草酸镍钴固溶体的制备与鉴别

以可溶性氯化镍、氯化钴和草酸或草酸铵为原料,氨水为pH值调节剂,采用液相共沉淀法合成草酸镍钴共沉淀产物,借助X射线衍射(XRD)、热重-差热分析(TG-DTA)和扫描电镜(SEM)对共沉淀产物进行表征,并将结果与机械混合物进行比较.结果表明:在共沉淀过程中,当溶液pH≤5.0时,钴离子易进入草酸镍晶格中形成置换固溶体,得到的共沉淀产物为草酸镍钴单相固溶体,其热分解行为明显不同于具有相同配比的机械混合物;当pH＞5.0时,镍离子和钴离子与草酸根离子的共沉淀过程为分步沉淀,得到的共沉淀产物为组分分布均匀的复杂混合物,而非单相固溶体.     

纤维状复杂钴盐的制备

以氨水、草酸和氯化钴为原料, 通过配位沉淀制备得到了纤维钴粉前驱体--纤维状复杂钴盐粉末。通过XRD分析、化学成分分析和电位-pH图可以得知该复杂钴盐分子式为[Co(NH₃)_x]C₂O₄·yH₂O (x=1.2…6)。初始Co²⁺浓度、反应时间和温度等因素都能够影响纤维状复杂钴盐的形成。通过电镜图片分析了这些因素对前驱体形貌的影响行为。     

配位沉淀-直接还原法制备球形超细镍粉

以碳酸氢铵为沉淀剂、氯化镍为原料、氨为配位剂, 用配位沉淀法制备球形镍粉前驱体沉淀, 再于氢还原气氛中直接还原前驱体制备球形超细镍粉。系统地研究了前驱体制备过程中反应物浓度、pH值、添加剂、温度和直接还原过程中反应温度、还原气氛对镍粉形貌及粒度的影响。实验结果表明: 在Ni²⁺浓度为0.8 mol/L, pH值为7.5, 反应温度为室温, 添加剂PVP添加量为1%的条件下可制备出类球形、形状较规则、分散性好的镍粉前驱体; 将球形的、分散性好的前驱体粉末在350～400 ℃的N₂和H₂混合气氛中进行还原即可得到分散性好、纯度高的超细金属镍粉。     

形貌控制合成纤维状氧化亚镍粉末新型前驱体

以可溶性镍盐和草酸或草酸铵为原料, 利用氨为配位剂, 通过配位沉淀法制备了纤维状氧化亚镍粉新型前驱体, 并采用XRD、红外光谱(IR)和扫描电镜(SEM) 研究了前驱体粉末的物相、成分与形貌, 系统考察配位沉淀条件包括溶液pH值、反应温度、反应物浓度和表面活性剂对前驱体粉末形貌、粒度和成分的影响。结果表明: Ni(Ⅱ)-C₂O4^2--NH₃-NH₄⁺-H₂O反应体系中, 在溶液pH值为8.2～8.8, 温度为60～70 ℃, Ni²⁺浓度为0.5～0.8 mol/L, 表面活性剂聚乙烯吡咯烷酮(PVP)用量为0.1%～0.5%条件下得到的新型前驱体为草酸镍氨复盐, 其形貌为纤维状; 氨与镍离子配合并生成草酸镍氨复盐是纤维状形貌形成的内在机制。通过在空气中热分解该种前驱体即可得到比表面积为5.944 m²/g、轴径比大于50的纤维状氧化亚镍粉末。     

超细钴粉制备的研究进展

本文综述了国内外制备超细钴粉的一些方法,并对我国这方面的研究和开发工作提出了建议。     

Thermodynamic equilibrium calculation on preparation of copper oxalate precursor powder

