超细镍粉复合材料的微波电磁特性研究

以蒸馏水为溶剂,利用快捷、温和的液相还原法制备超细镍粉,将得到的超细镍粉作为填料制备了复合材料,考察了复合材料的电磁屏蔽和吸波性能．结果表明,超细镍粉质量分数为80％的树脂基复合材料在130MHz～1．5GHz测试频段范围内的电磁屏蔽性能高于45dB;而厚度为2mm的超细镍粉／石蜡复合材料在7GHz附近的反射率可达-27dB．     

磁场对超细镍粉的磁性能及电磁屏蔽性能的影响

分别在水和乙二醇溶液中,于搅拌条件下采用液相还原法制备超细镍粉,研究反应过程中外加磁场对产物形貌及性能的影响。结果表明,水中得到的产品为刺球状颗粒,外加磁场对产物的形貌影响不大;乙二醇中得到类球形颗粒,加磁场后得到短链状结构。外加磁场使超细镍粉的饱和磁化强度值降低而矫顽力值升高。将水体系中得到的超细镍粉作为导电填料制备电磁屏蔽涂料,结果发现外加磁场条件下得到的超细镍粉/树脂复合涂料在130 MHz～1.5 GHz频段内具有更好的电磁屏蔽性能。     

高分子保护溶液还原法制备球形超细镍粉

高分子保护溶液还原法制备球形超细镍粉沈勇，张宗涛，赵斌，朱裕贞，胡黎明（华东理工大学国家超细粉末工程研究中心，上海２００２３７）戴慕仉（华东理工大学分析测试中心，上海２００２３７）超细镍粉由于表面活性高、导电性和导热性好而被广泛用于电池电极、硬质合金...     

SDS-PVP水溶液中超细镍粉的制备

在十二烷基硫酸钠(SDS)-聚乙烯吡咯烷酮(PVP)混合水溶液中, 采用水合肼还原氯化镍制备超细镍粉. SEM结果表明, 该超细镍粉为球形, 表面呈现针状叠合的特殊形貌. XRD结果表明,该超细镍粉由平均粒径约为10 nm的面心立方结构(fcc)的原生纳米镍晶粒组成, 且主要沿(111)晶面生长. TEM清晰观察到原生纳米镍晶粒在PVP的空间桥联作用下自组装成超细镍粉的中间过程. SDS-PVP的组成对超细镍粉的粒径和表面形貌有显著影响, 在一定浓度范围内, 随着SDS或PVP浓度增大, 原生纳米镍晶粒和超细镍粉的平均粒径均呈减小趋势, 表明通过改变SDS-PVP组成可以调控超细镍粉的粒径和形貌.     

溶液还原法制备球形超细镍粉

超细镍粉由于表面活性高、导电性和导热性好而被广泛应用于化学催化剂、烧结活化剂、导电浆料门等方面．目前，制备超细镍粉的方法主要有问：真空蒸馏冷凝法、机械粉碎法、电解法、羰基镍热分解法、浆化氢还原法和溶液还原法等．在这些方法中，溶液还原法的工艺简单，所得粉末纯度高，颗粒尺寸小且分布均匀[3]．法国的Figlarz等[4]用弱有机还原剂乙二醇还原粒径小干0．1μm的Ni（OH）2。超细粉末，引入AgNO3。作为成核剂后，制得了粒径＜1μm的超细镍粉，但这种方法需长时间高温回流反应，对原料要求苛刻，且采用有机分散介质成本较高，…     

纳米镍包覆超细铝复合粉末的氧化性能

通过置换还原法, 快速、简洁、定量地制备出了纳米镍包覆的超细铝粉复合粉末. 利用扫描电子显微镜(SEM)、热重分析(TGA)、差示扫描量热(DSC)和X射线衍射(XRD)等分析手段对原料Al粉和复合粉末的形貌及其氧化性能进行研究. 结果表明, 原料Al粉在1050 ℃时增重率为122%, 当包覆的纳米镍粉质量分数为0.75%时, 可以使铝粉在1050 ℃时的增重率达到135%, 并且随着镍粉含量的增加, 铝粉的增重率进一步提高. 当镍的质量分数达到8.93%时, 复合粉末在约1000 ℃时出现点火燃烧现象. 纳米镍粉的氧传递对促进超细铝粉的氧化起到了至关重要的作用.     

五羰基铁催化羰化反应的研究进展

1827年,丹麦药剂师Zeise在加热PtCl2/KCl的乙醇溶液时得到了世界上第一个金属有机化合物,即后来人们命名的Zeise盐[1].1890年,Mond[1]等在研究一氧化碳（CO）对不锈钢阀门的腐蚀原因时发现：CO与镍粉反应生成的四羰基镍（Ni（CO）4）对阀门具有腐蚀作用．     

片状镍粉的制备及其磁性研究

利用湿法研磨法由微米镍粉制得了不同尺寸的片状镍粉;利用X射线衍射仪和扫描电子显微镜研究了研磨参数对片状镍粉形貌和微观结构的影响;测定了产物的室温磁性能.结果表明,球料比和研磨时间是影响片状镍粉形貌的关键因素,片状镍粉的剩磁比和矫顽力都比原料微米镍粉的高.所采用的制备方法具有效率高、成本低且产物形状及磁性能可控的特点,适...     

