机械热化学法制备纳米W-Cu复合粉末及其烧结性能研究

WO3和CuO原料粉末经气流粉碎后,在H2气氛中进行共还原,制得了Cu含量为20%(wt%)的纳米W-Cu复合粉末;通过X射线衍射,透射电镜和扫描电镜等方法研究分析所制备W-Cu粉末的烧结行为和烧结体性能.结果表明:气流粉碎可以明显地降低WO3和CuO的粒度;通过对气流粉碎氧化物粉末进行共还原,可获得粒度为50～100nm的W-Cu复合粉末.该粉末烧结活性较高,其成形压坯在1200℃下于H2气氛中烧结后相对密度可达98%以上,且烧结体晶粒细小均匀.其抗弯强度和维氏硬度分别超过1000MPa和300MPa,电导率高于35%IACS.     

碳热还原法制备纳米碳化铬粉末及其特性表征

以纳米Cr2O3和纳米碳黑为原料,采用碳热还原法制备纳米碳化铬(Cr3C2)粉末。采用XRD、SEM和TEM等测试手段对反应产物进行表征。结果表明:当碳含量为28%(质量分数)、反应温度为1 100℃及保温时间为1 h时,反应产物为单一的Cr3C2,平均晶粒尺寸为25.6 nm;反应产物分散较好且颗粒呈球形或类球形,无明显团聚现象,颗粒尺寸在30 nm左右;试样表面主要由Cr、C和O这3种元素组成,O 1s谱主要包括3个峰(Oa,Oh和Od),分别对应于O、OH和Cr2O3;C 1s谱主要包含4个峰(Cf,Cc,Cd和Ce),分别对应污染碳、碳化铬(Cr3C2)及其他类型的碳化铬Cr3C2 x(0≤x≤0.5)。     

钨铜复合材料研究现状与展望

钨铜复合材料具有高导电导热性能、低膨胀系数、良好的高温强度和抗电弧烧蚀性能,在电气工程、机械加工及电子信息等领域获得了广泛应用。介绍了钨铜复合材料的传统工艺及制备新技术,综述了其在电器开关、电极、微电子及军工等领域的应用,并对其制备技术和应用开发进行了展望。     

纳米W-Cu粉末的热机械化学法制备及其烧结性能研究

通过均相沉淀获得Cu2WO4(OH)2/CuWO4·2H2O共沉淀物,并对煅烧该沉淀物所得的W、Cu氧化物进行球磨,然后H2还原,得到了含Cu量为30%的W-Cu复合粉末。对该复合粉末的性能进行了表征,并对其烧结体的密度、微结构和力学性能等进行了测试分析。结果表明,热机械化学法制备的W-Cu复合粉末粒度为纳米级,烧结活性高,其压坯在H2气氛中固相烧结可达到96%的相对密度,液相烧结则可达到高于99%的相对密度,烧结体具有细小均匀的微结构和良好的力学性能。     

纳米W-Cu粉末的均相沉淀法制备及其烧结性能

采用湿化学工艺--蒸氨均相沉淀法,制备了纳米CuWO4·2H2O/Cu2WO4(OH)2均相沉淀物,然后煅烧、还原,得到含Cu 30%的W-Cu复合粉.将该复合粉压坯在H2气氛中于不同温度下烧结后,对烧结体的微结构和物理、力学性能等进行了测试分析.实验结果表明:蒸氨均相沉淀法制备的W-Cu复合粉体具有纳米粒度和均匀的化学组成,其烧结活性高,在较低温度下烧结即可达很高的致密化程度.由上述W-Cu粉体所制备的烧结体具有良好的物理、力学性能.     