According to the principles of simultaneous equilibrium and mass balance, a series of thermodynamic equilibrium equations of Cu^2＋-C2O4^2--NH3-NH4^＋＋-H2O system at ambient temperature were deduced theoretically and the logarithm concentration versus pH value （lg[Cu^2＋]T--pH） diagrams at different solution compositions were drawn. The results show that when pH is below 5.0, copper ion reacts with C2O4^2- directly and the morphology of copper precursor powder is of pie-shape, when pH is above 5.0, copper ion coordinates with ammonia, and the precipitation proceeds slowly accompanying with the release of copper ions fi＇om the multi-coordinated Cu（NH3）n^2＋（n =1, 2,…, 5） and the morphologies of copper precursor powder are respectively of rod aggregation shape （when 5.0〈pH〈8.0） and of rod-shape （when pH〉8.0）. Some experiments were performed to confirm the relation between the total concentration of copper ion and pH value. It is shown that the thermodynamic mathematical model is correct and the calculated values are basically accurate.     

配位共沉淀-直接还原法制备超细纤维状铁镍合金粉(英文)

采用配位共沉淀制备了铁镍合金前驱体,用氢气直接还原前驱体得到了超细纤维状铁镍合金粉。系统研究了反应物浓度、pH值、反应温度及添加剂等参数对前驱体制备过程的影响。分别采用XRD、TG-DTA和SEM对前驱体的结构、热分解过程和形貌进行了表征。结果表明,采用质量分数2%的PVP作为添加剂,当Fe2+和Ni2+(1:1)总浓度为0.8mol/L,pH值为6.2,反应温度为60°C时,可以制得分散良好、形貌均匀的纤维状前驱体。前驱体在420°C的氮气和氢气混合气氛下直接还原可以得到纯度高、分散性好的纤维状铁镍合金粉。     

Fe2+-Ni2+-NH3-NH4+-C2O42-H2O体系的沉淀配合平衡热力学

针对草酸盐配位共沉淀热分解还原法制备超细铁镍合金粉过程中Fe2+-Ni2+-NH3-NH4+-C2O42--H2O体系的溶液平衡建立热力学分析模型,并根据模型进行相关计算,揭示反应体系中各物质随pH值、氨及草酸浓度的变化关系。结果表明:溶液中的Fe主要以[Fe(C2O4)n]2 2n络合物形式存在,而铁氨络合物含量很低。当氨含量较低时,溶液中的Ni主要以[Ni(C2O4)n]2 2n存在;氨含量较高时,在酸性条件下,溶液中的Ni主要以[Ni(C2O4)n]2 2n存在,在碱性条件下,则主要以[Ni(NH3)n]2+存在。低pH值下,Ni的沉淀率较Fe的高,而高pH值下,Ni的沉淀率则较Fe的低。     

纳米CoO粉的制备方法及其应用

综述了制备纳米CoO粉的各种方法,介绍了其在电池、催化剂、电子电器元件等方面的用途。同时,针对目前国内外的研究现状,为今后的研究和开发工作提出了几条建议。     

Composition and morphology of complicated copper oxalate powder

In Cu(Ⅱ)-C2O42--NH3-NH4+-H2O system, complicated copper oxalate powders were synthesized by coordination-precipitation process with ammonium oxalate as precipitating agent. The composition and morphology of the powders were characterized by chemical analysis, X-ray diffraction (XRD), scanning electron microscopy (SEM), infrared spectroscopy (IR), and thermogravimetric and differential thermal analysis (TGA-DTA). The effects of temperature, copper ion concentration and pH value were investigated. The experimental results show that pure copper oxalate hydrate is prepared below a critical pH value of 6.0, whereas the powder turns to be a complicated copper salt combined with NH3 over the pH value. Probable chemical formula, CuC2O4·x(NH3) ·yH2O can be assumed, where x and y relate to experimental conditions. Technological parameters, such as temperature, initial copper concentration and solution pH value, have significant effects on particle size, morphology and dispersion of the powders. Powders with various morphologies, pie shape, spindle shape and rod shape, can be synthesized under certain technological conditions.