Study of deposition patterns of plating layers in SiC/Cu composites by electro-brush plating

SiC reinforced copper composite coatings were prepared by electro-brush plating with micron-size silicon carbide (SiC) ranging from 1 to 5 μm on pure copper sheet in this paper. The micro-structural characterizations of SiC/Cu composite coatings were performed by optical microscope and Scanning Electron Microscope (SEM) coupled with spectrometer, to study co-deposition mechanism of SiC/Cu. It was found that there were three different patterns of SiC deposition in plating layers during electro-brush plating process, i.e. the particles could deposit inside copper grains, in grain boundaries, or in holes of the surface. To investigate deposition mechanism of each pattern, size of SiC and copper grains was compared. By comparison of size of copper grains and hard particles, SiC were either wrapped in copper grains or deposited in grain boundaries. Moreover, electro-brush plating layers at different brush velocities and current densities were obtained respectively, to analyze the microstructure evolution of the composite coatings. The hardness of plating layers was measured. The results indicated at the current density of 3 A/dm², the SiC/Cu coating was compact with SiC content at a high level and the hardness reached a maximum.     

Microstructure and surface mechanical properties of pulse electrodeposited nickel

The surface of carbon steel was modified by electrochemical deposition of Ni in a standard Watt's bath using dc and pulse plating electrodeposition. The aim was to compare the microstructure and surface mechanical properties of the deposit obtained by both techniques. Materials characterization was conducted using field emission scanning electron microscope fitted with scanning transmission electron detector, atomic force microscope and X-ray diffractometer. Nanoindentation hardness, elastic modulus, adhesion, coefficients of friction and wear rates were determined for both dc and pulse electrodeposits. Experimental results indicate that pulse electrodeposition produced finer Ni grains compared to dc plating. Size of Ni grains increased with deposition. Both dc and pulse deposition resulted in grain growth in preferred (2 0 0) orientation. However, presence of Ni (1 1 1) grains increased in deposits produced by pulse deposition. Pulse plated Ni exhibited higher hardness, creep and coefficient of friction and lower modulus of elasticity compared to dc plated Ni.     

Complete filling of 41 nm trench pattern using Cu seed layer deposited by SAM-modified electroless plating and electron-beam evaporation

To overcome the limitation of the sputtered Cu seed layer in electroplating of Cu interconnects imposed by the shadow effect, a new method for depositing a Cu seed layer on a 41 nm trench pattern based on combination of electroless plating (ELP) and electron-beam (E-Beam) evaporation was developed. A Cu seed layer formed by ELP alone was too thin to be used for electroplating due to its high resistivity. To solve this problem, an additional Cu layer was deposited on top of the trench by E-Beam evaporator to enhance the electrical conductivity of the Cu seed layer. The electrical resistivity of the resulting Cu layer was reduced to 4.8 μΩ cm, which was sufficient for the conductive seed layer for electroplating the 41 nm trench pattern. The gap-filling capability also improved and there were no voids or seams in the 41 nm trench pattern. The proposed method can be an effective solution for fabrication of a conductive seed layer to fill a 41 nm trench pattern by electroplating.     

Current density effect on magnetic properties of nanocrystalline electroplated Ni80Fe20/Cu composite wires

In developing high-sensitivity micro sensors for very weak magnetic field, extremely high permeability magnetic material is essential for the sensing element. In this study, the effect of plating current density in nanocrystalline electrodeposition of permalloy on the crystal grain size and consequently on the soft magnetic properties of the deposited layer of Ni₈₀Fe₂₀/Cu composite wire is investigated. It is found that the coercivity of the deposited Ni₈₀Fe₂₀ increases and the MI effect ratio of the Ni₈₀Fe₂₀/Cu wire decreases with increasing current density in the lower range of current density (0.6–2 A/dm²) while the opposite trend is observed as the current density range increases in a higher range (2–8 A/dm²). It seems that increasing plating current density has the effect of decreasing the crystal grain size of the plated material, resulting in lower coercivity of the plated material. This effect, due to decreased grain size, is dominating in the higher range of plating current density. However, it also has the effect of increasing residual stresses in the plated material, which is dominating in the lower range of plating current density, resulting in higher coercivity of the plated materials.     

