PREPARATION AND ANALYSIS OF Ni-P-Zn ELECTROLESS DEPOSITION FROM ALKALT BATH

Electroless Ni-P-Zn alloys deposited from alkali bath were investigated in this paper. The deposition bath contained nickel sulfate, zinc chloride and hypophosphate. The process parameters, such as temperature, pH and zinc salt concentration were presented and discussed.The microstructure of the coatings was studied by XRD and SEM. The cathode glowing discharge characters of Ni-P-Zn depositions were studied with luminous Neon lamps. Electrodes deposited by electroless Ni-P alloys were apt to sputter during luminous working hours. Electroless Ni-P-Zn depositions improved the discharge characters of the electrodes.With the concentration of zinc in the deposition rising to 4wt%, electrode sputter was largely restrained. The thickness of the deposition also influenced the discharge characters of the electrode. To avoid electrode sputter, the concentration of zinc has to rise with the thickness of the depositions.     

Effects of rare earth cerium addition on the synthesis and corrosion resistance of electroless Ni–PTFE–P coating

Electroless Ni–PTFE–P coatings have been successfully deposited on the surface of mild steel shaft from plating baths containing various concentrations of rare earth metal cerium (RE Ce). Surface morphology, Ce fraction, and thickness of the coatings were characterized by scanning electron microscope, inductively coupled plasma optical emission spectrometry, and reflection optical microscope, respectively. Salt spray test was used to determine the corrosion resistance of the coating. Results revealed that structure, compactness, and deposition rate of the Ni–PTFE–P coatings were increased significantly by addition of a small amount of RE Ce (10–20 ppm) to the plating bath. Electroless Ni–PTFE–P coating deposited from plating baths with 20 ppm Ce shows the highest corrosion resistance, owing to its high compactness and thickness. Deposition rate and corrosion resistance of the Ni–PTFE–P coating were deteriorated greatly as concentration of RE Ce in the plating baths exceeds 100 ppm.     

Electrochemical deposition of nanocrystalline zinc on steel substrate from acid zincate bath

Nanocrystalline zinc coatings were deposited from acid zincate bath containing newly synthesized condensation product. The effect of bath constituents, pH, temperature and current density on the deposit nature were investigated through Hull cell experiments. Current efficiency, throwing power, cathodic polarization and corrosion behavior in 3.5 wt.% NaCl were studied under optimum concentration of additives. Salt spray test and electrochemical measurements showed that nanocrystalline zinc coatings have better corrosion resistance than the zinc coatings deposited from a simple acid zincate bath without additive. The surface morphology and thickness (cross section) of the zinc deposits were studied by scanning electron microscopy (SEM). The preferred orientation and average grain size of the zinc electrodeposit were obtained by X-ray diffraction analysis. The particle size was also characterized by TEM analysis. Energy X-ray diffraction (EDX) and FT-IR spectral analysis were carried out to determine the inclusion of addition agent in the deposit. The experimental results indicated that the addition of condensation product of thiamine hydrochloride (THC) and furfural (FFL) leads to a more uniform nanocrystalline deposition with the grain sizes varying from 20-22 nm.     

工艺参数对连续碳纤维表面电磁搅拌化学镀镍的影响

目的解决连续碳纤维在镀覆过程中易出现黑心现象以及无法完全浸泡于镀液中的问题,制备镀层均匀的连续碳纤维镍镀层。方法引入外加电磁搅拌对连续碳纤维进行化学镀镍,研究了施镀时间、镀液温度、镀液pH值以及电磁搅拌转速对连续碳纤维表面微观形貌及镀层沉积速率的影响规律。结果当搅拌转速一定时,随着施镀时间、镀液温度、镀液pH值的不断增加,碳纤维表面镀层逐渐变得均匀完整,且镀层厚度逐渐增大。但当施镀时间超过20 min,镀液温度超过75℃,镀液pH值超过8时,镀层表面沉积了大量形状不一的胞状镍颗粒,形成粗糙的表面形貌。镀层的沉积速率随着镀液温度、镀液pH值的升高而增大。当搅拌转速由200 r/min增加到300 r/min时,镀层的沉积速率随着搅拌转速的增加而不断增大;当搅拌转速由300 r/min增加到400 r/min时,镀层的沉积速率随着搅拌转速的增加而不断减小。结论电磁搅拌辅助连续碳纤维化学镀镍的最佳施镀工艺参数为:施镀时间15~20 min,镀液温度75℃,镀液pH为8,搅拌转速200~250 r/min。采用此工艺参数能获得表面致密、均匀完整的镍镀层。     

Electroless cobalt deposition from a glycinate solution using morpholine borane as a reducing agent

Electroless cobalt films were deposited from a neutral pH glycinate solution without additives using morpholine borane (MB) as a reducing agent. The rate of deposition rises with increase in concentration of solution components (Co ions, MB and glycine), and pH. The efficiency of cobalt discharge increases when the deposition is performed from the Co(II) complex with glycine. XPS data indicate that boron and oxygen are incorporated into the cobalt films. Two forms of boron (elemental and its oxide) were detected in the electrolessly deposited cobalt films.     

