Synthesis of CuO nanometer powder by one step solid state reaction at room temperature

Copper oxide nanometer powder wau synthesized by one step solid state reaction of CuCl₂ · 2H₂O with NaOH at room temperature. The solid product CuO was characterized by X-ray diffraction and a transmission electron microscope. It has been found that the particles of prepared copper oxide are spherical with average diameter of 20 nm. This new method has the advantages of convenience and high yield compared with literature methods.     

锂离子电池正极材料LiNi_(0.8)Co_(0.2)O_2的制备与表征

用2次干燥化学共沉淀法制得高密度前驱体Ni0.8Co0.2(OH)2,使之与LiOH.H2O混合经过2个恒温阶段烧结(600℃恒温6 h、850℃恒温24 h)得到LiNi0.8Co0.2O2材料,探讨了镍源、Li/(Ni+Co)摩尔比、合成温度、合成时间等因素对产品的影响,从而优化了LiNi0.8Co0.2O2的合成工艺.所得非球形LiNi0.8Co0.2O2粉末振实密度高达2.94 g/cm3,X射线衍射分析表明该材料具有规整的层状NaFeO2结构,充放电测试表明材料具有良好的电化学性能.     

Role of trivalent antimony in the removal of As, Sb, and Bi impurities from copper electrolytes

The role of trivalent antimony was investigated in removing As, Sb, and Bi impurities from a copper electrolyte. Purification experiments were carried out by adding a various concentrations of Sb(III) ions in a synthetic electrolyte containing 185 g/L sulfuric acid, 45 g/L Cu2+, 10 g/L As, and 0.5 g/L Bi under stirring at 65℃ for 2 h. The electrolyte was filtered, and the structure, morphology and composition of the precipitate were analyzed by means of chemical analysis, scanning electron microscopy (SEM), X-ray diffraction (XRD), transmission electron microscopy (TEM), and IR spectroscopy. The precipitate is composed of irregular lumps which are agglomerated by fine dendritic and floccus particles, and it mainly consists of As, Sb, Bi, and O elements. Characteristic bands in the IR spectra of the precipitate are As-OX (X=As, Sb, Bi), Sb-OY (Y=Sb, Bi), O-As-O, As-OH, Sb-OH, and O-H. The precipitate is a mixture of microcrystalline SbAsO₄, (Sb,As)₂O₃, and amorphous phases. As, Sb, and Bi impurities are effectively removed from the copper electrolyte by Sb(III) ions attributing to these precipitates.     

用非均相形核法制备Cu包裹MoSi2复合粉体

采用非均相形核法制备铜包裹MoSi2的复合粉体.利用场发射扫描电镜、X射线衍射仪、电子探针等分析手段对复合粉体进行表征,并讨论包裹结构的形成机制和影响因素.结果表明,采用非均相形核法可以制备出MoSi2颗粒表面被细小的铜微晶包裹的复合粉体;用壬基酚聚氧乙烯醚作为分散剂有助于提高纳米铜的稳定性,并能有效防止复合粉体的团聚,MoSi2颗粒的分散性得到显著改善,包裹效果较好;MoSi2颗粒大小和形状对复合粉体的包裹情况有较大影响;包裹结构取决于铜在MoSi2颗粒表面的沉积以及对复合粉体团聚的控制.     

Cu2O-templated fabrication of Ni(OH)2·0.75H2O hollow tubes for electrocatalytic oxygen evolution reaction

Cu₂O is an ideal template material for the preparation of transition metal hydroxide/oxyhydroxides with oxygen evolution reaction (OER) enhanced catalytic performance. Here, inspired by Pearson's principle, Cu₂O wires were prepared and used as a sacrificial template to prepare Ni(OH)₂·0.75H₂O hollow tubes (Ni(OH)₂ HTs) with highly improved surface roughness. Benefiting from unique structural advantages, the Ni(OH)₂ HTs showed excellent catalytic activity, rapid kinetics and a long-term stability as the OER catalyst, where an overpotential of only 207 ?mV was required to drive a current density of 10 ?mA ?cm^?2, an ideal kinetics with a Tafel slope as 79.8 ?mV dec^?1 was calculated, and no obvious attenuation in chronoamperometry was discovered after operation for 24 ?h. This paper provides a novel template-assisted strategy to prepare high-performance transition metal-based OER catalysts possessing hollow and tubular structures.     

