XPS Studies on Electroless As-Deposited and Annealed Ni-P Films

Electroless deposition has been used to deposit Ni-P films on glass slides using the reducing agent sodium hypophosphite. This has been done with a purpose to use Ni-P films as back contact for silicon carbide radiation detectors. By keeping deposition time, temperature, pH and concentration of the precursor solution constant, the film deposition has been done. XPS studies were done to analyze the composition and stoichiometry of Ni-P thin films.

Microstructure and depositional mechanism of Ni-P coatings with nano-ceria particles by pulse electrodeposition

Nano-CeO2 （RE） particles were co-deposited into Ni-P binary composite coatings by applying pulse current （PC） under ultrasonic （U） field. Morphology, chemical content and crystal microstructure were characterized by environmental scanning electron microscopy （E-SEM） with energy dispersive X-ray analysis （EDXA）, XRD diffractometry and transmission electron microscopy （TEM）. Experimental results show that Ni-P coating reinforced with 15g/L nano-CeO2, in amorphous state and with compact structure, can be improved in the microhardness from HV0.2580 to HV0.2780 by annealing at 600 °C for 2 h. The highest content of codeposited Ce and deposition rate can reach 2.3% and 68 μm/h, respectively. Furthermore, the effect of RE adsorption and pulse overpotential on depositional mechanism was investigated. n-CeO2 particles or Ce4＋ ions with strong adsorption capacity acted as the catalytic nucleus to improve densification effectively. During annealing at 600 °C for 2 h, n-CeO2 particles will uniformly adsorb on crystal grain to preferentially pad and heal up gaps of cracking Ni boundaries, promoting dispersion strengthening with refiner-grained structure.

An in situ measure method to study deposition mechanism of electroless Ni-P plating on AZ31 magnesium alloy

An in situ method was designed to measure a continuous open circuit potential （OCP） curve of AZ31 magnesium alloy and to observe the morphology variation of Ni-P coating during the process of the electroless plating. The deposition mechanism of the electroless Ni-P plating on AZ31 Mg alloy was studied by OCP curve, scanning electron microscopy （SEM）, and energy dispersion spectroscopy （EDS）. The process of electroless Ni-P plating contains the coating formation stage and the coating growth stage. The formation stage includes three procedures, i.e., the nucleation and growth of Ni crystallites, the extension of the coating in two-dimensional （2D） direction and the coalescence of the coating along three-dimensional （3D） direction. SEM investigations demonstrate that the spherical nodules of the Ni-P coating are not only formed during the coating growth stage, but also generated in the initial deposition stage of electroless Ni-P plating. The variation of the coating rates at different deposition stages corresponds to the deposition mechanism of their respective deposition stage.

EFFECTS OF DEPOSITION PROCESS ON PHOSPHORUS CONTENT IN ELECTROLESS Ni－P COATINGS

There are many factors that affect the phosphorus content in the electroless Ni-P coatings The effects of the compositions of plating solution,the PH values of plat ing solution and the deposition temperature on the phosphorus content in Ni-P coatings were investigated in this paper It is found that the phosphorus content in Ni-P coatings increases and the deposition rate decreases with decreasing PH values,nickel sulphate NiSO4 content of plating solution and the deposition temperature.

Effect of wear conditions on tribological properties of electrolessly-deposited Ni-P-Gr-SiC hybrid composite coating

The friction and wear properties of the electrolessly-deposited Ni-P-Gr-SiC composites were investigated. The effects of graphite content, load and rotation speed on the friction coefficient and wear resistance of the composite coatings were mainly investigated. The worn surface and cross section of the coatings were characterized by scanning electron microscopy and energy-dispersive X-ray analysis. The results show that the composite coatings reveal good antifriction and wear resistance due to the synergic effect of graphite and SiC particles. The formation of graphite-rich mechanically mixed layer （GRMML） on the surface of Ni-P-Gr-SiC coating contributes to the good tribological behavior of the wear counterparts and SiC particles play a load bearing role in protecting GRMML from shearing easily.

