• Journal of Surface Science and Engineering
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• v.19 no.2
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• pp.31-43
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• 1986

The properties of the electroless nickel deposit mainly depends on the pH of the bath, the plating temperature, and the molar ratio of nickel to hypophosphite but they are also affected by its formulation and concentration of complexing and buffering agents. According to changeing the concentration of triethanolamine and boric acid, phosphorous contents, microsturcture, crystalline, hardness and wear resistance of deposits obtained from ammoniacal alkaline bath were investigated by EPMA, differential thermal analyser, X-ray diffractometer and wear tester. The results are as follows; (1) Increasing concentration of triethanolamine in the bath, the deposits is slightly inclined to increase its phosphorous content(3.7% P). (2) In the as-plated state, the deposits are not crystallized state but they are thermally unstable phase, and they are crystallized with precipitating $Ni_3P$ at 400$^{\circ}C$. (3) The deposit containing 2.3% P has higher hardness value in the as plated and heat treated state at below 300$^{\circ}C$ than those of 3.7% phosphorous deposit (1090Hk). But in the case of heat treating at 400$^{\circ}C$, the former has lower hardness value (1000Hk) than the latter and has remarkably Ni(III) orientation by heat treatment. (4) The 3.7% phosphorous deposit heat treated at 400$^{\circ}C$ has better wear resistance than hard chromium plating.

• Journal of Surface Science and Engineering
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• v.19 no.4
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• pp.140-148
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• 1986

Using sodium pyrophoshate as complexing agent, the characteristics and the magnetic properties of the films deposited from electroless cobalt plating bath have been studied. The result obtained are as following; 1. It was found that the optimum bath compositions consisted of 0.1M cobalt sulfate, 0.2M sodium hypophosphite as reducing agent, 0.4M sodium pyrophosphate as complexing agent and 0.5M ammonium sulfate as buffer agent, whereas good operating conditions were the bath of pH 10.5 adjusted with ammonia and 70$^{\circ}C$ of bath temperature, respectively. 2. The coercive force and the squareness of magnetic films were increased with deposition from the low temperature bath. 3. The phosphorous content in Co-P films deposited from these bath was relatively higher than that from Brenner bath. It was assumed to be due to codeposition of phosphorous from the pyrophosphate anion in the solution.

• Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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• 1999.05a
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• pp.708-711
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• 1999

The Cu/Ni/Au lamellar structure is extensively used as an under bump metallization on silicon file, and on printed circuit board(PCB) pads. Ni is plated Cu by either electroless Ni plating, or electrolytic Ni plating. Unlike the electrolytic Ni plating, the electroless Ni plating does not deposit pure Ni, but a mixture of Ni and phosphorous, because hypophosphite Is used in the chemical reaction for reducing Ni ions. The fracture crack extended at the interface between solder balls of plastic ball grid (PBGA) package and conducting pads of PCB. The fracture is duets to segregation at the interface between Ni$_3$Sn$_4$intermetallic and Ni-P layer. The XPS diffraction results of Cu/Ni/Au results of CU/Ni/AU finishs showed that the Ni was amorphous with supersaturated P. The XPS and EDXA results of the fracture surface indicated that both of the fracture occurred on the transition lesion where Sn, P and Ni concentrations changed.

• Proceedings of the KAIS Fall Conference
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• 2004.06a
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• pp.69-71
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• 2004

새로운 기술인 Momentary mold surface heating(MmSH)은 기존의 사출성형법으로 제조된 Acrylonitrile Butadiene Styrene(ABS)의 단점을 개선한 사출성형법이다. MmSH로 제조된 ABS와 기존의 사출성형법으로 제조된 ABS의 도금특성을 도금욕 pH 변화에 따라 연구하였다. Sodium hypophosphite가 첨가된 무전해 Ni 도금욕의 PH가 증가할수록 도금 두께가 증가하였고 기존의 사출성형법으로 제조된 ABS의 경우 pH 5이상에서 4B의 밀착력을 가졌다. MmSH로 제조된 ABS의 경우 pH 6이상에서 5B인 12.3N/25mm 이상의 가장 우수한 밀착력을 나타내었다.

• Resources Recycling
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• v.21 no.2
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• pp.41-46
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• 2012

An investigation on the recovery of nickel from spent electroless plating solutions has been performed using the electrowinning method. For this aim, nickel in spent electroless plating solutions was separated as nickel hydroxide through the addition of caustic soda. Nickel hydroxide was completely dissolved with sulfuric acid and an electrolysis was performed for electrowinning of nickel from nickel solutions. As a result, it was found that more than 99% of nickel in spent electroless plating solutions could be precipitated as nickel hydroxide above pH 10 with the addition of caustic soda. As far as the current efficiency in electrowinning of nickel was concerned, it was decreased with increase in the current density.

• Applied Chemistry for Engineering
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• v.26 no.3
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• pp.270-274
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• 2015

We develop advanced oxidation processes for the treatment of spent electroless nickel plating solution. Apart form recovering nickel by leaching and enrichment, more emphasis is placed on rendering the waste water recyclable via oxidizing phosphite and hypophosphite into phosphate which can then be precipitated easily. $UV/H_2O_2$ process is employed and the conversion efficiency of COD and $PO_4-P$, and $H_2O_2$ consumption are analyzed. Furthermore, the $UV/H_2O_2/O_3$ process in conjunction with $O_3$ generator enables us to not only save the treatment time by 6 hours but also reduce $H_2O_2$ consumption by 30%.

