• Journal of the Korean institute of surface engineering
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• v.49 no.5
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• pp.401-407
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• 2016

In this work, effect of zincate treatment of AZ91 Mg alloy on the following electrodeposition of copper was examined in a non-cyanide bath containing pyrophosphate ions in view of surface morphology and adhesion of the electrodeposited copper layer. Without zincate treatment, the electrodeposited copper layer showed very porous structure and poor adhesion. On the other hand, the copper layer electrodeposited on the zincate-treated surface showed dense structure and good adhesion. The dissolution rate of AZ91 Mg alloy after the zincate treatment appeared to decrease about 40 times in the copper pyrophosphate bath, as compared to that of the surface without zincate treatment. The porous morphology and poor adhesion of a copper layer on the AZ91 Mg alloy surface without zincate treatment were attributed to small number of nucleation sites of copper because of rapid dissolution of the magnesium substrate in the pyrophosphate bath. Based on the experimental results, it is concluded that the zincate treatment to form a conducting and protecting layer on the AZ91 Mg alloy surface is essential for successful electrodeposition of a copper layer on AZ91 Mg alloy with good adhesion and dense structure in the copper pyrophosphate bath.

• Proceedings of the Korean Institute of Surface Engineering Conference
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• 2016.11a
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• pp.124.1-124.1
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• 2016

In this work, uniform thickness and good adhesion of electrodeposited copper layer were achieved on AZ91 Mg alloy in alkaline noncyanide copper solution containing pyrophosphate ion by employing appropriate zincate pretreatment. Without zincate pretreatment, the electrodeposited copper layer on AZ91 Mg alloy was porous and showed poor adhesion which was explained by small number of nucleation sites of copper due to rapid dissolution of the magnesium substrate in the pyrophosphate solution. The zincate pretreatment was found as one of the most important steps that can form a conducting layer to cover AZ91 surface which decreased the dissolution rate of AZ91 Mg alloy about 40 times in the copper pyrophosphate solution. Electrodeposited copper layer on AZ91 Mg alloy after an appropriate zincate pretreatment showed good adhesion and uniform thickness with bright surface appearance, independent of the deposition time but the surface roughness of the electrodeposited copper layer increased with increasing Cu deposition time.

• Journal of the Korean Chemical Society
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• v.60 no.5
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• pp.317-320
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• 2016

Efficient copper removal from water was achieved by using surface modified silica spheres with 3-mercaptopropyltrimethoxysilane (MPTMS) using base catalyst. The surface modification of silica spheres was performed by hydrolysis and condensation reactions of the MPTMS. The characteristic infrared absorption peaks at 2929, 1454, and 1343 cm⁻¹ represent the −CH₂ stretching vibration, asymmetric deformation, and deformation, respectively. The absorption peaks at 2580 and 693 cm⁻¹ corresponding the −SH stretching vibration and the C-S stretching vibration indicate the incorporation of MPTMS to the surface of silica spheres. Field emission scanning electron microscope (FESEM) image of the surface modified silica sphere (SMSS) shows nano-particles of MPTMS on the surface of silica spheres. High concentration of copper solution (1000 ppm) was used to test the copper removal efficiency and uptake capacity. The FESEM image of SMSS treated with the copper solution shows large number of copper lumps on the surface of SMSS. The copper concentration drastically decreased with increasing the amount of SMSS. The residual copper concentrations were analyzed using inductively coupled plasma mass spectrometer. The copper removal efficiency and uptake capacity with 1000 ppm of copper solution were 99.99 % and 125 mg/g, respectively.

• Proceedings of the Korean Institute of Surface Engineering Conference
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• 2013.05a
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• pp.179-179
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• 2013

Surface resistance of electro-deposited copper with its thickness, current density and surface roughness was determined by using a 4-point probe analyzer. The copper was prepared electrochemically on 316 stainless steel substrate in copper sulfate solution at the condition of $1A/dm^2$, 298 K, and 6.5 cm-electrode distance. The surface resistance of the copper sheet in the range of $0.93-0.97{\Omega}$ increased with the copper thickness in the range of $21-70{\mu}m$. The surface resistance in the range of $0.963-1.009{\Omega}$ also increased with current density in the range of $0.5-2A/dm^2$. The increased surface resistances corresponded to 11% for thickness and 25% for current density, respectively.

• Corrosion Science and Technology
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• v.6 no.4
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• pp.154-158
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• 2007

For the application of flexible printed circuit board (FPCB), electroplated copper is required to have low surface roughness and residual stress. In the paper, the effects of surface roughness and residual stress of electroplated copper as thick as $8{\mu}m$ were studied on organic additives such as inhibitor, leveler and accelerator. Polyimide film coated with sputtered copper was used as a substrate. Surface roughness and surface morphology were measured by 3D-laser surface analysis and FESEM, respectively. Residual stress was calculated by Stoney's equation after measuring radius curvature of specimen. The addition of additives except high concentration of accelerator in the electrolyte decreased surface roughness of electroplated copper film. Such a tendency was explained by the function of additives among which the inhibitor and the leveler inhibit electroplating on a whole surface and prolusions, respectively. The accelerator plays a role in accelerating the electroplating in valley parts. The inhibitors and the leveler increased residual stress, whereas the accelerator decreased it. It was thought to be related with entrapped additives on electroplated copper film rather than the preferred orientation of electroplated copper film. The reason why additives lead to residual stress remains for the future work.

