Influence of pulse parameters on the microstructure and microhardness of nickel electrodeposits

Square-wave cathodic current modulation was used to electrodeposit fine-grained nickel from an additive-free and saccharin-containing Watts bath. The influence of pulse on-time, off-time, peak current density and saccharin on the grain size, surface morphology, crystal orientation, and microhardness was determined. The study showed that at constant off-time and peak current density, the crystal size of the deposits was found initially to decrease with pulse on-time before it started to increase with further increase in on-time. The crystal orientation progressively changed from a (111) texture at the on-time of 0.1 ms to a strong (200) texture at an on-time of 8 ms. An increase in the pulse off-time at constant on-time and peak current density resulted in a progressive increase in crystal size. However, the crystal orientation remained unaffected with increasing off-time. An increase in peak current density resulted in considerable refinement in crystal size of the deposits. The crystal orientation progressively changed from an almost random distribution at the lowest peak current density of 0.2 A/m² to a strong (200) texture at a peak current density of 2.0 A/m². The nanocrystalline nickel with grain size in the order of 30 nm can be produced from saccharin-containing Watts' baths. In contrast, when using an organic-free Watts' bath and similar pulse-plating conditions, the grain size can only be refined down to about 80-100 nm. The microhardness of deposits is related with grain size: when the grain size is large, the microhardness is consistent with Hall-Petch law (HPL); when the grain size is ultrafine, “nano-effect” would be generated, the microhardness is against HPL.     

Effect of substrate pretreatment on the porosity in thin nickel electrodeposits

Substrate pretreatment affects the porosity of thin nickel electrolytic coatings which is a combined function of the composition and the roughness of the substrate surface. Electropolishing the substrate surface is an effective method of reducing coating porosity, whereas coatings plated on either electroetched or mechanically ground substrates are relatively porous owing to the remaining oxide layer on the substrate and the increased roughness of the substrate. For nickel coatings plated on mechanically ground rough substrates, the relationship between nickel porosity, apparent coating thickness and substrate roughness has been examined.     

Porosity of nickel electrodeposits on mild steel using electrochemical impedance spectroscopy

Abstract

Impedance spectroscopy recorded at the open circuit potential in 1M H₂SO₄ at 293 K is shown to provide a convenient test for detecting the degree of through porosity in electroplated nickel coatings, electrodeposited from a Watts bath, on mild steel. The impedance data can be interpreted in terms of a simple equivalent circuit, and the corrosion resistance provides a reliable guide to the quality of the deposit. The quantitative estimation of porosity from these data is considered.     

熔烧状态对Co基合金涂层显微结构及硬度的影响

采用高频感应真空熔覆技术,制备钴基合金涂层.使用扫描电子显微镜观察涂层在不同深度的组织结构,用X射线能谱仪(EDS)探测涂层的化学元素组成,用显微硬度计测量涂层不同深度的显微硬度值.试验结果表明,熔烧状态的不同对涂层和基体化学元素之间扩散程度有显著的影响.熔烧时间越长,扩散程度越大.钴基合金涂层的硬度显著高于Q235钢基体,其显微硬度随着熔烧时间的延长而略有降低,但其硬度更均匀.     

选择性还原-磁选回收镍渣中的有价金属

采用选择性还原-磁选工艺富集某镍渣中的镍、铜,通过控制还原过程参数实现选择性还原。结果表明：添加熔剂并适当提高渣料的碱度（CaO与SiO2质量比）有助于镍、铜的富集;对碱度0.15、还原温度1200℃、还原时间20 min、内配煤量5%（质量分数）的优化条件下得到的还原样品,通过磨矿-磁选获得镍、铜、铁品位分别为3.25%、1.20%、75.26%的精矿,镍、铜、铁的回收率分别为82.20%、80.00%、42.17%,实现了镍、铜相对于铁的选择性富集;选择性还原-磁选没有显著降低S、P的含量,两者在工艺过程中的行为需要进一步研究。     

Use of the reverse pulse plating method to improve the properties of cobalt-molybdenum electrodeposits

Conditions leading to cobalt-molybdenum (Co-Mo) electrodeposits with high Mo percentages were studied. Deposits prepared by means of direct current electroplating showed a large amount of cracks. Maximum amount of Mo in the films was attained by applying deposition potentials in the − 1200 mV to − 1300 mV range. Reverse pulse plating mode has been proved useful for obtaining nanocrystalline, low stressed Co-Mo deposits with similar Mo percentages as in direct current conditions (35-40 wt.%). The coatings were exposed to a static microindentation test, which highlighted that the pulse plated samples were more compact and less fragile than the direct current plated ones.     

Effect of the magnetic state on the damping properties of iron and nickel alloys

The dependences of the ΔEeffect and internal friction on the magnetic field have been investigated upon the magnetization and magnetization reversal of some polycrystalline ferromagnetic materials with different properties. It has been shown that for all the materials that have been investigated there is characteristic a nonmonotonic dependence of the magnitude of internal friction on the magnetic field both for the magnetization curves and for the major hysteresis loops. It is shown that in the sonic frequency range of elastic vibrations the basic mechanism of the formation of the magnetic peaks of internal friction in the materials investigated is magnetostrictive; the damping depends simultaneously on the instantaneous values of magnetostriction and magnetostrictive sensitivity.     

