.与没有进行气氛改性的敏感膜相比,经10%H2气氛还原并在600℃空气中以5℃/min氧化处理后的敏感膜对CO具有最大的灵敏度,其对3.8×10-5CO的灵敏度提高了13.3倍.即通过对敏感膜进行气氛改性可显著提高对CO的敏感性能.     

碳酸钴分解的热力学平衡分析和试验研究

为查清碳酸钴的热分解行为和性状遗传特性,对Co—C—O体系的稳定区和碳酸钴在不同气氛下的分解平衡进行了研究。通过热力学分析得到,在无氧状态下CoCO_3主要分解为CoO,分解反应是在温度高于200℃时进行;在有氧状态下CoCO_3极易发生氧化并分解生成Co_3O_4,在含氧体积分数为1%的氧气-氮气混合气氛中温度为930℃时Co_3O_4开始分解为CoO和O_2,且分解温度随着系统中氧浓度的增加而降低。CoCO_3的热分解试验证实了热力学分析结论,同时表明CoCO_3的热分解产物具有一定的性状遗传性,Co_3O_4的形态依赖于CoCO_3的原始形态,分解温度的升高会导致产物结块收缩,使CoO颗粒增大。     

Pt-TiO_2-还原氧化石墨烯纳米复合材料的制备及氧还原性能

制备一种具有高氧还原电催化活性的Pt-Ti O2-还原氧化石墨烯复合材料;采用X射线衍射、扫描电镜、透射电镜、高分辨透射电镜和拉曼光谱分析手段对催化剂的组成和微观结构进行表征。结果表明:氧化石墨烯在复合材料的合成过程中被还原为还原氧化石墨烯,纳米Pt与Ti O2颗粒均匀地附着在还原氧化石墨烯的片层上形成Pt-Ti O2-还原氧化石墨烯复合材料;该复合材料氧还原起始电位为-0.20 V左右,通过Koutecky-Levich方程计算得到电催化过程中复合材料的交换电流密度为10-6~10-5m A/cm2,16 000 s的计时电流测试后其相对电流值高达起始值的88%以上。     

Hydrogen bubble flotation of silica

In this study the flotation recovery of silica using air, and molecular and electrolytically-generated hydrogen was investigated. For comparison of air and molecular hydrogen recoveries, a laboratory Denver, type D12, flotation machine was used. For both gases, pH of the suspension, gas flow rate, concentration of collector and frother, solids concentration, particle size and speed of impeller were kept constant. Almost identical recoveries were obtained for both gases, suggesting that gas composition played no significant role in silica flotation. Electroflotation experiments were carried out using 12.6 μm mean diameter silica particles. While fine particles had very poor recovery in the Denver cell, greater than 70% recoveries were achieved in the electroflotation cell. This was thought to be the result of the very small (less than 40 μm) bubbles generated by the electroflotation process. A population-balance model, incorporating the hydrogen generation process, supported the conclusion that increased recovery for electroflotation, for very fine silica particles at least, was attributed to the reduced bubble size and not by the composition of the gas.     

碳包覆氧化亚钴纳米颗粒的制备与性能研究

采用直流电弧放电等离子体技术成功制备了碳包覆氧化亚钴纳米颗粒,并对样品的形貌、晶体结构、粒度、比表面积和孔结构采用高分辨透射电子显微镜(HRTEM)、X射线衍射(XRD)、X射线能量色散光谱(XEDS)、拉曼散射光谱(Raman)和N_2吸-脱附等测试手段进行了分析。HRTEM表明该方法制备的碳包覆氧化亚钴纳米颗粒具有典型的核壳结构,颗粒形貌主要为球形或椭球结构,粒度均匀,分散性良好,粒径分布在20~60nm,平均粒径为40nm,外壳碳层的厚度为5nm。XRD证明样品的内核为面心立方结构的氧化亚钴纳米颗粒,外壳为碳层。XEDS图谱表明样品中主要存在Co、O和C元素的特征峰。Raman光谱说明样品中碳外包覆层的石墨化程度较低,发生了红移现象。样品的N_2吸附-脱附等温曲线属Ⅳ型,BET比表面积为33m~2/g,BJH脱附累积总孔孔容和脱附平均孔径分别为0.078cm~3/g和11nm。当量粒径为43nm,与TEM和XRD测得的结果基本一致。     

Facile Synthesis of Co<Subscript>3</Subscript>O<Subscript>4</Subscript>/CoO Nanoparticles by Thermal Treatment of Ball-Milled Precursors

Co₃O₄/CoO nanoparticles have been synthesized by a simple method which is based on the ball-milling and calcination of cobalt acetate and citric acid. The samples were characterized using X-ray diffraction, transmission electron microscope, and Fourier transform infrared spectroscopy. The results show that Co₃O₄ nanoparticles with an average particle size of ∼40 nm can be obtained by calcination of ball-milled precursors at relatively low temperature (350 °C) for 3 hours. It should be noted that it is possible to control the size of Co₃O₄ particles by calcination temperature, calcination time and also by ball-milling duration using this method. Meanwhile, the pure CoO nanoparticles were obtained successfully by thermal decomposition of Co₃O₄ at 950 °C and quickly quenching to liquid nitrogen.     