Surface chemical structure of titania-silica nanocomposite powder

Titania-silica （TS） nanocomposite powder with three different composite structures, containing 10-30 mol% SiO2 in each structure, have been prepared by sol-gel processes. The surface characteristics of these titania-silica samples have been investigated by X-ray photo-emission spectroscopy （XPS） and high resolution transmission electron microscopy （HRTEM）. The study for all TS oxides annealed at 773 and 1173 K showed： an abnormal surface enrichment in Si increased with increasing annealing temperature; the Ti^3＋, Ti^2＋, Si^3＋ and Si^2＋ oxides coexisted with Ti^4＋ and Si^4＋ oxides, and the contents of these Ti/Si suboxides increased with increasing SiO2 content and annealing temperature; there was a layer rich in O on the topmost surface and the excess O could be attributed to the chem-adsorption of H2O; different composite structures could lead to different contents of Ti/Si suboxides. These results indicated that the surface of TS oxide powder derived by sol-gel process was a double layer with enriched O first and then SiOx/TiOy（x, y〈2）. Ti/Si suboxides could result from the thermal diffusion of Ti^4＋ and Si^4＋, which might be induced by the strong interaction between Ti^4＋ and Si^4＋.     

柠檬酸对Y2O2S：Eu^3＋，Mg^2＋，Ti^4＋发光性能的影响

研究了柠檬酸对高温固相法合成的Y2O2S：Eu^3＋,Mg^2＋,Ti^4＋红色长余辉材料性能的影响,结果表明添加一定量的柠檬酸有利于提高Y2O2S：Eu^3＋,Mg^2＋,Ti^4＋的发光性能,其初始亮度为1800mcd／m^2,余辉时间为8h．采用X射线衍射（XRD）、扫描电镜（SEM）、荧光光谱（PL）对样品进行了表征．     

纳米二氧化锡粉体的超重力-水热法制备与表征

以SnCl₄·5H₂O和氨水为原料,用超重力-水热法制备了纳米SnO₂粉体。利用X射线衍射(XRD)、透射电镜(TEM)、高分辨透射电镜(HRTEM)和物理吸附仪(BET)等分析手段对其进行表征。考察了反应物浓度、反应温度和陈化时间等实验条件对纳米SnO₂粉体的晶体结构、粒度及分散性的影响。结果表明,在SnO₂溶液浓度为0.05mol/L、水热温度240～280℃以及陈化时间3～8h得到的粉体结晶性良好、比表面积大(90～170m²/g)、粉体的颗粒大小在2～6nm左右,并具有良好的分散性。     

Nitridation of chromium powder in ammonia atmosphere

CrN powder was synthesized by nitriding Cr metal in ammonia gas flow, and its chemical reaction mechanism and nitridation process were studied. Through thermodynamic calculations, the Cr-N-O predominance diagrams were constructed for different temperatures. Chromium nitride formed at 7002-1200℃ under relatively higher nitrogen and lower oxygen partial pressures. Phases in the products were then investigated using X-ray diffraction (XRD), and the Cr₂N content varied with reaction temperature and holding time. The results indicate that the Cr metal powder nitridation process can be explained by a diffusion model. Further, Cr₂N formed as an intermediate product because of an incomplete reaction, which was observed by high-resolution transmission electron microscopy (HRTEM). After nitriding at 1000℃ for 20 h, CrN powder with an average grain size of 63 nm was obtained, and the obtained sample was analyzed by using a scanning electron microscope (SEM).     

Microstructural characterization of as-cast and homogenized 2D70 aluminum alloy

The microstructure of the as-cast 2D70 aluminum alloy and its evolution during homogenization were investigated by means of optical microscopy (OM), scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS), X-ray diffraction (XRD), and differential scanning calorimetry (DSC) analysis. The results indicate that the microstructure of the as-cast 2D70 aluminum alloy mainly consists of the dendritic network of aluminum solid solution and intermetallic compounds (Al₂CuMg, Al₂Cu, Al₉FeNi, Cu₂FeAl₇, and Al₇Cu₄Ni). After conventional homogenization, Al/Al₂CuMg eutectic phases are dissolved into the matrix, and a small amount of high melting-point eutectic Al/Al₂Cu phases exist in the matrix, resulting in an increase in the starting melting temperature. Under double homogenization, the high melting point Al/Al₂Cu phases are dissolved, and no obvious change is observed for the size and morphology of Al₉FeNi, Cu₂FeAl₇, and Al₇CuaNi compounds.     

Synthesis,structure and mechanical properties of Zr-Cu-based bulk metallic glass composites

The unusual glass-forming ability (GFA) of the Zr₄₈Cu₃₆Ag₈Al₈ alloy and the high ductility of the Zr₄₈Cu₃₆Ag₈Al₈ metallic glass-matrix composites containing Ta powder were reported. The bulk metallic glass rod with a diameter of 25 mm was successfully synthesized using copper mold casting for the Zr₄₈Cu₃₆Ag₈Al₈ alloy. High GFA of this alloy was found to be related to a large supercooled liquid region and a quaternary eutectic point with low melting temperature. The bulk metallic glass matrix composites were prepared by introducing extra Ta particles into the Zr₄₈Cu₃₆Ag₈Al₈ melt. The composites consist of Ta particles homogenously distributed in the Zr₄₈Cu₃₆Al₈Ag₈ metallic glass matrix. The optimum content of Ta powder is 10at% for the composite with the highest plasticity, which shows a plastic strain of 31%.     