Combination of zinc alloy coating with thin plasma polymer films for novel corrosion protective systems on coated steel

Steel sheet used in automotive applications has to be corrosion protected effectively, which is usually realized by zinc or zinc alloy coatings with a thickness range of 5–10 μm. Steel sheet for areas of a car body which are exceptionally stressed by corrosion, e.g. cavity flanges or joints, may be protected additionally by a thin weldable organic coating with a thickness of 2–4 μm. A very promising approach to a significantly reduced use of resources is the combination of zinc alloy coatings with thin plasma polymer films deposited by means of plasma-enhanced chemical vapour deposition (PECVD). Such plasma polymer films of just a few 100 nm thickness show excellent barrier and adhesion properties as well as a high mechanical stability.Within this work thin plasma polymer films were deposited on zinc alloy coated steel substrates using the strip hollow cathode (SHC) method, which was modified for application on grounded substrates. A pulsed DC glow discharge in a mixture of argon and an organosilane precursor was used for the deposition of films with a thickness of 100–500 nm.The chemical compositions of the coatings were determined by means of X-ray photoelectron spectroscopy and Fourier transform infrared spectroscopy. The morphologies of the coating systems were studied by means of scanning electron microscopy. The performance of the coating systems has been studied in different specific tests of corrosion and processing behaviour. The investigated coating systems show a corrosion resistance comparable to reference samples of electro-galvanised steel sheet with additional organic coating even with a coating thickness less of half of the reference samples.     

Role of Thiamine Hydrochloride and Gelatin on the Electrodeposition of Zinc

A search for a non-cyanide zinc plating bath resulted on the development of a zinc acetate bath. To obtain bright zinc deposits, thiamine hydrochloride and gelatin were added. Hull cell studies revealed that in presence of 3 g dm^?3 thiamine hydrochloride a bright deposit was obtained at a current density above 2.5 A dm^?2. Addition of 3 g dm^?3 gelatin produced a bright yellow tinge deposit above 2.5 A dm^?2. Voltammetric studies carried out at a glassy carbon electrode in the plating solution revealed that in the pH range of 4.5-5.5, zinc acetate complexes underwent successive reduction to zinc. Acetate ions and pH affected both the dissolution and deposition of zinc. The dissolution of zinc took place with the participation of OH^? ions. Gelatin molecules adsorbed on the electrode surface. They favoured both zinc dissolution and deposition and prevented hydrogen evolution in the potential range of interest. Thiamine hydrochloride caused a reduction in zinc dissolution and deposition rates but favoured hydrogen evolution.     

PET表面化学镀Ni-P合金工艺的研究

研究了在PET表面化学镀Ni-P合金的工艺,结果表明:实验选定的粗化时间对镀层形貌,镀速没有明显的影响;活化时间影响镀速,时间的增加镀速加快;施镀时间增加,镀层厚度增加,但平均镀速下降;镀槽温度增加,明显增加施镀速度。     

Improvement of a-C:H film adhesion by intermediate layers and sputter cleaning procedures on stainless steel, alumina and cemented carbide

The adhesion of amorphous hydrogenated carbon (a-C:H) films deposited in a radio frequency (r.f.) plasma discharge on stainless steel, alumina and cemented carbide with different intermediate layers (Ni, Ti and TiC) and sputter cleaning procedures was studied. The composition of the carbon films and the intermediate layers as well as the interface between the coating and the substrate was determined by secondary ion mass spectroscopy (SIMS). The adhesion experiments were carried out using a scratch tester. Tested specimens were also studied by scanning electron microscopy (SEM) to reveal the morphology of the coatings and the scratches.

Without any intermediate layer, the a-C:H coatings generally had insufficient adhesion to the substrate materials studied. For stainless steel and cemented carbide substrates, the TiC intermediate layer and, for alumina substrates, the titanium intermediate layer gave the best adhesion values evaluated by the scratch test. Also, the sputter cleaning of the substrates prior to deposition was necessary for sufficient adhesion of the coating. The intermediate layers also change the failure mode of the coating in the scratch test in some cases.     