Characteristics of microstructure and performance of laser-treated electroless Ni-P/Ni-W-P duplex coatings

Characteristics of microstructures of electroless Ni-P/Ni-W-P duplex coatings were investigated using SEM/EDX and XRD analysis techniques. Microhardness and wear behaviour of the coatings before and after laser crystallization were evaluated by measurements of hardnesses of coating surface and cross-section, and by unlubricated friction and wear experiments. The results indicate that it is possible to prepare electroless Ni-P/Ni-W-P duplex coatings by sequential immersion in two different plating baths. After laser crystallization, the microstructures of electroless Ni-P/Ni-W-P duplex coatings present the characteristics of higher degree of crystallization and larger grain size for outer layer Ni-W-P than inner Ni-P, but outer layer has a higher hardness. The wear resistance of laser-treated duplex coatings in a given process parameter conditions is superior to the as-plated ones. Laser treatment was performed directly in air without argon protection, which provides the possibility for application of industrialized production.

Mechanical assisted electroless barrel-plating Ni-P coatings on magnesium alloy

A mechanically assisted electroless barrel-plating Ni-P was carried out in a rolling drum containing Mg alloy specimens and ceramic balls, which was submerged in a bath containing electroless plating solution deposited by this novel technique have a It is demonstrated that the Ni-P coatings crystallized Ni-P solid solution structure, showing fine-grains, higher hardness, and higher corrosion resistance compared with the conventional electroless plated amorphous Ni-P coatings. After heat treatment at 400 ℃ for 1 h, the structure of such Ni-P coatings were transformed to a structure with Ni-Ni3P double phases, and cracks in these coatings could not be observed, whereas cracks appeared seriously in the conventional electroless plated Ni-P coating after same heat treatment. Therefore, both hardness and corrosion resistance of these Ni-P coatings can be improved further by heat treatment. All of these beneficial effects can be attributed to the role of mechanical attrition during the mechanically assisted electroless barrel-plating process.

Microstructure and corrosion behavior of electroless deposited Ni-P/CeO_2 coating

Electroless Ni-P/nano-CeO2 composite coating was prepared in acidic condition, and its microstructure and corrosive property were compared with its CeO2-free counterpart. Scanning electronic microscopy （SEM） and X-ray diffraction （XRD） spectrometer were used to examine surface morphology and structure of the as-plated coating. Differential scanning calorimeter （DSC） and transmission electronic microscopy （TEM） were used to study the coating＇s phase change at high temperature. The coating＇s corrosive behavior in 3%NaCl ＋ 5%H2SO4 solution was also investigated. The results showed that Ni-P coating had partial amorphous structure mixed with nano-crystals, while the Ni-P/CeO2 coating had perfect amorphous structure. In high-temperature condition, Ni3P precipitation and Ni crystallization took place in both coatings but at different temperatures, while the Ni-P/CeO2 coating had sintered phase of NiCe2O4 spinels. The anti-corrosion property was better in the CeO2-containing coating, and this was due to its less liability to undergo local-cell corrosion than its CeO2-free counterpart. Ni-P/CeO2 coating＇s pure amorphous structure was the result of Ni＇s hindered crystal-typed deposition and P＇s promoted deposition.

Evaluation of residual stress and corrosion behaviour of electroless plated Ni-P/Ni-Mo-P coatings

Single Ni-P and Ni-Mo-P coatings as well as duplex Ni-P/Ni-Mo-P coatings with the same compositions were prepared by electroless plating.The residual stresses of the coatings on the surface and cross sections were measured by nanoindentation and AFM analysis,and the corrosion behaviour of the coatings in10%HCl solution was evaluated by electrochemical methods,to establish the correlation between the residual stresses and corrosion behaviour of the coatings.The results showed that the single Ni-P and duplex Ni-P/Ni-Mo-P coatings presented residual compressive stresses of241and206MPa respectively,while the single Ni-Mo-P coating exhibited a residual tensile stress of257MPa.The residual compressive stress impeded the growth of the pre-existing porosity in the coatings,protecting the integrity of the coating.The duplex Ni-P/Ni-Mo-P coatings had better corrosion resistance than their respective single coating.In addition,the stress states affect the corrosive form of coatings.