制备铋靶的脉冲电镀工艺

 采用脉冲电镀工艺,以直径为1 mm的铜丝为芯轴,在无氰镀液体系中,制备出惯性约束聚变实验用铋靶所需的金属铋镀层。通过正交试验得到的最佳脉冲工艺条件为：电流密度5 A/cm²,频率600 Hz,占空比1∶6,温度20 ℃。利用扫描探针显微镜和扫描电子显微镜分别对铋镀层表面形貌进行分析,同时利用X射线衍射对铋镀层物相成分进行分析。表征结果表明：所得铋镀层表面细致均匀,孔隙率低,平整性好,无裂纹。     

Mechanical properties and wear and corrosion resistance of electrodeposited Ni-Co/SiC nanocomposite coating

Ni-Co/SiC nanocomposite coatings with various contents of SiC nano-particulates were prepared by electrodeposition in a Ni-Co plating bath containing SiC nano-particulates to be co-deposited. The influences of the nanoparticulates concentration, current density, stirring rate and temperature of the plating bath on the composition of the coatings were investigated. The shape and size of the SiC nano-particulates were observed and determined using a transmission electron microscope. The polarization behavior of the composite plating bath was examined on a PAR-273A potentiostat/galvanostat device. The wear behavior of the Ni-Co/SiC nanocomposite coatings was evaluated on a ball-on-disk UMT-2MT test rig. The worn surface morphologies of the Ni-Co/SiC nanocomposite coatings were observed using a scanning electron microscope. The corrosion behavior of the nanocomposite coatings was evaluated by charting the Tafel curves of the solution of 0.5 mol L⁻¹ NaCl at room temperature. It was found that the cathodic polarization potential of the composite electrolyte increased with increasing SiC concentration in the plating bath. The microhardness and wear and corrosion resistance of the nanocomposite coatings also increased with increasing content of the nano-SiC in the plating bath, and the morphologies of the nanocomposite coatings varied with varying SiC concentration in the plating bath as well. Moreover, the co-deposited SiC nano-particulates were uniformly distributed in the Ni-Co matrix and contributed to greatly increase the microhardness and wear resistance of the Ni-Co alloy coating.     

Studies on influence of zinc immersion and fluoride on nickel electroplating on magnesium alloy AZ91D

The effect of zinc immersion and the role of fluoride in nickel plating bath were mainly investigated in nickel electroplating on magnesium alloy AZ91D. The state of zinc immersion, the composition of zinc film and the role of fluoride in nickel plating bath were explored from the curves of open circuit potential (OCP) and potentiodynamic polarization, the images of scanning electron microscopy (SEM) and the patterns of energy dispersive X-ray (EDX). Results show that the optimum zinc film mixing small amount of Mg(OH)₂ and MgF₂ is obtained by zinc immersion for 30-90 s. The corrosion potential of magnesium alloy substrate attached zinc film will be increased in nickel plating bath and the quantity of MgF₂ sandwiched between magnesium alloy substrate and nickel coating will be reduced, which contributed to produce nickel coating with good performance. Fluoride in nickel plating bath serves as an activator of nickel anodic dissolution and corrosion inhibitor of magnesium alloy substrate. 1.0-1.5 mol dm⁻³ of F⁻ is the optimum concentration range for dissolving nickel anode and protecting magnesium alloy substrate from over-corrosion in nickel plating bath. The nickel coating with good adhesion and high corrosion resistance on magnesium alloy AZ91D is obtained by the developed process of nickel electroplating. This nickel layer can be used as the rendering coating for further plating on magnesium alloys.     

Electron microscopic study on interfacial characterization of electroless Ni-W-P plating on aluminium alloy

The interface between electroless plating Ni-W-P deposit and aluminium alloy (Al) matrix at different temperature heated for 1 h was studied using transmission electron microscope. The results show that the interface between as-deposited Ni-W-P deposit and Al matrix is clear. There are no crack and cavity. The bonding of Ni-W-P deposit and Al matrix is in good condition. The Ni-W-P plating is nanocrystalline phase (5-6 nm) in diameter. After being heated at 200 °C for 1 h, the interface of Ni-W-P deposit and Al matrix is clear, without the appearance of the diffusion layer. There exist a diffusion layer and educts of intermetallic compounds of nickle and aluminium such as Al₃Ni, Al₃Ni₂, NiAl, Ni₅Al₃ and so on between Ni-W-P deposit and Al matrix after being heated at 400 °C for 1 h.     