一种电火花沉积接触力自动控制装置和沉积试验

为了研究接触力对电火花沉积过程的影响,设计了一种电火花沉积接触力自动控制装置,进行了不同接触力下的自动沉积试验,分析了不同接触力下的沉积效率、质量转移效率、沉积层表面形貌和各种放电波形的数量等.结果表明,接触力为1.0 N时,取得了较大的沉积效率和质量转移效率,沉积层的表面质量也较好.设计的电火花沉积接触力自动控制装置...     

Study of structure development of Titanium Nitride on inclined substrates

For magnetron sputter deposited coatings, the structure development during growth mostly depends on the mobility of the adatom over the substrate. The mobility is significantly affected by the orientation of the substrate with respect to the direction of the incident flux of sputtered atoms. The structural properties like crystallite size, crystallographic structure, column orientation, etc., are therefore influenced. This is relevant as the real work pieces over which the overlay functional coatings has to be applied are three dimensional in nature with the surfaces being off-normal to the incident flux. In the present investigation, the effect of incident angle on the various aspects of the structure development of Titanium Nitride coatings, having wide tribological applications, deposited on Si substrates by reactive magnetron sputter deposition was studied. A planar magnetron, with cathode diameter 75 mm and mounted with pure Ti target was used and TiN was deposited in a mixture of argon and nitrogen gas. The deposition was done for different durations. The deposited coatings were characterized using scanning electron microscopy (SEM) and X-ray diffraction (XRD). Results indicate the formation of well defined columnar microstructure in the coatings. The column inclination is compared with the well known ‘Tangent rule’.     

Co-development of stress and texture in reactive magnetron sputtered TiN films revealed by in situ film stress measurements

Titanium nitride (TiN) films up to 100 nm thickness were deposited by reactive magnetron sputter deposition on silicon substrates while measuring the film force in situ. The energy per deposited atom supplied to the growing film by ion bombardment was varied in two ways: a) by changing the deposition pressure and b) by changing the bias voltage applied to the substrate. Both variations affected the film force, the microstructure and the film texture. More energetic deposition conditions led to a continuous build up of stress, a dense microstructure and a 001 film texture almost independent of film thickness. These findings lead us to conclude that a 001 film texture is more susceptible to stress generation by an ion bombardment than a 111 film texture. Further, from the similar effect of a pressure increase and a bias voltage decrease on the film growth and characteristics we identify ion-neutral charge transfer collisions in the substrate sheath as the mechanism by which the deposition pressure influences film characteristics.     

Surface mechanical characterization of sputtered nickel using nanoindentation

The surface of carbon steel (CS) samples was deposited with pure Ni for the durations of 2, 5 and 10 minutes using DC magnetron sputter deposition process. The aim was to examine the microstructure and surface mechanical properties of Ni coatings. Field emission scanning electron microscope coupled with an energy dispersive x-ray spectrometer and x-ray diffractometer were used to undertake materials characterization. Instrumented nanoindentation hardness, elastic modulus, adhesion and coefficients of friction of coatings were evaluated. Nickel coatings obtained were relatively uniform, continuous and adherent for all deposition times. Thickness of Ni coatings increased with deposition times. Coatings with lower deposition times showed relatively higher nanohardness, elastic modulus and creep which is thought to be due to its lower thickness. Coatings were found to crack and delaminate at relatively low applied normal force during micro-scratch testing. Coefficient of friction values of coatings was comparable with that found in the literature.     

The Structure and Protective Properties of Zinc and Nickel Alternate Electrodeposits

A NEW TYPE of coatings consisting of a large numberof laminar deposits has been the keen subject of muchresearch,because these layered-structure coatingspossess improved properties or novel phenomenon suchas increased mechanical strength,micro-hardness,giantmagnetoresistance and corrosion resistance[1"6'.Thesecoating systems with individual layers making upoverall structure are also called compositionallymodulated multilayer(CMM)coatings'3"5'.In view ofthe plating historical use of surface…     

EFFECT OF ELECTROLESS DEPOSITION CONDITIONS ON THE STRUCTURES AND THE MAGNETIC PERFORMANCES OF THE Co-Fe-P ALLOY

Electroless Co-Fe-P alloys were deposited from an alkaline bath, containing boric acid as a buffer agent and sodium citrate as a complexing agent. As a result, with the increase of pH of the bath, the iron content of the deposit increased, whereas the cobalt and phosphorus contents decreased. The structure of the deposit was investigated using X-ray diffraction （XRD） and transmission electron microscope （TEM）. The deposit consisted of hexahedron phase Co, cubic phase Fe-Co, and amorphous phase （crystalline）. The magnetic performances of the deposit were studied using vibrating sample magnetometer （VSM）. The more the content of Fe and the less the content of P （the content of Co being less）, the better the magnetic performances of the deposit. The Co-Fe-P deposit was suitable for use as soft magnetic material.     