Fabrication of multi-shell coated silicon nanoparticles via in-situ electroless deposition as high performance anodes for lithium ion batteries

Si-based materials have been extensively studied because of their high theoretical capacity,low working potential,and abundant reserves,but serious initial irreversible capacity loss and poor cyclic performance resulting from large volume change of Si during lithiation and delithiation processes restrict their widespread application.Herein,we report the preparation of multi-shell coated Si(DS-Si)nanocomposites by in-situ electroless deposition method using Si granules as the active materials and copper sulfate as Cu sources.The ratio of Si and Cu was readily tuned by varying the concentration of copper sulfate.The multi-shell(Cu@CuxSi/SiO2)coating on Si surface promotes the formation of robust and dense SEI films and the transportation of electron.Thus,the obtained DS-Si composites exhibit an initial coulombic efficiency of 86.2%,a capacity of 1636 mAh g^-1 after 100 discharge-charge cycles at 840 mA g^-1,and an average charge capacity of 1493 mAh g^-1 at 4200 mA g^-1.This study provides a low-cost and large-scale approach to the preparation of nanostructured Si-metal composites anodes with good electrochemical performance for lithium ion batteries.

Erosion and Toughening Mechanisms of Electroless Ni-P-Nano-NiTi Composite Coatings on API X100 Steel under Single Particle Impact

The addition of superelastic NiTi to electroless Ni-P coating has been found to toughen the otherwise brittle coatings in static loading conditions, though its effect on erosion behaviour has not yet been explored. In the present study, spherical WC-Co erodent particles were used in single particle impact testing of Ni-P-nano-NiTi composite coatings on API X100 steel substrates at two average velocities—35 m/s and 52 m/s. Erosion tests were performed at impact angles of 30°, 45°, 60°, and 90°. The effect of NiTi concentration in the coating was also examined. Through examination of the impact craters and material response at various impact conditions, it was found that the presence of superelastic NiTi in the brittle Ni-P matrix hindered the propagation of cracks and provided a barrier to crack growth. The following toughening mechanisms were identified: crack bridging and deflection, micro-cracking, and transformation toughening.

Preparation and tribological performances of Ni-P-multi-walled carbon nanotubes composite coatings

Multi-walled carbon nanotubes （MWNTs） were wet-milled in the presence of ammonia and cationic surfactant and then used as reinforcements to prepare Ni-P-MWNTs composite coatings by electroless plating. The tribological performances of the composite coatings under dry condition were investigated in comparison with 45 steel and conventional Ni-P coating, Micrographs show that short MWNTs with uniform length and open tips were obtained through the wet-milling process. The results of wear test reveal that the Ni-P-MWNTs composite coatings posses much better friction reduction and anti-wear performances when compared with 45 steel and Ni-P coating. Within the MWNTs content range of 0.74%-1.97%, the friction coefficient and the volume wear rate of the composite coatings decrease gradually and reach the minimum values of 0.08 and 6.22x10-15 m3/（N.m）, respectively. The excellent tribological performances of the composite coatings can be attributed to the introduction of MWNTs, which play both roles of reinforcements and solid lubricant during the wear process.

Study of the Corrosion Resistance of Electroless Ni-P Deposits in a Sodium Chloride Medium