Preparation and wear resistance of pulse electrodeposited Ni-W/Al2O3 composite coatings

The aim of this work is to obtain the electroplating parameters for preparation of Ni-W/Al₂O₃ composite coating with high tungsten content, high micro-hardness and excellent wear resistance by pulse plating procedure. Our results showed that the duty cycle is a dominant parameter for the tungsten content in the coating and the tungsten content increases significantly with increasing duty cycle. The further analysis showed the great influence of tungsten content on micro-hardness of the coating. A maximum micro-hardness of about 859 Hv was obtained in pulse electrodeposited Ni-W/Al₂O₃ composite with tungsten content of 40 wt.% at a peak current density of 20 A/dm², a duty cycle of 80%, a pulse frequency of 1000 Hz and a particle loading of 10 g/L alumina in the plating bath. Although the hardness of Ni-W/Al₂O₃ composite coating was only slightly affected by the alumina content of the deposits prepared in present investigation, the alumina content effect on the tribological characteristic of Ni-W/Al₂O₃ composite coatings is significant. The friction coefficient was lowered to 0.25 and the wear loss was reduced to 1.05 mg by setting the control factors according to the values mentioned above for obtaining the coating with the highest micro-hardness.     

The characteristics of chromized 1020 steel with electrical discharge machining and Ni electroplating pretreatments

A uniform and continuous chromized coating on AISI 1020 steel is produced by low-temperature pack chromization (LTPC) with electrical discharge machining and Ni electroplating pretreatments. The anticorrosive performance of the chromized steels is investigated in a 0.5 M H₂SO₄ solution at room temperature. The testing results indicate that the chromized specimen with electrical discharge machining and Ni electroplating pretreatments exhibits the lowest corrosion current density, 2.16 × 10⁻⁸ A cm⁻², among the tested specimens. The corrosion resistance of all tested specimens are in the order of bare 1020 < 1020-Cr(700-2) < 1020-Ni-Cr(700-2) < 1020-EDM-Ni-Cr(700-2). Moreover, the 1020-Ni-Cr(700-2) specimen have the best conductivity as a result of the less amount of oxides in the superficial coating.     

Local electrical characteristics of passive films formed on stainless steel surfaces by current sensing atomic force microscopy

A current sensing atomic force microscope was used to study the topography and the local electronic properties of the passive film formed on a duplex ferrite-austenite stainless steel (Uranus 50). Comparison of current maps with topography AFM images reveals that the passive film covering austenite and ferrite phases exhibits different properties. On freshly formed passive film, a high and homogenous resistance (typically 10 GΩ for 1 V) characterises the film on austenite grains while current maps of the passive layer covering the ferrite grains show a high density of spots (few 100 MΩ for 1 V). Besides the current maps, local I-V curves acquired on austenite show wider band gap energy than the ones obtained on ferrite grains. Finally, the conductivity difference in passive films covering ferrite and austenite grains is discussed.     

Preparation and characterisation of electrodeposited amorphous Sn-Co-Fe ternary alloys

Electrochemical deposition was investigated as a process to obtain alloys of Sn-Co-Fe, which to date have not been reported in the literature. A constant current technique was used to electrochemically deposit tin-cobalt-iron alloys from a gluconate electrolyte. The gluconate system was chosen as an electrolyte, which could potentially provide an environmentally safe process. The effect of plating parameters such as current density, deposition time, temperature and pH are discussed. Results are reported for current density and plating time using an electrolyte temperature of 20-60 °C and pH of 7.0 in relation to phase composition, crystal structure and magnetic anisotropy of the deposited alloys.Investigations were conducted using ⁵⁷Fe conversion electron Mössbauer spectroscopy (CEMS), ¹¹⁹Sn CEMS, transmission Mössbauer Spectroscopy and XRD. The ⁵⁷Fe and ¹¹⁹Sn CEMS spectra and XRD showed that the dominant phase in the deposits was amorphous Sn-Co-Fe. The relative area of the 2nd and 5th lines of the sextets representing the magnetic iron containing phases was found to decrease continuously with increasing current density while at the same time no significant changes in the magnetic anisotropy was found with plating time. Magnetically split ¹¹⁹Sn spectra reflecting a transferred hyperfine field were also observed.A range of good quality amorphous Sn-Co-Fe ternary alloys was obtained over a range of operating conditions from an environmentally acceptable gluconate electrolyte.     