Preparation of microsized silver crystals with different morphologies by a wet-chemical method

A wet-chemical method was presented for preparation of spherical, flowerlike, hexagonal, and triangular microsized silver crystals. Well-defined particles were prepared by mixing of iron(II) sulfate heptahydrate solution with silver nitrate solution at the presence of different modifiers with high-speed stirring at 8–20°C. It is found that the diameters of resulting products are 0.6–6.0 μm and the morphologies of the silver microcrystals are greatly affected by the introduced modifiers. It is concluded that the microsized silver crystals with different morphologies can be synthesized by introducing appropriate modifiers at appropriate experimental parameters. Scanning electron microscopy and X-ray diffraction were used to characterize the resulting products.     

Structure and Properties of W-Cu/AlN Composites Prepared via a Hot Press-Sintering Method

采用高能球磨技术制备W-30%Cu（质量分数）纳米晶粉体,再通过球磨混粉的方法添加不同质量分数的纳米AlN颗粒,然后采用热压烧结法得到W-30Cu/x%AlN复合材料。研究并比较了纳米AIN的加入对材料组织结构、物理以及力学性能的影响。结果表明,W-30Cu/x%AlN复合材料都有较致密和均匀的组织结构,AlN的添加,细化了烧结体中W颗粒;纳米AlN颗粒的添加提高了复合材料的硬度,但是随着A1N纳米颗粒含量的增加,基体晶界上的增强相颗粒分布过多,而使材料的抗弯强度有所下降;少量纳米AlN颗粒(≤1%)的添加有利于W-Cu复合材料的热导率提高,随AIN添加量的增加,复合材料的电阻率升高,电导率下降。     

Effect of vanadium on synthesis of WC nanopowders by thermal processing of V-doped tungsten precursor

The effect of vanadium on the synthesis of WC nanopowders by carbon thermal processing of V-doped tungsten precursor has been discussed. The V-doped tungsten precursor was prepared by a wet chemical method with ammonium tungstate and ammonium vanadate as its starting materials. The precursor was carbonized in the vacuum furnace using phenol formaldehyde resin as a carbon agent. The results of XRD revealed that the tungsten oxide and vanadium oxide obtained from the precursor preparation formed V–O–W bronze with the structure of WO₃ · 0.33H₂O. The carbonization reactions of WO₃ with 1 wt% of vanadium took place in a temperature range from 900 to 1050 °C to obtain V-doped WC nanopowder. The results of particle size measurement and morphological analysis show that the vanadium effectively inhibits the particle growth of tungsten carbide powder during carbonization processes, resulting in the particle size to be within the range from 64 to 184 nm after heat treatment in the temperature range from 900 to 1200 °C. V₂O₃ particles decomposed from V–O–W bronze can act as a nucleation aid for tungsten during reduction, and those on the surface of tungsten powder can hinter the growth of tungsten carbide crystal by the pinning effect.     

Features of passivation, oxidation and combustion of tungsten nanopowders by air

The passivation, oxidation and combustion of tungsten nanopowders (NP) (a_s  100 nm), produced by an electrical explosion of wires (WEE) method, has been studied in air medium. The phase transformation for W nanopowders under air-oxidation was investigated. The oxidation process and an analysis of passivated powders were studied by FESEM, EDS, XPS, XRD, TEM, DTA-TGA and size distribution analysis was also observed by a video camera. After the comprehensive testing of passivated, oxidized and burned powders, a chemical process of oxidation of W nanoparticles was suggested.     

高压扭转制备钨铜梯度材料的仿真和实验研究

采用ABAQUS软件对钨铜材料高压扭转变形进行有限元模拟,分析了扭转变形过程中的应力场分布和应变累积状态,以及压力和温度对界面层应变累积的影响。模拟结果表明,铜在HPT变形过程中为剪切变形的主要承受方,钨未得到充分的剪切变形,界面层应变累积最大;较高的温度和压力有利于界面层的应变累积,但温度的提升效果并不显著,并且高压力和高温度易导致铜反挤和模具失效。在300 ℃、1 GPa、扭转5圈的工艺条件下采用高压扭转工艺制备了界面连接质量良好的钨铜梯度材料。实验结果表明,随着扭转半径的增大,钨和铜的组织均得到显著细化,平均晶粒尺寸分别约为32.6 μm和0.28 μm,并且在界面处出现晶粒尺寸约为4.8 μm的铜组织过渡层;界面处钨和铜结合良好,钨和铜元素的扩散距离分别约为1.74 μm和2.59 μm。铜的显微硬度由初始态的79 Hv提升至131 Hv,界面处钨的显微硬度由初始的347 Hv提高到424 Hv,表明大变形条件下的晶粒细化和缺陷累积有利于界面连接和性能提升。     