Comparative studies on the electroless deposition of Ni-P, Co-P and their composites with SiC particles

Electroless deposition of nickel and cobalt from alkaline baths as well as their codeposition with SiC particles were compared. It was found that despite similarity in properties of the metals their behavior in the electroless process was different. Maleic acid was used to stabilize plating baths, however the optimal concentration of the additive depended on the type of deposited metal. The electroless deposition characterized with low plating efficiency and it was higher for nickel than for cobalt. The composition as well as the morphology of Ni-P and Co-P deposits were also dissimilar. SiC particles inhibited the metal deposition, affected the plating potential, but did not alter the matrix composition. SiC entrapment was more preferential within the cobalt matrix than the nickel one. Some adsorption phenomena on SiC powder were also studied.     

氧化铝陶瓷基板化学镀铜工艺优化

目的化学镀铜是氧化铝陶瓷基板金属化的一种重要手段,为了进一步优化氧化铝陶瓷基板化学镀铜工艺,研究了化学镀铜液配比(尤其是镀液中铜离子和甲醛含量)对氧化铝陶瓷覆铜板微结构和导电性的影响。方法在对氧化铝陶瓷基板经过前期处理后,采用化学镀铜法在基板上镀铜。采用X射线衍射仪、光学显微镜对氧化铝基板上的化学镀铜层物相和形貌进行观察。采用覆层测厚仪、四探针测试仪对化学铜镀层的膜厚和方阻进行测量。结果 XRD结果表明,不同配比镀液得到的化学镀铜层均具有较好的晶化程度,镀液中甲醛和铜含量较低的镀液可制备出晶粒更为细小的化学镀铜层。甲醛和铜离子含量均较高时,沉积速度过快,使镀铜层的均匀性和致密性不佳。但当甲醛含量较高、铜离子含量较低时,沉积速度适中,从而获得了均匀性和致密性较好的镀铜层,同时这种镀层具有良好的导电性。结论采用表面活性化学镀铜工艺,当镀液中甲醛浓度为0.25 mol/L和硫酸铜质量浓度为1.2 g/L时,无需高温热处理,即获得了均匀性和致密性俱佳的铜镀层,可满足覆铜板的使用要求。     

Nanocrystalline zinc–nickel alloy deposition using pulse electrodeposition (ped) technique

Abstract

Zinc–nickel alloy was electrodeposited on stainless steel using pulse current deposition (PED) from a chloride–sulphate bath. Duty cycles were varied between 10 and 80% and frequency was changed from 10 to 100 Hz. The deposit characteristics were analysed using SEM, XRD and AFM and the results are presented in this paper. The corrosion resistance of zinc–nickel alloy deposited from direct current deposition (DCD) has been compared with that of the deposit obtained by pulse current using the electrochemical impedance spectroscopy method.     

Electrodeposition and Corrosion Resistance of Ni-Graphene Composite Coatings

The research on the graphene application for the electrodeposition of nickel composite coatings was conducted. The study assessed an important role of graphene in an increased corrosion resistance of these coatings. Watts-type nickel plating bath with low concentration of nickel ions, organic addition agents, and graphene as dispersed particles were used for deposition of the composite coatings nickel-graphene. The results of investigations of composite coatings nickel-graphene deposited from the bath containing 0.33, 0.5, and 1 g/dm³ graphene and one surface-active substance were shown. The contents of particles in coatings, the surface morphology, the cross-sectional structures of the coated samples, and their thickness and the internal stresses were studied. Voltammetric method was used for examination of the corrosion resistance of samples of composite coatings in 0.5 M NaCl. The obtained results suggest that the content of incorporated graphene particles increases with an increasing amount of graphene in plating bath. The application of organic compounds was advantageous because it caused compressive stresses in the deposited coatings. All of the nickel-graphene composite layers had better corrosion resistance than the nickel coating.     

The corrosion-protective traits of electroplated multilayer zinc-iron-chromium deposits

A novel kind of three-layer zinciron-cbromium electroplated coating was tested and proven to possess good corrosion protective characteristic as well as acceptable decorative properties. A citric-chloride bath containing Fe(III)-complexes is suggested for electrodeposition of iron intermediate layer on the zinc deposit surface. Due to the low acidity (pH 5) and medium operating temperature (20-30°C), the electrolyte involved has no a strong etching effect and can be used for direct iron deposition on zinc. A finish chromium layer is deposited from formate-sulfate trivalent bath. The zinc layer corrodes through the pores of Fe and Cr layers and protects the steel substrate against corrosion. The iron and chromium layers decelerate the corrosion rate of zinc. The finish chromium layer provides with good decorative properties, and the intermediate iron layer ensures adhesion of chromium to the zinc.