沉淀转化-热分解法制备纤维状镍粉

以氯化镍、草酸铵和氨水为原料,通过沉淀转化制备纤维状前驱体。采用XRD、SEM、IR和 DTA/TGA分析手段研究前驱体粉末的成分与形貌。结果表明：在pH=8.4~8.8时得到的前驱体在形貌和成分等方面均不同于在 pH=6.0得到的前驱体,且两种条件下所得前驱体热分解的机理也不同。研究前驱体形貌、热分解气氛、温度及时间对镍粉形貌及分散性的影响,发现前驱体粉末在弱还原性气氛、温度为400~440°C下分解30 min时,最终产品基本保持前驱体的形貌。得到的纤维状镍粉分散性良好,但每根纤维表面不再光滑,而是具有大量微孔的粗糙形态。     

Preparation and characterization of fibrous NiO particles by thermal decomposition of nickelous complex precursors

The influences of pyrolytic conditions, including temperature, time, the flow rate of air, and the heating rate, on the morphology, average size and specific surface area of the NiO particles were investigated, and the composition and morphologies of the products were characterized by using of XRD, SEM and BET. It is found that fibrous NiO particles were produced under the optimal conditions. A suitable range of pH for preparing dispersive precursors was chosen according to analysis of zeta potential. Based on the observations of NiO precursors growth and SEM morphology of the precursor, the oriented attachment was proposed for the well-aligned growth of the NiO precursor fibres. The final product NiO inherits the morphology of the precursor.     

Thermodynamic analysis on preparation of fibrous NiO precursor powders with oxalate precipitation process

According to the principles of simultaneous equilibrium and mass balance, a series of thermodynamic equilibrium equations of Ni（ Ⅱ）-C2 O4^2--NH3-NH4^＋-H2O system at ambient temperature are deduced theoretically and the logarithm concentration versus pH value（lg[Ni^2＋ ]r-pH） diagrams at different solution compositions are drawn. The results show that when pH is above 8.0, nickel ions coordinate with ammonia, the precipitation proceeds slowly accompanying with the release of nickel ions from the multi-coordinated Ni（NH3）n^2＋ （n= 1, 2,…, 6） and the morphology of NiO powder precursor is fibrous; when pH is below 8.0, nickel ion directly reacts with C2O4^2- and the morphology of NiO powder precursor is of cubic-shape. Some experiments were made to confirm the relation between the total concentration of nickel ion and pH. It is shown that the thermodynamic mathematical model is correct and the calculated values are basically accurate.     

固相诱导沉淀法制备单分散NiO微粒

将草酸以固体粉末形式添加到镍氨配合溶液中,沉淀出均一分散的草酸镍铵复合盐(类)球形颗粒,经热分解后可得到单分散NiO微粒。草酸以粉末形式加入,其固液界面对草酸镍铵沉淀微粒的形貌具有显著的诱导效应。实验研究表明,当配合溶液的氨镍摩尔浓度比等于5︰1(其中镍离子浓度设定为0.5mol·dm-3),反应温度为40℃,加入草酸后混合溶液pH值为8.8,反应时间为10min时,得到平均粒度为1.1μm的沉淀颗粒,450℃下热分解后粒子体积发生收缩,形成平均粒度为0.8μm的NiO微粒。该方法易于得到均一的单分散微粒,并可显著减小沉淀母液的体积量。     

废镍催化剂回收制备纤维状氢氧化镍

研究从废旧镍催化剂中回收镍以制备氢氧化镍。采用酸浸法,在90℃下用1mol／L硫酸浸没废镍催化剂,从中提取镍。向净化后的含镍溶液中加入NaOH,分别采用3种不同的方法,即尿素水解、传统方法和水热方法制得3种不同的氢氧化镍,分别命名为Ni（OH）2-U,Ni（OH）2-C和Ni（OH）2-H。与传统方法相比,采用水热方法制得的氢氧化镍具有更好的结晶度。Ni（OH）2-C和Ni（OH）2·H都含有β-Ni（OH）2与a-Ni（OH）2·0．75H20的混合相,而Ni（OH）2．U只含有a-Ni（OH）2．0．75H20相。TEM观察显示Ni（OH）2-U样品具有棒状结构。在这3种样品中,Ni（OH）2-U表现出最好的电化学活性。     