化学共沉淀-封闭循环氢还原法制备纳米W-Cu复合粉

以H2WO4和CuSO4·H2O(W:Cu=70g:30g)为原料,采用化学共沉淀方法制备W-Cu化合物粉末,其反应条件为:反应温度25℃±1℃,pH值5.0-5.2,陈化时间8h±1h。设计了封闭循环氢还原系统,用此系统进行氢气热还原,不仅使氢气得到充分利用,而且容易判断反应终点。通过系统内的特殊装置除水,降低了还原温度,在600℃下还原得到W和Cu混合均匀的复合粉。其粒径小于70nm。     

Preparation of micro-sized and uniform spherical Ag powders by novel wet-chemical method

A novel wet-chemical method was presented for the preparation of the micro-sized and uniform spherical Ag powders on a mass-production scale. The well-defined particles were synthesized by mixing the iron(II) sulfate heptahydrate solution with silver nitrate solution directly by high-speed stirring at room temperature. It is found that a large number of micro-sized and uniform spherical particles with rough surfaces are obtained. The mass ratio of iron(II) sulfate heptahydrate to silver nitrate greatly affects the shape of particles, and when it is relatively low, spherical particles cannot be obtained. The reaction temperature has a great impact on the particle size. As the reaction temperature increases from 8 to 15 °C, the mean diameter of particles decreases from 3.5 to 1.6 (m. The additive n-methyl-2-pyrrolidone improves the surface smoothness and compactness of the particles while the particle size is kept unchanged. Scanning electron microscopy, X-ray diffractometry and energy dispersive X-ray analysis were used to characterize the particle products.     

NaBH_4的水性还原法制备纳米铜颗粒(英文)

在碱性溶液中用NaBH4还原Cu2+制备纳米铜颗粒,研究NaBH4浓度和滴加速率对Cu纳米颗粒制备的影响。反应的最佳条件是:0.2mol/LCu2+,溶液pH12,温度313K,1%明胶作为分散剂,将0.4mol/LNaBH4溶液以50mL/min的速率加入CuSO4溶液中。氨水是最佳的络合剂。采用一系列实验研究不同时间点的反应进程。     

超重力燃烧熔渗钨铜合金绝热温度计算及其显微组织

根据燃烧合成体系绝热温度的热力学基本理论,通过计算机编程,对CuO/Al铝热剂体系的绝热温度进行了数值计算.结果表明,在考虑产物Cu的汽化焓情况下,体系绝热温度为2846 K(Cu的沸点温度),同时还有52.9 at％的Cu产物以气相形式存在,而该体系中钨粉添加量超过30 mass％时,绝热温度低于1800 K而不能自蔓延燃烧.采用超重力燃烧熔渗方法制备出组织致密,钨颗粒体积分数呈梯度分布(沿超重力方向70％～80 at％)的钨铜合金.进一步检测结果表明,该方法与传统烧结方法制备的钨铜合金其相结构及显微组织形貌相同,并对其成型机制进行了初步分析讨论.     

Synthesis of VN nanopowders by thermal nitridation of the precursor and their characterization

Vanadium nitride (VN) nanopowders can be synthesized by thermal nitridation of the precursor of ammonium vanadate (NH₄VO₃) and nanometer carbon black. The products were characterized by X-ray diffractometry (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and X-ray photoelectron spectroscopy (XPS) techniques. The results show that the single phase VN powders can be synthesized at 1100 °C for 1 h, and the powders show good dispersion and are mainly composed of uniformly sized spherical particles with a mean diameter of 50 nm. The surface of the specimen mainly consists of V, N, O and C four species elements, the peak core at 397.24 eV corresponds to N 1s of VN. The O 1s peaks with the binding energies of 530.40 eV and 532.15 eV are ascribed to vanadium pentoxide (V⁵⁺) and H₂O (OH⁻), and the contents are very little. The C 1s profile is a single symmetric peak, which mainly comes from the polluted carbon used for the correction of the XPS measurement.     