The corrosion resistance of electroless Ni-P deposits with phosphorous contents from 12% to 14% in sodium chloride solutions was studied. The deposits were immersed in 3.5% NaCl solutions for 29 d to obtain the electrochemical parameters and were examined in a standard salt spray test for 15 d respectively. The corrosion resistance of the deposits was studied by poten- tio-dynamic scan, electrochemical impedance spectroscopy (EIS), X-ray diffraction (XRD) and cold-field emission scanning electron microscopy (FE-SEM) equipped with an energy dispersive X-ray detector (EDX). The patterns of XRD and the results of FE-SEM showed that the prepared deposits were amorphous. But after a 15 d standard salt spray test, a few pinholes appeared on the surface of the deposit and the weight content of phosphorus on the surface of the deposit was higher (which was beneficial to the formation of the passivation films) than that before the standard salt spray test when the nickel content was lower because the dissolved weight of nickel was greater than that of phosphorus. The results from potentio-dynamic scan and EIS showed that passivation films formed on the Ni-P deposit after immersion in the NaCl solutions, which decreased the corrosion rate of Ni-P samples. The results of this work show their potential applications in marine corrosion.

Wear and Corrosion Resistance of Electroless Plating Ni-P Coating on P110 Steel

In order to improve the surface performance and increase the lifetime of P 110 oil casing tube steel during operation, electroless plating was conducted to form Ni-P coating onto its surface. The surface morphology/element distribution and phase constitution of the Ni-P coating were analyzed using scanning electron microscope （SEM） equipped with energy dispersive spectrometry （EDS） and X-ray diffraction （XRD）. Tribological and electrochemical measurement tests were applied to investigate the wear and corrosion resistance of P110 steel and the Ni-P coating. The results showed that a uniform and compact, high phosphorous Ni-P coating was formed. The obtained Ni-P coating indicated certain friction-reduction effect and lower mass loss during friction-wear tests. The Ni-P coating also exhibited higher corrosion resistance in comparison with bared P 110 steel. The obtained N i-P coating has significantly improved the surface performance of P110 steel.

Effect of Addition of Polytetrafluoroethylene (PTFE) and Silicon Carbide (SiC) on Properties of Electroless Nickel Alloy Coatings

Electroless nickel (copper)-phosphorus-silicon carbide (SiC)-polytetrafluoroethylene (PTFE) composite coatings were prepared by adding SiC and PTFE into electroless nickel (copper)-phosphorus alloy baths. The effects of addition of SiC and PTFE on depositing rate, microhardness, wear resistance and anti-friction of the resulted composite coatings were studied. The results indicated that electroless nickel (copper)-phosphorus alloy coatings were greatly improved in depositing rate, microhardness, wear resistance and antifriction by co-deposited proper amount of SiC and PTFE.

Electroless copper-phosphorus coatings with the addition of silicon carbide (SiC) particles

Cu-P-silicon carbide （SiC） composite coatings were deposited by means of electroless plating.The effects of pH values,temperature,and different concentrations of sodium hypophosphite （NaH2PO2·H2O）,nickel sulfate （NiSO4·6H2O）,sodium citrate （C6H5Na3O7·2H2O） and SiC on the deposition rate and coating compositions were evaluated,and the bath formulation for Cu-P-SiC composite coatings was optimised.The coating compositions were determined using energy-dispersive X-ray analysis （EDX）.The corresponding optimal operating parameters for depositing Cu-P-SiC are as follows：pH 9;temperature,90oC;NaH2PO2·H2O concentration,125 g/L;NiSO4·6H2O concentration,3.125 g/L;SiC concentration,5 g/L;and C6H5Na3O7·2H2O concentration,50 g/L.The surface morphology of the coatings analysed by scanning electron microscopy （SEM） shows that Cu particles are uniformly distributed.The hardness and wear resistance of Cu-P composite coatings are improved with the addition of SiC particles and increase with the increase of SiC content.