Preparation of pulse plated GaAs films

Thin GaAs films were prepared by pulse plating from an aqueous solution containing 0.20 M GaCl₃ and 0.15 M As₂O₃ at a pH of 2 and at room temperature. The current density was kept as 50 mA cm⁻² the duty cycle was varied in the range 10-50%. The films were deposited on titanium, nickel and tin oxide coated glass substrates. Films exhibited polycrystalline nature with peaks corresponding to single phase GaAs. Optical absorption measurements indicated a direct band gap of 1.40 eV. Photoelectrochemical cells were made using the films as photoelectrodes and graphite as counter electrode in 1 M polysulphide electrolyte. At 60 mW cm⁻² illumination, an open circuit voltage of 0.5 V and a short circuit current density of 5.0 mA cm⁻² were observed for the films deposited at a duty cycle of 50%.     

Effects of peak current density on the mechanical properties of nanocrystalline Ni-Co alloys produced by pulse electrodeposition

Cobalt content, grain size, microhardness and tensile strength of nanocrystalline Ni-Co deposits produced from a solution containing saccharin and cobalt sulfate at constant electrodeposition conditions (pulse on-time T_on at 1 ms and pulse off-time T_off at 15 ms) but varying the peak current density J_p were investigated. It is found that an increase in J_p makes the deposit Co content lower, colony-like morphology more obvious, grain size smaller, and hardness and tensile strength higher. All of the facts are believed to result from the higher overpotential and nucleation rates caused by the J_p increase. But its further increase could lead to reduction in the hardness and tensile strength. Peak current densities in the range of 100-120 A dm⁻² are recommended for the preparation of nanostructured Ni-Co alloy deposits with grain sizes in the range of 15-20 nm, containing 7-8% Co, possessing hardness of 590-600 kg mm⁻² and tensile strength of 1180-1200 MPa—significantly higher than the strength of pure nickel deposit which is produced by the similar method and gets similar grain size.     

Effect of pulse electrodeposition parameters on the properties of Ni/nano-SiC composites

Pure nickel and nickel matrix composite deposits containing nano-SiC particles were produced under both direct and pulse current conditions from an additive-free nickel Watts’ type bath. It has been proved that composite electrodeposits prepared under pulse plating conditions exhibited higher incorporation percentages than those obtained under direct plating conditions, especially at low duty cycles. The study of the textural perfection of the deposits revealed that the presence of nano-particles led to the worsening of the quality of the observed [1 0 0] preferred orientation. Composites with high concentration of embedded particles exhibited a mixed crystal orientation through [1 0 0] and [2 1 1] axes. The embedding SiC nano-particles in the metallic matrix by an intra-crystalline mechanism resulted in the production of composite deposits with smaller crystallite sizes and more structural defects than those of pure Ni deposits. A dispersion-hardening effect was revealed for composite coatings independently from applied current conditions. Pulse electrodeposition significantly improved the hardness of the Ni/SiC composite deposits, mainly at low duty cycle and frequency of imposed current pulses.     

Microstructure and mechanical properties of CrN films fabricated by high power pulsed magnetron discharge plasma immersion ion implantation and deposition

CrN films with strong adhesion with the substrate have been fabricated on Ti6Al4V alloy using novel plasma immersion ion implantation and deposition (PIII&D) based on high power pulsed magnetron sputtering (HPPMS). A macro-particle free chromium plasma is generated by HPPMS while the samples are subjected to high voltage pulses to conduct PIII&D. The CrN coatings have a dense columnar structure and low surface roughness. The grains in the films have the face-center cubic (fcc) structure with the (2 0 0) preferred orientation. An excellent adhesion is achieved with a critical load up to 74.7 N. An implantation voltage of 18 kV yields a hardness of 18 GPa and better wear resistance and a low friction coefficient of 0.48 are achieved.     

