Electrochemical impedance studies of modified Ni-P and Ni-Cu-P deposits in alkaline medium

Ni-P and Ni-Cu-P deposits were supported over the commercial carbon using the electroless plating technique. The formed samples were characterized by applying SEM, XRD and EDX analyses. An amorphous Ni-P surface was obtained with 73.70 wt% Ni and 11.45 wt% P. The addition of copper to the plating bath reduces the deposited amount of nickel and phosphorus. The electrochemical performance of these deposits has been investigated in 0.1 M KOH solution using electrochemical impedance spectroscopy (EIS) measurements. The effect of pH, deposition time and temperature of the plating bath on the impedance characteristics of the two deposits was studied. It was found that the resistance (R_T) and relative thickness (1/C_T) of the two coatings in 0.1 M KOH solution increase with increasing either pH or deposition time or temperature of the plating bath. Our results indicate that Ni-Cu-P deposit has more corrosion resistance and lower corrosion current density (i_corr) value than Ni-P deposit under different conditions. EIS results were well confirmed by potentiodynamic polarization and cyclic voltammetry techniques.     

钨对化学镀Ni-W-P合金镀层结构及性能的影响

通过不同的化学镀工艺配方,获得了4种不同钨含量的化学镀Ni-W-P三元合金镀层.研究了钨含量对镀层结构、硬度及在5%H2SO4溶液中耐蚀性的影响规律.研究发现,化学镀Ni-W-P三元合金镀层的结构受镀层中钨含量的影响较大,非晶态Ni-W-P三元合金镀层所需磷含量较非晶态Ni-P二元镀层所需磷含量要低,并且钨含量越高,所需磷含量越少;镀层硬度随镀层结构从非晶态→混晶态→纳米晶态转变而增加;镀层的耐蚀性随镀层中钨含量增加而变好,且非晶态镀层较混晶态和纳米晶态镀层更易形成钝化区.     

化学镀Ni-W-P镀液及工艺优化研究

采用正交试验,以镀层的耐硝酸变色时间为评价标准,得到化学镀Ni—W—P溶液最佳配方为：20g／L硫酸镍、20g／L钨酸钠、20g／L次磷酸钠、40g／L络合剂、20g／L缓冲剂、pH值为60对该优化镀层的沉积速度、耐蚀性、孔隙率及结合力进行了测定,并与Ni—P二元合金镀层进行了比较。结果表明,该优化镀层的性能优于Ni—P二元合金。采用扫描电镜及X-射线衍射仪分别对该优化镀层的微观形貌、组成及结构进行的分析表明,该镀层结构致密,磷含量高达13.9％,且为非晶态结构。     

High corrosion resistance of electroless composite plating coatings on AZ91D magnesium alloys

The process of electroless plating Ni-P on AZ91D magnesium alloys was improved. The Ni-P-ZrO₂ composite coatings and multilayer coatings were investigated based on the new electroless plating process. The coatings surface and cross-section morphologies were observed with scanning electron microscopy (SEM). The chemical compositions were analyzed by EDXS. The corrosion behaviors were evaluated by immersion, salt spray and electrochemical tests. The experimental results indicated that the Ni-P-ZrO₂ composite coatings suffered attack in NaCl solution but displayed passivation characteristics in NaOH and Na₂SO₄ solutions. The corrosion resistance of Ni-P-ZrO₂ coatings was superior to Ni-P coatings due to the effect of ZrO₂ nano-particle. The multilayer coatings consisting of Ni-P-ZrO₂/electroplating nickel/Ni-P (from substrate to surface) can protect magnesium alloys from corroding more than 1000 h for the salt spray test.     

Vacuum thermal treated electroless NiP-TiO2 composite coatings

Composite NiP-TiO₂ layers were prepared by simultaneous electroless deposition of Ni-P and TiO₂ on steel substrate, from a solution in which TiO₂ particles were kept in suspension by stirring. Deposits were characterized for its structure, morphology and hardness. It was found that the chemical composition of Ni-P matrix has been influenced by the incorporation of TiO₂ particles. TiO₂ particle incorporation increases with increase in their bath concentrations (0.5-2.0 g/l). An improvement (up to 20%) in microhardness was observed in both as plated and vacuum heat-treated composite coatings compared to Ni-P coatings. Electroless deposited composite coatings exhibit an amorphous structure of the nickel matrix in which crystalline titanium oxide is incorporated. Vacuum heat treatment leads to the formation of a crystalline layer in which the Ni and Ni₃P crystallites appear apart from those of the TiO₂ (anatase). Potentiodynamic polarization measurements made on these deposits in 3.5 wt.% sodium chloride solution showed decrease in the corrosion resistance for the as-plated and heat-treated composite coatings.     

