• Journal of the Korean institute of surface engineering
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• v.37 no.1
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• pp.40-48
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• 2004

Hardness and internal stress are very important in nickel electroforming. Nickel sulfamate bath has been widely used in electroforming because of its low internal stress and moderate hardness. Nickel sulfamate bath without chloride was chosen to investigated the effect of plating variable such as temperature, PH, current density and sodium naphthalene trisulfonate as addition agent on the hardness and internal stress. It was found that hardness increased with increasing temperature and decreasing current density and ranged from 150∼310 DPH. The hardness was highest at $55^{\circ}C$ and 10∼40 mA/$\textrm{cm}^2$. The internal stress increased with increasing current density and decreasing temperature. It was minimum at PH 3.0∼3.8. Low internal stress within $\pm$1,500 psi was obtained at both $50^{\circ}C$ and $55^{\circ}C$ in 10-20 mA/$\textrm{cm}^2$. The addition of sodium naphthalene trisulfonate was found to be effective in refine columnar grains thus resulted in decreasing internal stress, increasing hardness and improving brightness.

• Corrosion Science and Technology
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• v.13 no.3
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• pp.102-106
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• 2014

Nickel electrodeposition from sulfamate bath has several benefits such as low internal stress, high current density and good ductility. In nickel deposited layers, sulfur induces high temperature embrittlement, as Ni-S compound has a low melting temperature. To overcome high temperature embrittlement problem, adding manganese is one of the good methods. Manganese makes Mn-S compound having a high melting temperature above $1500^{\circ}C$. In this work, the mechanical properties of Ni-Mn deposited layers were investigated by using various process variables such as concentration of Mn$(NH_2SO_3)_2$, current density, and bath temperature. As the Mn content of electrodeposited layers was increased, internal stress and hardness were increased. By increasing current density, internal stress increased, but hardness decreased. With increasing the bath temperature from 55 to $70^{\circ}C$, internal stress of Ni deposit layers decreased, but hardness didn't change by bath temperature. It was likely that eutectoid manganese led to lattice deformation, and the lattice deformation increased hardness and internal stress in Ni-Mn layers. Increasing current density and decreasing bath temperature would increase a mount of $H_2$ absorption, which was a cause for the rise of internal stress.

• Journal of the Korean institute of surface engineering
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• v.53 no.1
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• pp.1-8
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• 2020

Sulfamate-chloride baths were fabricated to study the properties of the electrodeposited Ni and NiCo thin films. The dependences of current efficiency, deposit composition of Ni and Co, residual stress, surface morphology and microstructure of electrodeposited Ni and NiCo thin films on CoCl₂ concentration in sulfamate-chloride baths were investigated. The current efficiency was measured to be more than about 90%, independent of the changes of CoCl₂ concentration in the baths. Residual stress of Ni and NiCo thin films was increased from about 45 to about 250 MPa with varying CoCl₂ concentration from 0 to 0.210 M CoCl₂ in the baths and then reached to a plateau, about 250 MPa above 0.420 M CoCl₂ concentration. Nodular surface morphologies were observed at most CoCl₂ concentrations in the baths except 0.210 M. NiCo thin film electrodeposited from the bath with 0.210 M CoCl₂ concentration showed an acicular surface morphology. Pure Ni thin film consists of FCC(111), FCC(200), FCC(220), and FCC(311) peaks without any preferred orientation. On the other hand NiCo thin films make up of HCP(100), FCC(111), HCP(101), FCC(200), FCC(220) or HCP(110), FCC(311) or HCP(112) and FCC(222) peaks. It was revealed from the analysis of XRD result that FCC(111) peak at the NiCo thin film electrodeposited from the bath with 0.084 M CoCl₂ concentration can be regarded as the preferred orientation. However the peak of the preferred orientation was changed to FCC(220) or HCP(110) above 0.084 M CoCl₂ concentration in the baths. Then the intensity of FCC(220) or HCP(110) peak was gradually decreased with increasing CoCl₂ concentration further. The crystalline size of pure Ni thin film was observed to be about 53 ㎛ and those of NiCo thin films were in the range of 35~45 ㎛.

• Proceedings of the Korean Institute of Surface Engineering Conference
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• 1999.05a
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• pp.137-137
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• 1999

• Journal of the Korean institute of surface engineering
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• v.38 no.1
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• pp.14-20
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• 2005

The control of internal stress is extremely important in electroforming because of the deliberately low adhesion between the electro form and the mandrel. Excessive tensile or compressive stress can cause distortion, separation problem, curling, peeling or separation of electroform prematurely from the mandrel, buckling and blistering. Nickel sulfamate bath has been widely used in electroforming because of its low internal stress and moderate hardness. In this study, real-time stress sensor has been used for stress control in chloride-free nickel sulfamate bath for 400 mm x 300 mm x 500 ㎛ nickel electroform. It was found that compressive stress found at low current density indicated the contamination of electrolyte, which is very useful in procuring buckling and peeling of electroform. No compressive stress is allowed for plate electroform. The real-time stress can also be used for accurate stress control of nickel electroform. The tensile stress was found to be increased slightly with increase in nickel electroform thickness, i.e., from initial 1.47 ksi to 2.02 ksi at 320 ㎛.