Characterization of Ti-Zr-N films deposited by cathodic vacuum arc with different substrate bias

Ti-Zr-N (multi-phase) films were prepared by cathodic vacuum arc technique with different substrate bias (0 to −500 V), using Ti and Zr plasma flows in residual N₂ atmosphere. It was found that the microstructure and mechanical properties of the composite films are strongly dependent on the deposition parameters. All the films studied in this paper are composed of ZrN, TiN, and TiZrN ternary phases. The grains change from equiaxial to columnar and exhibit preferred orientation as a function of substrate bias. With the increase of substrate bias the atomic ratio of Ti to Zr elements keeps almost constant, while the N to (Ti + Zr) ratio increases to about 1.1. The composite films present an enhanced nanohardness compared with the binary TiN and ZrN films deposited under the same condition. The film deposited with bias of −300 V possesses the maximum scratch critical load (L_c).     

Electrical properties and enhanced room temperature magnetoresistance in La0.7Ca0.2Sr0.1MnO3/Pd composites prepared by chemical plating

A series of bulk polycrystalline La_0.7Ca_0.2Sr_0.1MnO₃ (LCSMO)/Pd composites were prepared by chemical plating and structural, electrical, magnetic, and magnetoresistance (MR) properties were investigated. It is found that Pd additions are uniformly distributed on the grain boundaries of the LCSMO grains, which decrease the resistivity and the saturation magnetic moment of the matrix. An interesting phenomenon is observed that at a given field, when the plating time increases, the MR increases at low addition level (0>t (plating time)<40 min) and decreases at high addition level (t>40 min), indicating an optimal plating time of 40 min, at which the MR value is maximum. Our analysis suggests that the improvement of grain boundaries originating from Pd addition plays an important role in enhancing the MR.     

Effects of excessive grain growth on the magnetic and mechanical properties of hot-deformed NdFeB magnets

The magnetic and mechanical properties of rare-earth magnets hot-deformed at temperature range 750-950 °C have been investigated. The grains tended to grow excessively from dozens of nanometers to several microns at the temperatures above 850 °C. The alignment of grains was disrupted by the hot deformation at the high temperatures. The Nd-rich phase was extruded at the temperatures which are higher than 850 °C. The Nd-rich phase extrusion resulted in the reduction of density by 1% and the reduction of remanence from 1.42 to 0.72 T. The reduction of grain boundaries caused by flat platelet-shaped grains changing to spherical grains and the weak binding strength among large grains of Nd₂Fe₁₄B phase may be the main reasons for the low mechanical strength of hot-deformed magnets.     

Low-phosporous nickel-coated carbon microcoils: Controlling microstructure through an electroless plating process

Carbon microcoils (CMCs) have been coated with a nickel-phosphorus (Ni-P) film using an electroless plating process, with sodium hypophosphite as a reducing agent in an alkaline bath. CMC composites have potential applications as microwave absorption materials. The morphology, elemental composition and phases in the coating layer of the CMCs and Ni-coated CMCs were investigated by scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS) and X-ray diffraction (XRD), respectively. The effects of process parameters such as pH, temperature and coating time of the plating bath on the phosphorus content and deposition rate of the electroless Ni-P coating were studied. The results revealed that a continuous, uniform and low-phosphorous nickel coating was deposited on the surface of the CMCs for 20 min at pH 9.0, plating bath temperature 70 °C. The as-deposited coatings with approximately 4.5 wt.% phosphorus were found to consist of a mix of nano- and microcrystalline phases. The mean particle size of Ni-P nanoparticles on the outer surface of the CMCs was around 11.9 nm. The deposition rate was found to moderately increase with increasing pH, whereas, the phosphorous content of the deposit exhibited a significant decrease. Moreover, the material of the coating underwent a phase transition between an amorphous and a crystalline structure. The thickness of the deposit and the deposition rate may be controlled through careful variation of the coating time and plating bath temperature.