化学镀Ni-P-石墨复合镀层的特性

与化学镀Ni-P镀层比较,化学镀Ni-P-石墨复合镀层的机械性能得到了改进,适合于工程方面的应用。Ni-P-石墨复合镀层是从含有硫酸镍、次磷酸镍、丁二酸、表面活性剂和稳定剂的镀液中制备的。当镀液中石墨含量为15g/L时,镀层中石墨的复合量最大。采用维氏硬度测试仪、泰伯磨耗实验机、交流阻抗和SEM等手段对复合了石墨颗粒的Ni-P化学镀层进行了测定,其硬度,耐磨、耐蚀性随镀层中石墨含量的增加而增强。     

镍-磷-硫酸钡化学复合镀层的研制

在由硫酸镍31g/L、次磷酸钠22g/L、乙醇酸30g/L、乙酸钠13g/L、二甲胺0.8g/L、全氟乙基碘化铵0.1g/L及重晶石(即硫酸钡)0～25g/L组成的稳定镀液中,采用化学镀的方法在低碳钢上制备了Ni-P-BaSO4复合镀层.其表面形貌采用扫描电镜进行分析,耐蚀性以动电位极化及电化学阻抗谱测试.镍-磷合金基...     

稳定剂对化学镀镍液及镀层性能的影响

在前期确定的基础化学镀镍液配方基础上,分别添加KI、苯骈三氮唑、含硫有机杂环化合物A等稳定剂,考察了其对镀液的稳定性能、镀速、镀层性能等影响.优选了一种不仅能使镀液稳定性能良好,而且镀层耐蚀性能优异的药品A作为化学镀镍液的稳定剂.研究表明,合适的稳定剂在不改变镀层中磷含量的基础上,不但可以提高镀液的稳定性,同时还可获得高耐蚀性镀层.     

电路板化学镀镍液EN-600的研制

文章介绍一种用于电路板化学镀镍／沉金工艺的化学镀镍液EN-600。这种处理液采用独特的稳定体系,使镀液性能在寿命周期内保持稳定一致,同时能形成致密的镍磷合金层,增强镀层的耐蚀性,减少镍表面的过腐蚀,提高化学镀镍／沉金处理的良晶率。     

铝合金化学镀Ni-P合金的研究进展

本文分析了铝合金化学镀的特点,综述了铝合金化学镀Ni-P合金、Ni-W-P等三元合金、Ni-P/Ni-B双层复合镀及Ni-P-微粒化学复合镀的工艺流程及应用。     

Effect of Annealing Temperature and Alumina Particles on Mechanical and Tribological Properties of Ni-P-Al<Subscript>2</Subscript>O<Subscript>3</Subscript> Composite Coatings

In this study, the effect of annealing temperature and alumina particles on micro-hardness, corrosion, wear, and friction of Ni-P-Al₂O₃ composites coating is studied. The electroless nickel composite coating with various alumina particle content is deposited on a mild steel substrate. The corrosion behaviour and tribological behaviour (wear and friction) of the composite coated samples are investigated and compared with Ni-P coated samples. The micro-hardness, wear resistance, and corrosion resistance of the composite coating improved significantly after heat treatment (400 °C) and in the presence of alumina particles. The composite coating deposited with alumina particle concentration of 10 g/L in an electroless bath and heat treated at 400 °C shows excellent results compared to Ni-P, as-deposited Ni-P-Al₂O₃ coating and coatings heat treated at different annealing temperature (200 °C, 300 °C, and 500 °C). Microstructure changes and composition of the composite coatings due to incorporation of alumina particles and heat treatment are studied with the help of SEM (scanning electron microscopy), EDX (energy dispersive X-ray analysis and XRD (X-ray diffraction analysis).     