NiB和NiP超细非晶合金的退火晶化行为及催化性能

 采用X射线吸收精细结构（XAFS）,X射线衍射（XRD）和差热分析（DTA）等方法研究了以化学还原法制备的NiB和NiP超细非晶态合金催化剂在退火过程中的结构变化．XRD结果表明,在300℃下退火时,NiB超细非晶态合金晶化生成纳米晶Ni3B亚稳物相,NiP超细非晶态合金则主要晶化生成金属Ni和部分晶态Ni3P的混合物相;在500℃退火且近于完全晶化的条件下,大部分超细非晶态合金都晶化为金属Ni．XAFS结果定量地说明,对于NiB和NiP初始样品,第一近邻Ni－Ni配位的平均键长Rj分别为0.274和0.271nm,其结构无序度σS很大,分别为0.033和0.028nm,其热无序度σT分别为0.0069和0.0060nm．300℃退火后,晶化生成的Ni3B的Ni－Ni配位的σS降低到初始样品的33％,仅为0.011nm．500℃退火后,NiB样品的结构参数与金属Ni基本一致,但NiP样品的Ni－Ni配位的σS还远大于σT,仍为0.0125nm,表明NiB和NiP超细非晶态合金的退火晶化行为有很大的差别．纳米晶Ni3B催化苯加氢反应的转化率比超细Ni－B非晶态合金或多晶金属Ni更高,表明纳米晶Ni3B中的Ni与B原子组成了苯加氢催化反应的活性中心．     

以甲醛作还原剂制备超细铜粉

以甲醛作还原剂制备超细铜粉刘志杰，赵斌，张宗涛，胡黎明（华东理工大学化学系，上海２００２３７）（华东理工大学国家超细粉末工程研究中心）超细铜粉已得到广泛应用，不同粒径的铜粉有不同的用途：应用于电学领域的铜粉大部分是微米级铜粉［１］；纳米级铜超微粒子分...     

Nickel nanoparticles obtained by a modified polyol process: synthesis, characterization, and magnetic properties

The synthesis of nickel nanoparticles using poly(N-vinilpyrrolidone) (PVP) as protective agent was studied. The nanoparticles were prepared in air according to a modified polyol route, using nickel chloride as precursor and sodium borohydride as reducing agent. Samples with different nickel/PVP ratio were obtained. The X-ray diffraction and transmission electron microscopy (TEM) measurements indicate the occurrence of face-centered cubic metallic nickel nanoparticles with a medium diameter of 3.8 nm and good size dispersion. Fourier transformed infrared spectroscopy (FT-IR) and X-ray photoelectron spectroscopy (XPS) data show an effective interaction between the nickel nanoparticles surface and the carboxyl oxygen atoms of PVP. Magnetic measurements show single-domain nonideal superparamagnetism behavior due to dipolar magnetic coupling between particles.     

Synthesis of nickel nanoparticles and carbon encapsulated nickel nanoparticles supported on carbon nanotubes

Nickel nanoparticles were prepared and uniformly supported on multi-walled carbon nanotubes (MWCNTs) by reduction route with CNTs as a reducing agent at 600 °C. As-prepared nickel nanoparticles were single crystalline with a face-center-cubic phase and a size distribution ranging from 10 to 50 nm, and they were characterized by transmission electron microscopy (TEM), high-resolution TEM and X-ray diffraction (XRD). These nickel nanoparticles would be coated with graphene layers, when they were exposed to acetylene at 600 °C. The coercivity values of nickel nanoparticles were superior to that of bulk nickel at room temperature.     

铝表面前处理及化学沉积镍初期行为

利用开路电位-时间(EOCP-t)曲线,研究铝表面经浸镍和化学预镀镍前处理后,化学沉积镍的初期行为;通过扫描电子显微镜(SEM)观察铝表面经前处理后的表面形貌.结果表明:未经及经前处理的铝表面,化学沉积镍的初期行为都经历去氧化膜、活化、混合控制以及化学沉积过程.经过浸镍和化学预镀镍前处理后的铝表面附着细小的镍颗粒.依据EOCP-t和SEM的最佳实验结果,在含有络合剂和还原剂的碱性预镀镍溶液中,经二次化学预镀镍前处理,成功实现铝基底弱酸性化学镀镍.所获得的化学镀镍层与铝基底结合牢固,呈团颗粒状形貌和非晶态结构.     

Electrodeposited paint-and-varnish nickel–polymer coatings

Specific features of preparation of paint-and-varnish nickel–polymer coatings by joint cathodic electrodeposition of an amine-containing oligomeric electrolyte and nickel were studied. The coatings obtained exhibit layer-by-layer heterogeneity, with the lowest layer constituted by an intermetallic compound of nickel with iron. The coatings are characterized by higher degree of cross-linking compared to the polymer coatings without nickel. A paint-and-varnish formulation based on a nickel–polymer film-forming agent was developed for electrodeposition of corrosion- and wear-resistant coatings.     