• Journal of the Korean institute of surface engineering
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• v.41 no.1
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• pp.23-27
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• 2008

The effect of solution agitation on the copper electroless deposition process of ULSI (ultra large scale integration) interconnections was investigated by using physical, electrochemical and electrical techniques. It was found that proper solution agitation was effective to obtain superconformal copper configuration within the trenches of $130{\sim}80nm$ width. The transition of open potential during electroless deposition process showed that solution agitation induced compact structure of copper deposits by suppressing mass transfer of cuprous ions toward substrate. Also, the specific resistivity of copper layers was lowered by increasing agitation speed, which made the deposited copper particles smaller. Considering both copper deposit configuration and electric property, around 500 rpm of solution agitation was the most suitable for the homogeneous electroless copper filling within the ultra-fine patterns.

• Nuclear Engineering and Technology
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• v.55 no.8
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• pp.2742-2746
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• 2023

The corrosion behavior of copper immersed in dilute oxychloride solution (100 mM) was studied through surface investigation and in-situ monitoring of open-circuit potential. The copper corrosion was initiated with copper dissolution into a form of CuCl^-₂, resulting in mass decrease within the first 40 h of immersion. This was followed by a hydrolysis reaction initiated by the CuCl^-₂ at the copper surface, after which oxide products were formed and deposited on the surface, resulting in a mass increase. The formation of nucleation sites for copper oxide and its lateral extension during the corrosion process were examined using focused ion beam (FIB)-scanning electron microscopy (SEM). The presence of metastable compounds such as atacamite (CuCl₂·3Cu(OH)₂) on the corroded copper surface was revealed by X-ray photoelectron spectra (XPS) and transmission electron microscopy (TEM)-energy dispersive spectrometry (EDS) analysis.

• Journal of the Korean institute of surface engineering
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• v.47 no.1
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• pp.1-6
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• 2014

The copper deposit on steel plate was prepared by pyrophosphate copper plating solution made with variation of inorganic additive. $NH_4OH$ and $NH_4NO_3$ were used as inorganic additives. The copper layer characteristics - tensile strength, crystallite size and crystal orientation - were evaluated by X-ray diffraction and Universal Test Machine. The presence of ammonium nitrate results in reduction of average roughness value from $0.08{\mu}m$ to $0.03{\mu}m$. In pyrophosphate copper plating solution without Inorganic additive, tensile strength of electrodeposit copper foil was reduced from 600 MPa to 180 MPa after 7 days aging. However, when adding ammonium nitrate, there was almost no change of tensile strength, intensity of crystal orientation - (111), (200) and (220) - and crystallite size (2~30 nm).

• Proceedings of the KWS Conference
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• 2006.05a
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• pp.24-26
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• 2006

The copper foil of 10fm of thickness was prepared, and the surface treatment on the copper foil was done by the method of the electrolytic plating in the acid solution with the sulfate ion as a purpose to remove the main element of the surface contaminant of copper variously. The structure on the surface of the copper foil in this study investigated AFM with SEM the changed phenomenon according to added plating time and current. The phenomenon of the structure's of the oxide on the surface of long plating time and high current growing was confirmed.

• Journal of the Korean institute of surface engineering
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• v.42 no.6
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• pp.280-286
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• 2009

In this study, the corrosion property of copper alloy tubes in seawater has been investigated. Three copper alloys of nominal composition Cu-20Zn-2Al(Al-Brass), Cu-30Ni(CN70/30) and Cu-10Ni(CN90/10) were considered. The samples were immersed in 3%NaCl flowing solution at $90^{\circ}C$ for 30, 50 and 80 days. Corrosion rate of copper alloy tubes in 3%NaCl flowing solution was investigated by weight-loss measurements and electrochemical test. The CN70/30 showed lowest corrosion rate among three copper alloy tubes. Because of passive films formation, corrosion rates of three types of copper tubes were decrease with time. Surface characteristics of copper alloy tubes were analyzed by optical micrograph(OM), scanning electronic microscopy (SEM), energy dispersive X-ray analysis(EDAX) and X-ray diffraction patterns(XRD). CN70/30 showed partly pitting problem on the surface owing to high Fe content, even though having high resistant against corrosion. Cracks appeared on the surface of CN90/10 and CN70/30 after more than 50 days immersion, which could be derived from high nickel contents.