水热条件下反应介质对Mg(OH)2晶体晶形的影响

以氯化镁和氨水为原料,在室温下制得Mg(OH)2,在不同的反应介质中对Mg(OH)2进行水热处理,制备出了超细、高纯的Mg(OH)2颗粒,利用X射线衍射仪(XRD)和扫描电子显微镜(SEM)对所制得Mg(OH)2颗粒的晶相、形貌和颗粒尺寸进行了表征.研究结果表明,水热条件下反应介质对Mg(OH)2晶体的形成有十分显著的影响,NaOH溶液、乙二胺和乙醇溶液能够显著改善Mg(OH)2晶体的晶形和分散性.初步探讨了水热条件下反应介质对Mg(OH)2晶形的影响机制.     

Facile synthesis of monodispersed copper oxalate flaky particles in the presence of EDTA

Monodispersed copper oxalate particles with flaky morphology were prepared via a simple one-pot synthesis method. Scanning electron microscope (SEM), X-ray diffraction (XRD), and fourier transform infrared (FTIR) spectra were used to characterize particle morphology, size, phase composition, and functional groups. It was found that the presence of ethylenediaminetetraacetic acid (EDTA) and the solution pH value had strong influence on the morphological and size evolution of the precipitated particles. On the basis of controlled release of copper ions from a Cu2+–EDTA complex and Weimarn’s law, a strategy for the controlled synthesis of monodispersed copper oxalate particles was designed by referring to the basic mode of the Stöber method. The inherent nature of crystallization to form the flaky solid in the early stage of precipitation as well as the driving force of the long-lasting low supersaturation in the growth stage was proposed to explain the size and morphological evolution of the copper oxalate precipitates. Thermodynamic equilibrium concentrations of copper(Ⅱ) species in the Cu(Ⅱ)–EDTA–oxalate–H₂O solution system were calculated to help explain the possible formation mechanism of copper oxalate precipitates.     

Formation of highly crystalline maghemite nanoparticles from ferrihydrite in the liquid phase

Fe₅O₇(OH)·4H₂O ferrihydrite is a low-crystallinity antiferromagnetic material. γ-Fe₂O₃ (maghemite) magnetic nanoparticles were prepared from a ferrihydrite precursor, by chemically induced transformation in FeCl₂/NaOH solution. The magnetization, morphology, crystal structure and chemical composition of the products were determined by vibrating sample magnetometry, transmission electron microscopy, X-ray diffraction (XRD), energy-dispersive X-ray spectroscopy and X-ray photoelectron spectroscopy (XPS). Ferrihydrite underwent aggregation growth and transformed into α-FeO(OH) (goethite) particles, which subsequently transformed into γ-Fe₂O₃ nanoparticles, that became coated with NaCl. The γ-Fe₂O₃ particles had a flake-like morphology, when prepared from 0.01 mol/L FeCl₂ and a FeCl₂:NaOH molar ratio of 0.4. The γ-Fe₂O₃ particles were more spherical, when prepared from a FeCl₂:NaOH molar ratio of 0.6. The Fe content of the flake-like particles was lower than that of the spherical particles. Their magnetizations were similar, and the coercivity of the flake-like particles was larger. The differences in morphology and magnetization were attributed to the surface effect, and the difference in coercivity to the shape effect.     

Preparation and radar-absorbing properties of Al<Subscript>2</Subscript>O<Subscript>3</Subscript>/TiO<Subscript>2</Subscript>/Fe<Subscript>2</Subscript>O<Subscript>3</Subscript>/Yb<Subscript>2</Subscript>O<Subscript>3</Subscript> composite powder

Al₂O₃/TiO₂/Fe₂O₃/Yb₂O₃ composite powder was synthesized via the sol-gel method. The structure, morphology, and radar-absorption properties of the composite powder were characterized by transmission electron microscopy, X-ray diffraction analysis and RF impedance analysis. The results show that two types of particles exist in the composite powder. One is irregular flakes (100-200 nm) and the other is spherical Al₂O₃ particles (smaller than 80 nm). Electromagnetic wave attenuation is mostly achieved by dielectric loss. The maximum value of the dissipation factor reaches 0.76 (at 15.68 GHz) in the frequency range of 2-18 GHz. The electromagnetic absorption of waves covers 2-18 GHz with the matching thicknesses of 1.5-4.5 mm. The absorption peak shifts to the lower-frequency area with increasing matching thickness. The effective absorption band covers the frequency range of 2.16-9.76 GHz, and the maximum absorption peak reaches -20.18 dB with a matching thickness of 3.5 mm at a frequency of 3.52 GHz.     