Effect of electroless nickel interlayer on the electrochemical behavior of single layer CrN, TiN, TiAlN coatings and nanolayered TiAlN/CrN multilayer coatings prepared by reactive dc magnetron sputtering

The electrochemical behavior of single layer TiN, CrN, TiAlN and multilayer TiAlN/CrN coatings, deposited on steel substrates using a multi-target reactive direct current (dc) magnetron sputtering process, was studied in 3.5% NaCl solution. The total thickness of the coatings was about 1.5 μm. About 0.5 μm thick chromium interlayer was used to improve adhesion of the coatings. With an aim to improve the corrosion resistance, an additional interlayer of approximately 5 μm thick electroless nickel (EN) was deposited on the substrate. Potentiodynamic polarization and electrochemical impedance spectroscopy (EIS) were used to study the corrosion behavior of the coatings. Scanning electron microscopy and energy dispersive X-ray analysis were used to characterize the corroded samples. The potentiodynamic polarization tests showed lower corrosion current density and higher polarization resistance (R_p) for the coatings with EN interlayer. For example, the corrosion current density of TiN coated steel was decreased by a factor of 10 by incorporating 5 μm thick EN interlayer. Similarly, multilayer coatings of TiAlN/CrN with EN interlayer showed about 30 times improved corrosion resistance as compared to the multilayers without EN interlayer. The porosity values were calculated from the potentiodynamic polarization data. The Nyquist and the Bode plots obtained from the EIS data were fitted by appropriate equivalent circuits. The pore resistance (R_pore), the charge transfer resistance (R_ct), the coating capacitance (Q_coat) and the double layer capacitance (Q_dl) of the coatings were obtained from the equivalent circuit. Multilayer coatings showed higher R_pore and R_ct values as compared to the single layer coatings. Similarly, the Q_coat and Q_dl values decreased from uncoated substrate to the multilayer coatings, indicating a decrease in the defect density by the addition of EN interlayer. These studies were confirmed by examining the corroded samples under scanning electron microscopy.     

Studies on electroless Ni-P-Cr_2O_3 and Ni-P-SiO_2 composite coatings

本文对化学镀镍及化学镀镍磷基质中SiO2与Cr2O3的共沉积进行了研究。微粒在不断生长的膜层中共沉积引起了新的化学复合镀层的出现,这些复合镀层许多都具有优异的耐磨及耐蚀性能。通过选取镀层合金/复合微粒/金属基体的组分可改进镀层,获得所需的性能,以满足特别的需求。在对这些复合镀层的应用需求正在迫近与增长的同时,其市场正在迅速扩张。本文开发出了一种合适的复合化学镀镍液,并通过维氏硬度法对化学复合镀镍层进行了表征。采用动电位极化及交流阻抗法测定了镀层的Taber耐磨性能及耐蚀性能。采用SEM及XRD对复合镀层的表面形貌进行了分析。     

镍钨磷非晶态合金电刷镀工艺研究

在Ni-P电刷镀工艺的基础上,研究和开发了Ni-W-P电刷镀工艺,镀液中加入钨酸盐。通过试验确定各组分的含量及工艺条件。镀层测试结果表明：Ni-W-P镀层为非晶态镀层,硬度高、耐腐蚀性能好,并具有良好的结合力。可用于工、模具的修复。     

化学镀Ni-P-Cr2O3和Ni-P-SiO2复合镀层的研究

本文对化学镀镍及化学镀镍磷基质中SiO2与Cr2O3的共沉积进行了研究.微粒在不断生长的膜层中共沉积引起了新的化学复合镀层的出现,这些复合镀层许多都具有优异的耐磨及耐蚀性能.通过选取镀层合金/复合微粒/金属基体的组分可改进镀层,获得所需的性能,以满足特别的需求.在对这些复合镀层的应用需求正在迫近与增长的同时,其市场正在迅速扩张.本文开发出了一种合适的复合化学镀镍液,并通过维氏硬度法对化学复合镀镍层进行了表征.采用动电位极化及交流阻抗法测定了镀层的Taber耐磨性能及耐蚀性能.采用SEM及XRD对复合镀层的表面形貌进行了分析.     

Microstructure and electrochemical characterization of trivalent chromium based conversion coating on zinc

A trivalent chromium based conversion coating (CCC), based on chromium nitrate solution with Co(II) ions, was developed on Zn substrate. The corrosion resistance of the trivalent CCC, measured in deaerated pH 8.0 borate buffer + 0.01 M NaCl solution using anodic polarization and electrochemical impedance spectroscopy (EIS), was very sensitive to both immersion time and bath pH. Micro-cracks were found on the surface of the CCC. Besides, the density of micro-crack and the coating thickness also depended on immersion time and bath pH. With increasing the coating thickness its pitting potential increased and passive current density decreased. The trivalent CCC formed on Zn for 40 s in pH 1.7 bath showed the best corrosion resistance, and the pitting potential increased significantly from −355 mV_SCE for Zn to 975 mV_SCE for the trivalent CCC on Zn. To explain the corrosion behavior of the trivalent CCC using EIS analysis, a modified equivalent circuit, which considered the micro-cracks in the coating and chromium corrosion product (CCP) deposited in the micro-cracks, was designed and the variation of each electrical parameter was examined. Especially, its corrosion behavior was well described by the variation of the resistance of CCP (R_ccp).     