通过水溶液还原法用抗坏血酸制备纳米铜颗粒(英文)

通过水溶液还原法用抗坏血酸还原Cu2+制备纳米铜颗粒,并研究溶液pH和Cu2O平均粒径对纳米铜颗粒制备的影响。在溶液pH值为3、5和7时,可制得铜颗粒,并且在pH=7时制得的铜颗粒粒径最小。在溶液pH为9和11时无法制得铜颗粒。Cu2O的平均粒径能影响铜粉的粒径。Cu2O的平均粒径越大,得到的铜颗粒越大。通过对反应过程中不同时间点收集的样品进行XRD分析,可探索出反应的进程。在反应过程中,Cu(OH)2首先作为前驱体出现,然后被还原为Cu2O,最后被还原为铜颗粒。     

碳热还原结合熔盐法制备碳化钛粉末与表征

以NaCl为熔盐介质,采用锐钛矿型钛白粉和炭黑为原料,探索一种碳热还原结合熔盐法合成高纯碳化钛(TiC)的方法。借助XRD研究了反应温度和原料配比对合成碳化钛的影响,采用SEM、TEM、EDS、粒度分析仪、热力学分析等检测分析手段对合成产物的特性和过程进行分析。结果表明:相比传统的碳热还原合成碳化钛的方法,NaCl熔盐介质的引入可以有效地降低碳化钛的合成温度(从1700℃到1550℃)以及合成高纯碳化钛的时间(从10 h到3 h)。结合研究成果,提出了熔盐介质中溶解-沉淀的合成机理。     

一种新颖、简单的银微米线的湿化学制备方法(英文)

提供一种新颖简单的银微米线的湿化学制备方法。在反应温度为50℃的条件下,把硫酸亚铁溶液逐渐滴加到含有柠檬酸的硝酸银溶液中,合成银微晶体。采用扫描电镜(SEM)和X射线衍射仪(XRD)对所制备的银微晶体进行表征。结果表明:所制备的银微晶体主要由大量的银微米线组成;银微晶体的形态与反应温度有很强的联系;当硝酸银浓度降低时,银微米线的长度和直径都逐渐增大,且较低的硝酸银浓度不利于生成更多的银微米线。降低硫酸亚铁浓度时也出现类似的结果。柠檬酸的用量对银微晶体的微观形态有很大的影响。根据银微米线的形成机理,推断柠檬酸在Oswald熟化形成银微米线的过程中起着非常重要的作用。     

Synthesis of nanocrystalline molybdenum by hydrogen reduction of mechanically activated MoO3

Nanocrystalline molybdenum with a mean crystallite size of 50 nm was synthesized by mechanical activation of MoO₃ powder and its subsequent hydrogen reduction. MoO₃ powder was severely activated in a high energy planetary ball mill under a pure argon atmosphere. Temperature-programmed reduction (TPR) by hydrogen was used to investigate hydrogen reduction behavior of the powder samples activated for 5 and 20 h. It was found that by increasing the activation time, the peak temperature for the reduction was shifted slightly to lower temperatures and the peak for the reduction of MoO₃ to MoO₂ was completely separated from the one for the reduction of MoO₂ to molybdenum. In order to evaluate the effect of mechanical activation on the reduction behavior of MoO₃, the initial micron-sized powder and the sample activated for 20 h were reduced at similar conditions. It was found that the activated sample with finer particles was reduced faster than the un-milled sample. Hydrogen reduction of the non-activated MoO₃ produced a very fine grained molybdenum powder but the crystallite size changes of the sample activated for 20 h was negligible during reduction.