Preparation of fine nickel powders via reduction of nickel hydrazine complex precursors

Fine nickel(Ni) powders with controllable particle sizes were synthesized via the reduction of nickel hydrazine complex precursors of pure [Ni(N2H4)2]Cl2 and a mixture of [Ni(N2H4)2]Cl2 and [Ni(N2H4)3]Cl2 in aqueous solution. The mechanism of the formation of metallic Ni powders experiences the reduction of nickel hydroxide by hydrazine released from the ligand exchange reaction between nickel hydrazine complex and NaOH. In comparison with the method of preparing Ni powders from nickel salts, the method of making Ni powders via the reduction of nickel hydrazine complex precursors shows the advantages of using half dosage of hydrazine for complete reduction of nickel ions in solution, and the obtained Ni particles show less agglomeration and better dispersibility. Moreover, the average particle size of nickel powders can be controlled from 180 to 260 nm by adjusting the reaction molar ratio and concentration.     

均相沉淀法制备氧化镍纳米线

以尿素、硫酸镍为原料,用均相沉淀法制备了氧化镍纳米线,并通过X射线衍射(XRD)、透射电镜(TEM)及红外光谱等测试手段对所得产物的组成和形貌进行了研究.TEM结果表明,所得产物为多晶氧化镍纳米线,直径和长度分别为5～15 nm和250～350 nm.通过对前驱体产物在不同温度下煅烧,发现纳米线在600℃分解为颗粒.作为比较,以尿素为沉淀剂,用水热法制得氧化镍纳米粉体,结果得到球形和排列整齐的棒状两种形态.     

Prediction of powder characteristics of uniform NiO precursor prepared by homogeneous precipitation

Uniform NiO precursor particles were prepared by homogeneous precipitation in the presence of urea. Optimal discrimination plan, one of the chemical pattern recognition techniques, was applied to analyze the experimental data and the quantitative relationships among the process parameters and powder characteristics of the obtained particles were determined. It proves that the model fits well with the experimental results and it is quite effective to guide the process design. Based on the above results, an improved La Mer model and the reasonable formation mechanism of the particles are proposed.     

Cf／SiC陶瓷基复合材料的制备工艺研究

以先驱体浸渍裂解（PIP）工艺制备了2DC／SiC复合材料，研究了低温裂解工艺（裂解温度低于1000℃）对2D Cf/SiC复合材料结构和性能的影响，为Cf／SiC复合材料的低温制备探索可行之路。研究表明，采用900℃裂解工艺制备的复合材料其力学性能达到或高于目前同类工艺制备的2D Cf／SiC复合材料力学性能，其弯曲强度达到329．6MPa，剪切强度32．1MPa，断裂韧性14．7MPa·m^1/2。并采用差热（TG-DTA）、红外光谱（IR）、X射线衍射（XRD）等对先驱体聚碳硅烷（PCS）及其低温裂解产物的结构和性能进行了研究。     

碳纤维增强氮化物基复合材料的制备及其性能表征

合成了全氢聚硅氮烷和硼氮烷的混杂先驱体并对其结构进行了表征；以混杂先驱体和3D碳纤维编制体为原料，采用先驱体浸渍-裂解（PIP）工艺制得了碳纤维增强氮化硼．氮化硅混杂基体的复合材料，并对复合材料的力学性能和抗烧蚀性能进行了研究。结果表明，混杂先驱体中含有B—N，B—H，Si—N，Si—H，N—H等结构，无其它杂质出现；随着PIP工艺循环次数的增加，复合材料的密度随之提高：当进行4个循环时基本致密，密度达到1．50g／cm^3，弯曲强度达到156．4MPa；轨道模拟实验显示复合材料具有优异的抗烧蚀性能。     

形貌控制法合成一种新型的纤维状镍钴合金粉末前驱体(英文)

通过选择性控制合成条件,制备一种新型的纤维状镍钴合金粉末前驱体。该前驱体中镍、钴摩尔配比精确。采用X-射线衍射仪(XRD)、扫描电镜(SEM)、红外光谱(FT-IR)和能谱(EDS)研究前驱体粉末的成分与形貌;考察溶液pH值、反应温度、金属离子浓度和表面活性剂对前驱体粉末的形貌和分散性的影响。结果表明:前驱体的形貌取决于前驱体中氨的含量,这种纤维状前驱体为一种复杂的含氨草酸镍钴复盐。形貌控制合成纤维状镍钴合金粉末前驱体的最佳条件为:氨作为配位剂和pH值调节剂,草酸为沉淀剂,反应温度为50～65°C,镍、钴离子总浓度为0.5～0.8mol/L,PVP为分散剂,溶液pH值控制在8.0～8.4.     