The use of ACORN to determine Sub-structures

Using the concepts described in the preceding paper of this volume (Foadi, J. (2003). Cryst. Rev. , 9 , 43-65) and the references therein, it has been shown that the ACORN program can position the atoms of the sub-structure of a protein using the anomalous or dispersive differences generated from these sites.     

Improvement of physical properties of Cu-infiltrated W compacts via electroless nickel plating of primary tungsten powder

In the present research, tungsten particles were coated using nickel/nickel-phosphorus electroless plating technique. The coated tungsten powders were pressed under constant pressure to achieve compact material of cylindrical shape with same porosity. Then, attained compacts were infiltrated/penetrated by liquid copper under the hydrogen atmosphere in order to obtain W-15 wt.% Cu composites. The coated/uncoated powders as well as its infiltrated compacts were characterized by optical microscopy (OM) as well as scanning electron microscopy (SEM), EDS and XRD methods. The microstructure, relative density and specific resistivity of composites were compared. The microstructural observations revealed that the infiltration behavior can be improved in the compacts prepared by both nickel and nickel-phosphorus coated tungsten powders, in comparison with uncoated ones. In addition, it was found that relative density may be raised from < 85% to > 95% by nickel electroless plating, that leads to decrease specific resistivity from 6 to 4 µΩ cm. Enhancement of electrical conductivity of infiltrated W-15 wt.% Cu compacts prepared by electroless nickel coated tungsten powders was related to its higher density.     

Influence of process parameters on electrochemical and physical properties of sputtered iron-doped nickel oxide thin films

1Introduction A principal focus of modern research in electrocatalysis is to discover electrode materials that exhibit excellent electrochemical stability and show interesting activity towards typical electrochemical reaction[1?10].It is desirable that th…     

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.     

转速对高压扭转Cu试样的组织与性能的影响

通过高压扭转(HPT)技术在不同转速条件下实现了Cu试样的晶粒细化.利用光学显微镜(OM)、透射电镜(TEM)及显微硬度计观察并测试了组织的结构与性能,并基于有限元计算了变形诱导试样的温升,研究了转速对Cu试样的组织细化与性能的影响.结果表明:转速由1/3 r·min-1增大至1 r·min-1,经1圈扭转变形,试样温度由40.8℃升高到54.1℃,变形组织均为100～600 nm的高位错密度位错胞/亚晶组织,显微硬度由初始态的52HV0.05增大至140 HV0.05;经16圈扭转变形,试样温度由50.4℃升高到97.4℃,组织细化到200 nm.慢速扭转变形试样晶内位错密度高,微观组织处于严重变形状态;而快速扭转试样晶内衬度均匀,位错较少,微观组织经历明显的动态回复,显微硬度较慢速扭转变形试样低6%.     

钢带缠绕预应力模具缠绕层数的确定方法

采用钢带缠绕预应力模具,可有效提高模具的强度、刚度。确定缠绕层数是设计钢带缠绕预应力模具的关键问题之一,对建立缠绕张力计算公式具有重要作用。文章将缠绕对象简化为厚壁圆筒,基于拉美公式和强度理论等,建立了钢带预应力缠绕模具的缠绕层数确定方法。通过VC++设计了用户计算应用程序,实现了缠绕层数的自动计算。通过3个实际算例,分别比较了缠绕模具与组合预应力环模具的外形尺寸;脆性材料模芯与塑性材料模芯缠绕层数;塑性材料模芯的缠绕层数随其许用强度的增加的变化规律。其结果表明,该文建立的钢带缠绕预应力模具缠绕层数确定方法是可行的,钢带预应力模具具有比组合模具更为优越的性能。     

Structural-phase state and properties of film compounds obtained by different methods of physical deposition

Methods of physical deposition were used to prepare films of chemical compounds with different phase composition, structural perfection, and properties. A temperature criterion, which makes it possible to predict conditions for obtaining products of solid-state reactions with an assigned structural perfection, has been derived on the basis of the developed macroscopic theory of epitaxy. It is asserted that the main factor which determines the structural-phase state of the transition-metal films is the energy of atoms that are condensed on the substrate.     

一种求解双曲线本构方程中材料常数的方法

基于单参数非线性最小平方法,提出了一种优化求解双曲线本构方程中表观激活能和其他材料常数的方法。利用热压缩试验获得的热变形流变应力数据,采用该方法得到了T122和T91耐热钢不同应力水平的表观激活能和其他材料常数,确定材料常数后的双曲线方程所预测的流变应力与试验值符合很好,表明该方法可方便准确求解热变形激活能和其他材料常数,且确定材料常数后的双曲线本构方程能够应用于计算不同应变速率和温度下的热变形流变应力。根据双曲线正弦函数的定义,建立了T122钢和T91钢热变形条件下流变应力双曲线本构方程的显式表达式。     

Structural features of nanocrystalline nickel subjected to high-pressure torsion

The specific microstructural features of the nanocrystalline nickel obtained by the method of electrodeposition (ED) and then subjected to severe plastic deformation by torsion (HPT) were studied for the first time. For comparison, the specific structural features of the samples obtained by conventional HPT of an initially coarse-grained material are presented. The treatment of nanocrystalline nickel by HPT was established to retain a nanometer average grain size (30–40 nm), substantially (by a factor of 2–3) decrease internal stresses, and lead to the formation of a fundamentally new crystallographic texture type differing from the previously revealed type of the shear textures characteristic of the HPT samples prepared from coarse-grained samples.