Fabrication of Ni-W-B4C composite coatings and evaluation of its micro-hardness and corrosion resistance properties

Boron carbide (B₄C) particles were embedded in nickel-tungsten (Ni-W) coatings by pulse current electrodeposition technique. Physical properties of the composite coatings were studied by XRD, SEM, EDS and Vickers micro-hardness instrument. Corrosion protection of the deposited films was investigated utilizing potentiodynamic polarization and Electrochemical Impedance Spectroscopy (EIS). Results exhibited that the addition of B₄C nanoparticles into the Ni-W alloy can significantly improve the surface morphology and the micro-hardness of the composite coatings. The corrosion resistance of Ni-W-B₄C nanocomposite is much better than Ni-W alloy deposit, especially when the concentration of B₄C nanoparticles is 2?g/L in plating bath, the obtained Ni-W-B₄C composite coating has the best surface morphology, the highest micro-hardness and the excellent corrosion resistance.     

Composite Ni/Al2O3 coatings and their corrosion resistance

Composite coatings Ni/Al₂O₃ were electrochemically deposited from a Watts bath. Al₂O₃ powder with particle diameter below 1 μm was codeposited with the metal. The obtained Ni/Al₂O₃ coatings contained 5-6% by weight of corundum. The structure of the coatings was examined by scanning electron microscopy (SEM). It has been found that the codeposition of Al₂O₃ particles with nickel disturbs the nickel coating's regular surface structure, increasing its microcrystallinity and surface roughness. DC and AC electrochemical tests were carried out on such coatings in a 0.5 M solution of Na₂SO₄ in order to evaluate their corrosion resistance. The potentiodynamic tests showed that the corrosion resistance of composite coating Ni/Al₂O₃ is better than that of the standard nickel coating. After 14 days of exposure the nickel coating corrodes three times faster than the Ni/Al₂O₃ coating. The electrochemical behaviour of the coatings in the corrosive solution was investigated by electrochemical impedance spectroscopy (EIS). An equivalent circuit diagram consisting of two RC electric circuits: one for electrode, nickel corrosion processes and the other for processes causing coating surface blockage, were adopted for the analysis of the impedance spectra. The changes in the charge transfer resistance determined from the impedance measurements are comparable with the changes in corrosion resistance determined from potentiodynamic measurements.     

化学镀镍技术在电子工业的应用

化学镀镍层具有耐蚀性好、耐磨性高、焊接性良好、磁性可调等优点。因此,化学镀镍技术被广泛应用于电子工业。文章概述了化学镀镍的原理、常用的化学镀镍-磷合金工艺配方及各成分的作用,简述了化学镀镍技术在PCB制造、电子封装、电子元件制造、电磁屏蔽等领域的应用,介绍了近年来的化学镀镍新技术,并指出了今后化学镀镍技术的研究重点。     

Preparation and characterization of a double-layer coating on magnesium alloy AZ91D

A double-layer coating was prepared on AZ91D alloy by plasma electrolytic oxidation (PEO) plus electroless plating (EP). The plasma eletrolytic oxidation film was prepared in a silicate bath as an inner layer of the coating. Electroless plated Ni-P layer grew from the pores of the PEO film in a nickelous acetate bath and formed as the outer layer of the coating. The microstructure and crystallographic structure was observed with FESEM and XRD. The corrosion resistance of the double-layer coating was evaluated by means of chronopotentiometric (E-t), potentiodynamic polarization (E-i), neutral salt spray test and electrochemical impedance spectroscopy (EIS) test. Compared with the data of as-cast AZ91D magnesium, the open circuit potential of the double-layer coated AZ91D alloy increased by 1.1815 V, while the self-corrosion current density decreased by two orders of magnitude. E-i, EIS result showed that the corrosion resistance of magnesium alloy AZ91D was improved by the double-layer coating. The salt spray test and polarization test results show that the pitting corrosion resistance of AZ91D alloy was improved greatly. An equivalent circuit was proposed to fit the impedance diagrams of AZ91D alloy with the coating.