Preparation and Characterization of Co0.3Cr0.7Ox Particles Using for Thermal Radiation Coating

Novel Co0.3Cr0.7Ox(x=2-3)particles with spinel structure were synthesized via precipitation method through the reactions among CoSO4,Cr(NO3)3 and NaOH solutions,followed by spray-drying and sintering at 1200 ℃for 4h in the air.The particles were characterized by X-ray diffraction(XRD)and scanning electron microscopy(SEM).The XRD results revealed that the particles are composed of Co0.3Cr0.7Ox phase without the presence of other phases.The SEM observation showed that the particles are in the shape of sphere with well flowability.Infrared radiation test indicated that the total infrared normal emissivity of the coating made of Co0.3Cr0.7Ox can be up to 0.92 at 800℃.And the normal emissivities of the prepared Co0.3Cr0.7Ox particles are always slightly larger than those of CoCr2O4 particles prepared by solid-state reaction method in the test temperature range of 50-300℃.The relatively high thermal emissivity of Co0.3Cr0.7Ox is assumed to be mainly attributed to the spinel structure.These results indicated that Co0.3Cr0.7Ox particles are a good thermal radiation material,which can be used as infrared radiation layer in thermal protection system.     

Pyrolysis mechanism of ZrC precursor and fabrication of C/C-ZrC composites by precursor infiltration and pyrolysis

C/C-ZrC composites were prepared by precursor infiltration and pyrolysis using the organic zirconium as precursor. The conversion mechanisms of the precursors such as the thermal behavior, structural evolution, phase composition, microstructure, composition of the precursors and products were analyzed by thermal gravimetric analyzer, Fourier transform infrared spectrometer, X-ray diffraction and scanning electron microscope. The results indicate that the ZrC precursor transforms to inorganic ZrO₂ from room temperature to 1200 °C, then reduces to ZrC at 1600 °C through the carbothermal reduction reaction. The microstructure of the C/C-ZrC composites was also investigated. The composites exhibit an interesting structure, a coating composed of ZrC ceramic covers the exterior of the composite, and the ZrC ceramic is embedded in the pores of the matrix inside the composite.     

钛粉在聚硅氮烷裂解制备陶瓷材料中的应用

采用IR、TG、XRD等手段研究分析钛粉作为活性填料在聚硅氮烷裂解制备陶瓷材料中的应用。实验表明：钛粉可以有效改善先驱体的陶瓷产率,本实验中纯PSN-1先驱体在经1300 ℃裂解陶瓷产率仅为37.3%,通过加入质量比3/10（Ti/PSN-1）的钛粉,经1300 ℃裂解陶瓷产率为78.7%,提高了约40%;经红外光谱分析表明,通过向先驱体中加入Ti粉可以加速有机先驱体向无机陶瓷转化的速度;经X衍射分析表明,Ti粉作为活性填料能与先驱体裂解挥发份及保护气氛发生反应,生成TiC、TiN等新的物相,有利于提高陶瓷产率。     

Preparation of ultrafine core-shell nickel spheres via self-sacrificial template

1 Introduction Ultrafine particles stand for granules with diameter less than 0.5 μm. For their extremely small size and large specific surface area, these sub-micron powders can be widely used as catalysts, adsorbents in the fields of chemistry, physics…     

Discrepancies in the morphology and physical properties of amorphous and crystalline sprayed lanthanum nickel oxide films