Pulsed Current Electrochemical Synthesis of Nickel Nanoclusters and Application as Catalyst for Hydrogen and Oxygen Revolution

The main objective of this research is to prepare nickel nanoparticles with more porous structure by the pulsed current electrochemical method. A nickel optimized nanopowder was synthesized by using nickel chloride (0.005 M) as precursor, silver nitrate as a nucleation agent (at 0.5% mole of nickel salt in the starting solution), polyvinyl pyrrolidone (PVP) as structure director (with PVP/Ni = 1.7 g/g), ammonia (2 M), and hydrazine as reduction agent (with Hydrazine/Ni = 16 g/g) by pulsed current of 58 mA cm⁻² with a frequency of 12 Hz. The morphology and particle size of each synthesized sample was studied by scanning electron microscopy (SEM). The obtained results showed that temperature has no considerable effect on the morphology and particle size of nickel nanopowder. The nickel nanopowder synthesized in optimum conditions has excellent uniform and a more porous structure including nanoclusters with a particle size of approximately 10–20 nm. The obtained results indicate that the pulsed current electrochemical method can be used as a confident and controllable method for the preparation of nickel nanoparticles. Optimized nickel nanoclusters were used as catalyst for hydrogen and oxygen revolutions. Cyclic Voltammetry results showed that the synthesized nanoclusters can facilitate hydrogen reduction and increase hydrogen and oxygen revolution rates.     

漆原镍催化剂用于苯酚催化加氢

利用锌粉将NiCl₂液相还原制备漆原镍催化剂,考察了碱/酸活化方法、锌粉用量、还原温度、添加载体等条件下漆原镍催化苯酚加氢反应的性能。结果表明,锌粉还原的漆原镍催化剂可用NaOH或者乙酸活化处理,NaOH的效果优于乙酸。与不添加载体的催化剂相比,添加载体组分明显提高了金属镍的分散性和利用率。γ-Al₂O₃、CaCO₃、MgO均可作为漆原镍催化剂载体组分,而γ-Al₂O₃效果最好。还原剂锌粉用量、载体加入量过少或过多,都会造成催化剂活性降低,这与其影响金属镍的可接近性及分散性相关。无载体或加入载体的漆原镍催化剂均可在120~160 ℃催化苯酚加氢反应,主要产物为环己醇和环己酮,并以环己醇为主。     

Synthesis of nickel metal nanoparticles via a chemical reduction of nickel ammine and alkylamine complexes by hydrazine

Nickel nanoparticles were prepared from their coordination compounds, such as [Ni(NH₃)₆]Cl₂, [Ni(N₂H₄)₂Cl₂], [Ni(HNEt₂)₆]Cl₂, and [Ni(H₂NBu)₆]Cl₂ in aqueous solution by chemical reduction. The reaction of nickel ammine and alkylamine complexes with hydrazine monohydrate as a reducing agent was carried out at 90 °C and pH = 10–12. Depending on the influencing parameters such as oxidizing agent, pH, and temperature, the hydrazine reaction can be carried out in different pathways. The chemical reduction method is a simple procedure and also is the best one in the controlling of composition, size, and shape of Ni powder. The reduction of nickel complexes into the metallic Ni powder occurs via the dissociation of complexes and reduction by hydrazine in alkaline solution. Therefore, complexing agents have the most effect on the reduction reaction. The results show that, when the ligands in complexes were changed from ammine to diethylamine and butylamine, respectively, the crystalline size and morphology of nickel metal nanoparticles are changed. The chemical reduction of nickel complexes into metallic nickel can be accompanied with a change in the crystalline system. The pure nickel crystalline has a face-centered cubic structure. The nickel nanoparticles were characterized using IR spectroscopy, X-ray powder diffraction, scanning electron microscopy and vibrating sample magnetometer analyses.     

不同形貌Co3O4和NiO的可控合成及光学性质

采用沉淀法,选择不同的钴盐和镍盐,以草酸为沉淀剂,磷酸三钠作为形貌导向剂,分别合成了具有特殊形貌的四氧化三钴和氧化镍。并对样品进行了微观结构、形貌和光学性质的表征。结果表明:在磷酸三钠的辅助下,四氧化三钴的晶体生长沿一维方向发展,氧化镍的晶体生长沿二维方向发展。紫外光谱测试表明,磷酸三钠参与下得到的四氧化三钴和氧化镍的禁带宽均增加。     

Thermal properties and reactivity determination of micro- and submicrometer nickel powders

Monodispersed fine metal nickel powders of uniform shape and high purity are increasingly required for specific uses in many technological areas, especially in the preparation of electronic materials such as the manufacture of conductive inks and pastes and the formation of catalysts. Metallic nickel powders were prepared in ethylene glycol by the reduction of a nickel solution. Hydrazine was used as a reducing agent. Metal powders were characterized by chemical analysis, scanning electron microscopy (SEM), thermogravimetry (TG), derivative thermogravimetry (DTG) and differential scanning calorimetry (DSC). Particle size distributions were determined using laser light scattering. The reactivity and purity of these fine nickel powders were tested by repeated oxidation and reduction of nickel powders in oxidative and reductive atmospheres.