Sintering mechanism of Cu-9Al alloy prepared from elemental powders

The sintering behavior of Cu-9Al alloys prepared from die pressing of elemental powders was investigated. The experimental results and kinetic analysis showed the formation of three consecutive layers of Al₂Cu, Al₄Cu₉, and AlCu phases, with Al₂Cu appearing first in the initial solid phase sintering stage. A liquid phase formed in the intermediate stage, resulting from the eutectic reaction between Al and Al₂Cu phases at 500 °C, which is 47 °C lower than the equilibrium reaction temperature. Swelling occurred when the liquid phase infiltrated the gaps between the copper particles, leaving pores at the original sites of Al particles and Al₂Cu. In the final stage of sintering, the Al-rich phases (Al₂Cu and AlCu) transformed to Al-poor phases (Al₄Cu₉ and α-Cu) in the temperature range of 500–565 °C. Al₄Cu₉ and α-Cu then transformed to AlCu₃ (β) above the eutectoid reaction temperature (565 °C), whereas AlCu₃ transformed to α-Cu and eutectoid phases (α-Cu + Al₄Cu₉) during cooling. The pure copper transformed to AlCu₃, and the pore volume decreased at 1000 °C. The microstructure study helps manipulate precisely the sintering process of Cu-Al alloys and optimize the microstructure with a high dimensional accuracy.     

高浓度氯化钙水热环境下氢氧化镁颗粒生长行为研究

以石灰乳-卤水法制备的氢氧化镁为原料,对不同水热环境下高浓度氯化钙对氢氧化镁颗粒形貌的影响进行了研究。通过扫描电镜(SEM)、X射线衍射仪和氮气吸附比表面积分析仪(BET)对产物的比表面积和形貌进行表征。结果表明,较高的温度和高浓度氯化钙的存在有利于晶体的发育生长,其产物的分散性较好,粒径均匀并呈六方片状晶体,比表面积由22.17 m2/g变为14.84 m2/g。对水热条件下氯化钙对晶体生长的作用进行了机理分析,CaCl2的存在使得氢氧化镁基元在晶体表面横向叠加,促进了六方片状氢氧化镁颗粒的生成,并提出氢氧化镁颗粒的最稳定晶型为六方片状。     

Al2O3-SiC纳米复合陶瓷的制备及其表征

以分析纯Al(NO₃)₃·9H₂O, (CH₂)₆N₄和粒径为30 nm的SiC粉末为原料, 采用溶胶-凝胶(sol-gel)方法制备干凝胶, 经煅烧合成Al₂O₃-SiC纳米陶瓷粉, 利用真空热压装置对粉末进行烧结. 通过X射线衍射(XRD)、 扫描电镜(SEM)和维氏硬度实验分析了不同SiC含量和不同烧结温度的Al₂O₃-SiC陶瓷样品的结构、 形貌、 晶粒尺寸和硬度, 并研究了其机理.     

Effects of gadolinium addition on the microstructure and mechanical properties of Mg-9Al alloy

This research aims to study the significance of Gd addition (0wt%-2wt%) on the microstructure and mechanical properties of Mg-9Al alloy. The effect of Gd addition on the microstructure was investigated via X-ray diffraction (XRD), optical microscopy, scanning electron microscopy (SEM), and transmission electron microscopy (TEM). The Mg-9Al alloy contained two phases, α-Mg and β-Mg17Al12. Alloying with Gd led to the emergence of a new rectangular-shaped phase, Al₂Gd. The grain size also decreased marginally upon Gd addition. The ultimate tensile strength and microhardness of Mg-9Al alloy increased by 23% and 19%, respectively, upon 1.5wt% Gd addition. We observed that, although Mg-9Al-2.0Gd alloy exhibited the smallest grain size (181 μm) and the highest dislocation density (5.1×1010 m-2) among the investigated compositions, the Mg-9Al-1.5Gd alloy displayed the best mechanical properties. This anomalous behavior was observed because the Al₂Gd phase was uniformly distributed and present in abundance in Mg-9Al-1.5Gd alloy, whereas it was coarsened and asymmetrically conglomerated in Mg-9Al-2.0Gd.     

A magic eggshell: Cu<Superscript>2+</Superscript> reacts with S<Superscript>2−</Superscript> to produce metal Cu,rather than CuS

In common sense, the chemical reaction between Cu²⁺ and S^2– ions produces black precipitation of CuS. However, if they are separated by an eggshell, they produce copper with trace amount of CuS on the surface of the eggshell at the side of copper chloride solution within one week. Such an unexpected phenomenon strongly indicated that Cu²⁺ is able to be reduced into metal copper when S^2– diffuses throughout the porous eggshell. The produced copper was verified by reacting with nitric acid to generate red-brown nitrogen dioxide at ambient temperature, as well as by the powder X-ray diffraction (XRD) and energy dispersive analysis of X-rays (EDS).