Amorphous LaNiO₃ (a-LNO) and crystalline LaNiO₃ (c-LNO) films were prepared by spraying an aqueous precursor solution of lanthanum and nickel chlorides on hot (450 °C) fused silica substrates followed by annealing at high temperatures (550–850 °C). Thermal analysis of a dried precursor indicated that a stable oxide phase is formed at 560 °C with no distinct crystallization peak. Scanning electron microscopy (SEM) powered with energy-dispersive X-ray spectroscopy (EDX) of as-sprayed films showed rough surfaces with particulate-like deposits and incomplete pyrolysis chloride composition. No chloride contents were detected in annealed films. X-ray diffraction showed that films annealed at 550 °C and 650 °C were a-LNO and those annealed at 750 °C and 850 °C were c-LNO. The c-LNO phase was indexed as a single-phase perovskite structure with (1 1 0) orientation. SEM/EDX showed that a-LNO films have rough surfaces and c-LNO films have uniform crack-free smooth surfaces. Electrical properties measurements showed that c-LNO films have lower resistivity than a-LNO films and both types of LNO films have semiconductor resistant temperature dependence. The activation energy of electric conduction of a-LNO films was found to be much higher than that of c-LNO films. The optical transmittance and reflectance of the films were studied in the UV–visible–near IR range. The optical constants were obtained by modeling the measured transmission and reflection spectra. Because of the discrepancies in the morphology and in the physical properties of a-LNO and c-LNO films, the best fit modeling of transmission and reflection spectra was obtained by using different theoretical models and different geometrical configurations. While the Drude model accounting for larger carrier density was found to be significant for c-LNO, using the Bruggmann model and a configuration of a rough layer on top of a compact film was found to be significant for a-LNO.     

纳米金属颗粒分散氧化物Ag／NiO薄膜的制备与光吸收特性

利用溶胶．凝胶法制备了纳米金属颗粒分散氧化物Ag／NiO复合薄膜，用X射线荧光光谱、X射线衍射分析、透射电子显微镜、紫外可见分光光度计表征了薄膜的成分、相结构、微结构以及光吸收特性。X射线衍射分析结果表明存在NiO相和单质Ag相。光吸收谱研究表明，Ag／NiO薄膜在410nm波长附近有明显的表面等离子共振吸收峰，随着Ag含量的增加，吸收峰变窄，蓝移，强度增加。当Ag含量接近41％（质量分数）时，Ag／NiO薄膜在414nm波长附近表现的吸收峰呈现最大的吸收强度；当Ag分散颗粒的含量超过41％（质量分数）后，吸收峰的强度开始下降。随着保温时间的延长，薄膜的光学吸收峰的强度增强，并且吸收峰峰位向波长短的方向移动。     

Preparation of basic nickel carbonate particles in solution system of Ni( Ⅱ )-NH3-CO2-3-H2O

Based on the principles of simultaneous equilibrium and mass balance, a series of thermodynamic equilibrium equations of Ni( Ⅱ )-NH3-CO2-3-H2O system at ambient temperature were deduced theoretically and the thermodynamic diagrams of lg[Ni]T versus pH at different solution compositions were drawn, which was quite effective to explain the formation mechanism of precipitation particles with different microscopic shapes. When pH of the solution is below 7.0, free nickel ions are dominant and when the precipitant is added, the fast coagulation will take place leading to the loose flocculation particles. While pH is above 7.0, because of the coordination of nickelion with ammonia, the precipitation proceeds slowly accompanying with the release of Ni2 from the multi-coordinated Ni(NH3)2 n (n= 1, 2, …, 6), which easily leads to the formation of the dense spherical particles.     

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。     

碳纳米管铜基复合颗粒的制备

采用混酸纯化法在碳纳米管表面引入羟基和羧基等基团.利用明胶使碳纳米管均匀地分散在五水硫酸铜溶液中,用葡萄糖在碱性条件下还原得到氧化亚铜内嵌碳纳米管复合颗粒,将其还原获得铜基内嵌碳纳米管复合颗粒.SEM和TEM观察结果表明碳纳米管均匀地分布在几百纳米至1μm的复合颗粒中.XRD分析表明得到的产物是纯净的Cu2O和Cu颗粒.复合球形貌影响因素研究发现明胶在复合物成球过程中起着关键性的作用,明胶与CNTs质量比为5～7时配比效果最佳.