Effect of additives on nickel-phosphorus deposition obtained by electroless plating:Characterization and corrosion resistance in 3%(mass)sodium chloride medium

Nichel-phosphorus(Ni-P)coatings are deposited on mild steel by using an electroless plating process.The effect of three calix[4]arene derivatives,namely tetra methyl ester-P-tertbutyl calix[4]arene(Calix1),tetra acid-P-tert-butyl calix[4]arene(Calix2)and tetra methyl P-tert-butyl-thicalix[4]arene ester(Calix3)on the deposition rate,the deposit composition,and the morphological surface was investigated and the study of growth mechanisms has delivered useful information about the surface properties of deposit.It is found that these additives modify the deposition rate and the nickel crystallization process.In fact,the Calix1 and Calix3 act as an accelerator,while Calix2 acts as an inhibitor for the nickel electroless.Furthermore,it is shown that the chemical bath is more stable with calix[4]arene derivatives addition and the obtained deposits are compact and adherent.It is observed also that the nickel content increases with additives.On the other hand,the X-ray diffraction showed that the orientation peaks are intensified at{111}in the presence of Calix2,confirming obtained results of EDAX spectrum.The cyclic voltammetry revealed that the tested additives strongly influence the cathodic process and slightly affect the hypophosphite oxidation.Finally,it is found that these compounds improve the anticorrosion efficiency of Ni-P coating on the mild steel substrate in 3%(mass)NaCl,where its polarization resistance increases with Calix2 and Calix3 addition.

Electroless Ni-P plating on Mg-Li alloy by two-step method

Pretreated Mg-Li alloy sheets were pre-plated in a NiCO3？2Ni（OH）2？4H2O solution to form a thin Ni-P alloy film and then plating in a NiSO4？6H2O solution was carried out to obtain a protective coating.The surface morphology,structure and corrosion resistance of the coating were studied.The results showed that a flat,bright and compact plating layer,which was integrated into the matrix metal,was obtained.The P content of the Ni-P coating reached 13.56%（mass fraction）.The hardness value of the Ni-P coating was about HV 549.The polarization curve showed that the corrosion potential of the Ni-P coating reached ？0.249 V（vs SCE）.A long passivation region was found on the polarization curve,and this phenomenon indicated that the coating has an excellent anti-corrosion property.

Effect of novel ternary ligand system on acidic electroless Ni-P plating on AZ91D magnesium alloy

The electroless Ni-P coatings on AZ91 D magnesium alloy substrate were prepared using the acidic hypophosphite-reduced electroless nickel bath containing the novel ternary ligand system. The results indicate that the deposition rate varies with the ternary ligand concentration in plating solution. The structural and morphological characteristics of the coatings were analyzed by XRD and SEM. The anticorrosion properties of the Ni-P coatings were evaluated in 3.5% NaCl solution by electrochemical impedance and potentiodynamic polarization methods. The amount of ternary ligands in electroless plating bath has an significant effect on the surface morphology and structure of Ni-P coatings. The decrease of crystallization temperature and increase of crystallization heat of all the deposits with an increase in ternary ligand concentration are found by DSC measurements. The coating obtained with 0.035 mol/L ternary ligand additive in plating bath can offer a better surface homogeneity and improve corrosion resistance.

Structural characterization and corrosive property of Ni-P/CeO_2 composite coating

Electroless Ni-P/nano-CeO2 composite coating was prepared in acidic condition, and its microstructure and corrosive property were compared with its CeO2-free counterpart.Scanning electronic microscopy（SEM）, transmission electronic microscopy（TEM）, X-ray diffraction spectrometer（XRD）, and differential scanning calorimeter（DSC） were used to examine surface morphology and microstructure of the coating.Corrosive investigation was carried out in 3%NaCl＋5%H2SO4 solution.The results showed that Ni-P coating had partial amorphous structure mixed with nanocrystals, whereas the Ni-P/CeO2 coating had perfect amorphous structure.In high temperature condition, Ni3P precipitation and Ni crystallization occurred in both coatings but at different temperatures, whereas the Ni-P/CeO2 coating had sintered phase of NiCe2O4 spinels.The anticorrosion property and passivity were improved in the CeO2-containing coating due to its less liability to undergo local-cell corrosion than its CeO2-free counterpart.During the co-deposition process, some Cen＋（n=3, 4） ions may be adsorbed to the metal/solution interface, hinder nickel＇s crystal-typed deposition and promote phosphorous deposition.The nano-CeO2 doping finally resulted in the coating＇ perfect amorphous structure and good anti-corrosive property.