• Journal of environmental and Sanitary engineering
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• v.18 no.3 s.49
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• pp.35-42
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• 2003

The electric resistance and constant current were investigated on the nickel-thallium-phosphorus alloy deposits by electroless-plating. The Ni-Tl-P alloy deposits were achieved with a bath using sodium hypophosphit as the reducing agent and sodium citrate as the comlexing agent. The basic plating solution is composed of 0.1M NiSO$_4$, 0.005${\sim}$0.0IM Tl$_2$S0$_4$, 0.1${\sim}$O.2M sodium hypophosphite and 0.02${\sim}$O.IM sodium citrate and the plating condition were pH 5${\sim}$6, temperrature 80$_4$90${\circ}$C. The results obtained are summarized as follows: 1) The crystal structure of deposit was amorphous structure as deposited state, became microcrystallized centering on Ni(111) plane by heat treatment at 200${\circ}$C, and grew as polycrystalline Ni, Ni$_3$P, Ni$_5$p$_2$,Tl, etc. by heat treatment higher than 350${\circ}$C. The grain size of plated deposits was grown up to 28.3~42.0nm by heat treatment for 1hour at 500${\circ}$C. 2) The electrical resistivity showed a comparatively high value of 192.5$_4$208.3 ${\mu}$${\Omega}$Cm and its thermal stability was great with resistivity value less than 0.22% in the thermal surroundings of 200${\circ}$C. 3) Ni-Tl-P alloy deposit showed such good constant current-making-effect in the variation of electric voltage, heat treatment temperature, and the composition of the deposit that it can be put to practical use as the matter of constant current device.

• Korean Journal of Materials Research
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• v.23 no.11
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• pp.661-665
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• 2013

We investigated the characteristics of electroless plated Cu films on screen printed Ag/Anodized Al substrate. Cu plating was attempted using neutral electroless plating processes to minimize damage of the anodized Al substrate; this method used sodium hypophosphite instead of formaldehyde as a reducing agent. The basic electroless solution consisted of $CuSO_4{\cdot}5H_2O$ as the main metal source, $NaH_2PO_2{\cdot}H_2O$ as the reducing agent, $C_6H_5Na_3O_7{\cdot}2H_2O$ and $NH_4Cl$ as the complex agents, and $NiSO_4{\cdot}6H_2O$ as the catalyser for the oxidation of the reducing agent, dissolved in deionized water. The pH of the Cu plating solutions was adjusted using $NH_4OH$. According to the variation of pH in the range of 6.5~8, the electroless plated Cu films were coated on screen printed Ag pattern/anodized Al/Al at $70^{\circ}C$. We investigated the surface morphology change of the Cu films using FE-SEM (Field Emission Scanning Electron Microscopy). The chemical composition of the Cu film was determined using XPS (X-ray Photoelectron Spectroscopy). The crystal structures of the Cu films were investigated using XRD (X-ray Diffraction). Using electroless plating at pH 7, the structures of the plated Cu-rich films were typical fcc-Cu; however, a slight Ni component was co-deposited. Finally, we found that the formation of Cu film plated selectively on PCB without any lithography is possible using a neutral electroless plating process.

• Polymer(Korea)
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• v.31 no.3
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• pp.184-188
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• 2007

Monodisperse PMMA/HDDA polymer particles were coated via electroless Ni plating using sodium hypophosphite as a reducing agent in an acidic environment. In this study, the effects of 1) the pretreatment conditions, 2) the plating temperature, 3) the plating pH, and 4) the initial pH, control of plating bath on the variation of plating rate, surface state of plated particles and plating reproducibility were investigated. It was observed that every pretreatment steps, especially conditioning and acceleration step, were very important for obtaining uniform Ni plating and the plating rate was increased with the increase of plating temperature and pH. Moreover, the initial pH control of plating bath was critical for the plating reproducibility.

• Korean Journal of Materials Research
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• v.19 no.2
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• pp.61-67
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• 2009

Electrolessly deposited Co (Re,P) was investigated as a possible capping layer for Cu wires. 50 nm Co (Re,P) films were deposited on Cu/Ti-coated silicon wafers which acted as a catalytic seed and an adhesion layer, respectively. To obtain the optimized bath composition, electroless deposition was studied through an electrochemical approach via a linear sweep voltammetry analysis. The results of using this method showed that the best deposition conditions were a $CoSO_4$ concentration of 0.082 mol/l, a solution pH of 9, a $KReO_4$ concentration of 0.0003 mol/l and sodium hypophosphite concentration of 0.1 mol/L at $80^{\circ}C$. The thermal stability of the Co (Re,P) layer as a barrier preventing Cu was evaluated using Auger electron spectroscopy and a Scanning calorimeter. The measurement results showed that Re impurities stabilized the h.c.p. phase up to $550^{\circ}C$ and that the Co (Re,P) film efficiently blocked Cu diffusion under an annealing temperature of $400^{\circ}C$ for 1hr. The good barrier properties that were observed can be explained by the nano-sized grains along with the blocking effect of the impurities at the fast diffusion path of the grain boundaries. The transformation temperature from the amorphous to crystal structure is increased by doping the Re.