Liquid-phase synthesis of cobalt oxide nanoparticles

Various liquid-phase syntheses of CoO and Co3O4 nanoparticles have been studied. The experiments focus on two synthesis routes: the coprecipitation and the sol-gel methods combined with thermal decomposition. The effect of synthesis route, the type of precursors (cobalt nitrate/chloride) and precipitation agent (carbonate, hydroxide, oxalic acid, and ammonia), the chemical compositions, pH, application of surfactants (PDMS, Triton X-100, NaDS, NaDBS, TTAB, ethyl acetate, citric acid), and the heat treatments on the properties of particles were investigated. The particle size and distribution have been determined by dynamic light scattering (DLS). The phases and the morphology of products have been analysed by XRD and SEM. The coprecipitation technique is less able to shape the particles than sol-gel technique. PDMS can be applied efficiently as surfactant in preparation methods. The finest particles (around 85 nm) with narrow polydispersity (70-100 nm) and spherical shape could be achieved by using sol-gel technique in medium of 1-propanol and ethyl acetate.     

Impact of binary gas on nano-aluminium particle formation through wire explosion process

The nano-aluminium particles were produced in different atmospheres by the wire explosion process. The size of the particles was measured using Transmission Electron Microscope (TEM) studies and particle size distribution analyses were carried out by adopting log-normal distribution. The nano-powders produced in different atmospheres were characterized through wide angle X-ray studies and energy dispersive analysis by X-rays (EDAX). It is realized that nano-aluminium particles produced in binary gas (argon–helium) atmosphere have lower particle size.     

Bayesian Inference Approach to Particle Size Distribution Estimation in Ferrofluids

We present an effective direct extraction method for particle size distribution based on Bayesian inference theory with a free-form model. We give an example of the application to the particle size distribution analysis in ferrofluid consisting of cobalt particles in toluene. The method gives a unique solution to the distribution without assuming the shape of the distribution of the particle size     

Preparation of cobalt nanoparticles by hydrogen reduction of cobalt chloride in the gas phase

Cobalt nanoparticles were produced by the hydrogen reduction of cobalt chloride vapor in a multistage tubular aerosol flow reactor. Reaction zone temperature, preheating temperature, mole fractions of CoCl₂ and H₂, and residence time were considered as key process variables for the control of particle size and size distribution. Ranging from 50 to 78 nm in average diameter, cobalt nanoparticles with narrow size distributions were synthesized throughout our experiments. All of the considered process variables affected the particle size and size distribution in the synthesis of cobalt nanoparticles. As the reaction zone temperature and the CoCl₂ mole fraction increased, the average particle diameter increased. But the average particle diameter decreased as the residence time of reactants increased.     

Synthesis and sintering of barium titanate fine powders by ultrasonic spray pyrolysis

Crystalline, spherical barium titanate fine powders with a narrow particle size distribution were prepared by ultrasonic spray pyrolysis. The stability of the starting solution was influenced by type of barium source and peptizer. The particle structure was influenced by the pyrolysis temperature of the barium source. The particle structure derived from barium acetate was dense, while powders derived from barium nitrate involved a lot of hollow particles. As-prepared powders were crystallized to a perovskite structure. Inductively coupled plasma analysis showed that the BaO/TiO₂ molar ratio of as-prepared powders was 50.5:49.5. The effects of the concentration of the starting fluid, pyrolysis temperature and flow rate of carrier air through the furnace on powder characteristics such as particle size, size distribution and crystal phase were investigated. The particle size depended on the concentration of starting solution and the flow rate of carrier air, but the particle size distribution was independent of these variables. Single-phase BaTiO₃ was obtained at more than 700°C. The relative density of barium titanate sintered at 1200°C was 98%. The hollow particles in the powders resulted in a low sintering density and a large grain size. The dielectric constant and tan δ of barium titanate at 25°C were 4500 and 0.02, respectively.     

Synthesis of cobalt nanoparticles to enhance magnetic permeability of metal–polymer composites

Metallic cobalt nanoparticles were synthesized by hydrogen reduction method. Particles were coated in situ with carbon by adding ethene to reaction flow. Particles were characterized by transmission electron microscopy, energy dispersive X-ray emission, X-ray diffraction, X-ray fluorescence and BET method. The observed cobalt particle size distributions in different cobalt batches produced with unvarying reaction parameters was reproducible: The mean diameter of primary cobalt particle varied only 5% from the mean value of 76 nm in different batches. Increased carbon precursor concentration decreased mean diameter of cobalt particles to 17 nm. The produced nanoparticles were used as filler material in 0–3 type metal–polymer composites. Composite samples with varying filler loading were fabricated with mixing extrusion and injection moulding techniques. The magnetic properties of the fabricated composites were measured up to 1 GHz. In order to analyse the particle distribution in composite matrix and its effect on magnetic properties the microstructure was studied.     

尖晶石型纳米钴蓝陶瓷颜料的制备

采用化学共沉淀法作为钴蓝颜料的制备方法,探讨了主要工艺因素对制备钴蓝颜料性能的影响,对制备的样品进行了测试与表征。结果表明:Co2+和Al3+物质的量比为1∶2.5时,制备的钴蓝样品颜色饱和度与明度最高,沉淀剂为尿素时制得的样品的粒度最小,粒度分布比较均匀。前驱体的洗涤过程采取水洗加醇洗的方法可有效减少样品的硬团聚现象,且前驱体的最佳煅烧温度为950℃左右。