• Journal of the Korean institute of surface engineering
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• v.39 no.1
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• pp.13-17
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• 2006

The effects of an organic additive, naphthalene trisulfonic acid (NTSA), contained in the nickel sulfamate bath on the surface properties of the electrodeposited nickel layer were investigated through electrochemical technique, x-ray diffraction analysis, and microscopic observation. The addition of NTSA facilitated the oxidation process of electrodeposited nickel layer during anodic scan and also increased the hardness and internal stress of the nickel film as the applied current density became higher. It seems that NTSA modulated the deposit structure during electrodeposition and so induced higher distribution of (110) orientation with respect to (200). With the increase of the NTSA in the bath, nickel layer was formed in small grain size, which resulted in enhanced surface evenness and brightness.

• Journal of the Korean institute of surface engineering
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• v.43 no.4
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• pp.165-169
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• 2010

$Ni-Al_2O_3$ nanocomposite coatings were fabricated by conventional electrodeposition technique using nickel sulfamate bath. Effect of plating parameters on electrodeposition of $Ni-Al_2O_3$ nanocomposite were studied. The properties of the nano composite were investigated by using SEM, XRD, and Vicker's microhardness test. The results demonstrated that $Al_2O_3$ incorporation in the composite coatings was found to be increased by increasing stir rate and $Al_2O_3$ content in plating bath. Microhardness of the composite coatings was also increased with increasing content of the nano particles in the plating bath. The surface morphologies of the nanocomposite coatings were found to be varied with varying pH, current densities as well as alumina content in the plating bath.

• Corrosion Science and Technology
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• v.3 no.3
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• pp.112-117
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• 2004

This work investigated the material properties of Ni-P-B alloy electrodeposits obtained from a Ni sulfamate bath as a function of the contents of the P and B sources($H_3PO_3$ and dimethyl amine borane complex(DMAB), respectively) with/without additives. Chemical composition, residual stress, microstructure and micro hardness were investigated using ICP(inductively coupled plasma) mass spectrometer, flexible strip, XRD, TEM and micro Vickers hardness tester, respectively. From the results of the compositional analysis, it was observed that P and B are incorporated competitively during the electrodeposition and the sulfur from the additive is codeposited into the electrodeposit. The measured residual stress value increased in the order of Ni, Ni-P, Ni-B and Ni-P-B electrodeposits indicating that boron affects the residual tensile stress greater than phosphorus. As the contents of the alloying element sources of P and B increased, crystallinity and the grain size of the electrodeposit decreased. The effect of boron on crystallinity and grain size was also relatively larger than the phosphorus. It can be explained that the boron with a smaller atomic radius contributes to the increase of residual stress in the tensile direction and the larger restraining force against the grain growth more significantly than the phosphorus with a larger atomic radius. Introduction of an additive into the bath retarded crystallization and grain growth, which may be attributed to the change of the grain growth kinetics induced by the additive adsorbed on the substrate and electrodeposit surfaces during electrodeposition.

• Journal of the Korean institute of surface engineering
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• v.51 no.1
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• pp.62-70
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• 2018

Sulfamate plating solution containing a small amount of chloride bath was fabricated to study the properties of the electrodeposited Ni thin films. Effects of the changes of current density and additive concentration on current efficiency, residual stress, surface morphology and microstructure of Ni thin films electrodeposited from Ni sulfamate-chloride baths were investigated. The current efficiency was measured to be more than about 95%, independent of the changes of current density and saccharin concentration in the baths. Residual stress of Ni thin film was appeared to be the compressive stress modes in the range of $5{\sim}30mA/cm^2$ current density. Maximum compressive stress was observed at the current density of $10mA/cm^2$. Compressive stress values of Ni thin/thick films were increased to be about -85~-100 MPa with increasing saccharin concentration from 0 to 0.0195 M(4 g/L). Surface morphology was changed from smooth to nodule surface appearance with increasing the current density. Smooth surface morphology of Ni thin films electrodeposited from the baths containing saccharin was observed, independent of the saccharin concentration. Ni thin/thick films consist of FCC(111), FCC(200), FCC(220), FCC(311) and FCC(222) peaks. It was revealed that the FCC(200) peak of Ni thin films is the preferred orientation in the range of $5{\sim}30mA/cm^2$ current density. The intensity of FCC(200) peak was gradually decreased and the intensity of FCC(111) peak was increased with increasing saccharin concentration in the baths.

• Journal of the Korean institute of surface engineering
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• v.50 no.1
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• pp.24-28
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• 2017

The electrodeposition of Ni-Co alloy from a sulfamate bath was investigated. The cobalt content in the Ni-Co deposits is more influenced by the temperature or stirring effect than the current density in the process parameters. As cobalt contents in the Ni-Co deposited layer increased from 0 wt.% up to 43 wt.%, hardness value of the layer rised from 400 Hv up to 700 Hv and crystal orientation (111) increased. However, (200) and crystal size significantly reduced. The tensile and yield strength also increased, while the modulus of elasticity showed the maximum value of $10.4N/mm^2$ at 29 wt.%.