• Journal of the Korean institute of surface engineering
• /
• v.49 no.2
• /
• pp.135-140
• /
• 2016

In this study, we prepared magnesium ion containing oxide films formed on the Ti-6Al-4V using plasma electrolytic oxidation (PEO) treatment. Ti-6Al-4V surface was treated using PEO in Mg containing electrolytes at 270V for 5 min. The phase, composition and morphology of the Mg ion containing oxide films were evaluated with X-ray diffraction (XRD), Attenuated total reflectance Fourier transform infrared (ATR-FTIR) and filed-emission scanning electron microscopy (FE-SEM) with energy dispersive X-ray spectrometer (EDS). The biocompatibility of Mg ion containing oxide films was evaluated by immersing in simulated body fluid (SBF). According to surface properties of PEO films, the optimum condition was formed when the applied was 270 V. The PEO films formed in the condition contained the properties of porosity, anatase phase, and near 1.7 Ca(Mg)/P ratio in the oxide film. Our experimental results demonstrate that Mg ion containing oxide promotes bone like apatite nucleation and growth from SBF. The phase and morphologies of bone like apatite were influenced by the Mg ion concentration.

• Proceedings of the Korean Institute of Surface Engineering Conference
• /
• 2018.06a
• /
• pp.74-74
• /
• 2018

Ti-6Al-4V alloys have been widely used as orthopedic materials because of their excellent corrosion resistance and mechanical properties. However, it does not bind directly to the bone, so it requires a surface modification. This problem can be solved by nanotube and micropore formation. Plasma electrolytic oxidation (PEO) treatment for micropore, which combines high-voltage spark and electrochemical oxidation, is a new way of forming a ceramic coating on light metals such as titanium and its alloys. This method has excellent reproducibility and can easily control the shape and size of the Ti alloy. In this study, formation of bioactive surface by PEO-treatment after $2^{nd}$ ATO technique of Ti-6Al-4V alloy was invesgated by various instrument. Nanotube oxide surface structure was formed on the surface by anodic oxidation treatment in 0.8 wt.% NaF and 1M $H_3PO_4$ electrolytes. After nanotube formation, nanotube layer was removed by ultrasonic cleaning. PEO-treatment was carried out at 280V for 3 minutes in the electrolytic solution containing the bioactive substance (Mg, Zn, Mn, Sr, and Si). The surface of Ti-6Al-4V alloy was observed by field emission scanning electron microscopy (FE-SEM, S-4800 Hitachi, Japan). An energy dispersive X-ray spectrometer (EDS, Inca program, Oxford, UK) was used to analyze the spectra of physiologically active Si, Mn, Mg, Zn, and Sr ions. The PEO film formed on the Ti-6Al-4V alloy surface was characterized using an X-ray diffractometer (TF-XRD, X'pert Philips, Netherlands). It is confirmed that bioactive ions play an essential role in the normal bone growth and metabolism of the human skeletal tissues.

• Journal of the Korean institute of surface engineering
• /
• v.49 no.3
• /
• pp.280-285
• /
• 2016

In this study, we investigated the influences of potassium fluoride(KF) addition on the surface characteristics of plasma electrolytic oxidation(PEO) coating produced on Al alloy. The PEO of marine grade Al alloy(5083 grade) was conducted in KOH 1g/L solution adding different concentrations of KF(0, 1 and 2 g/L) under a galvanostatic regime. With KF addition, unusual behavior was observed on the voltage-time characteristic curves, which can be characterized by the following process: (i) initial rapid increase in voltage (ii) a short plateau after 1st breakdown (iii) gradual increase in voltage (iv) intermittent fluctuation of voltage after 2nd breakdown. The SEM observation revealed irregular surface morphology with KF addition, as compared with one formed without KF addition, which had a reticulate structure. The XRD analysis detected the formation of aluminium hydroxide fluoride hydrate($H_{4.76}Al_2F_{3.24}O_{3.76}$) on surface grown by PEO process with KF. Particularly, at very early stage of the process (~ 120 s), thin film was formed having nanoporous structure, and F element was confirmed on surface by EDS analysis. The thickness and surface roughness of the coating increased with increasing KF concentration. As a result, KF addition was found to be less beneficial influences on PEO of marine grade Al alloy, and therefore needs further research to improve its capability.

• Corrosion Science and Technology
• /
• v.15 no.3
• /
• pp.120-124
• /
• 2016

The effect of alloying element Ca (0, 1, and 2 wt%) on corrosion resistance and bioactivity of the as-received and anodized surface of rolled plate AM60 alloys was investigated. A plasma electrolytic oxidation (PEO) was carried out to form anodic oxide film in $0.5mol\;dm^{-3}\;Na_3PO_4$ solution. The corrosion behavior was studied by polarization measurements while the in vitro bioactivity was tested by soaking the specimens in Simulated Body Fluid (1.5xSBF). Optical micrograph and elemental analysis of the substrate surfaces indicated that the number of intermetallic particles increased with Ca content in the alloys owing to the formation of a new phase $Al_2Ca$. The corrosion resistance of AM60 specimens improved only slightly by alloying with 2 wt% Ca which was attributed to the reticular distribution of $Al_2Ca$ phase existed in the alloy that might became barrier for corrosion propagation across grain boundaries. Corrosion resistance of the three alloys was significantly improved by coating the substrates with anodic oxide film formed by PEO. The film mainly composed of magnesium phosphate with thickness in the range $30-40{\mu}m$. The heat resistant phase of $Al_2Ca$ was believed to retard the plasma discharge during anodization and, hence, decreased the film thickness of Ca-containing alloys. The highest apatite forming ability in 1.5xSBF was observed for AM60-1Ca specimens (both substrate and anodized) that exhibited more degradation than the other two alloys as indicated by surface observation. The increase of surface roughness and the degree of supersaturation of 1.5xSBF due to dissolution of Mg ions from the substrate surface or the release of film compounds from the anodized surface are important factors to enhance deposition of Ca-P compound on the specimen surfaces.

• Journal of Welding and Joining
• /
• v.32 no.3
• /
• pp.27-33
• /
• 2014

This paper presents a brief summary on a relatively new plasma aided electrolytic surface treatment process for light metals. A brief discussion regarding the advantages, principle, process parameters and applications of this process is discussed. The process owes its origin to Sluginov who discovered an arc discharge phenomenon in electrolysis in 1880. A similar process was studied and developed by Markov and coworkers in 1970s who successfully deposited an oxide film on aluminium. Several investigation thereafter lead to the establishment of suitable process parameters for deposition of a crystalline oxide film of more than $100{\mu}m$ thickness on the surface of light metals such as aluminium, titanium and magnesium. This process nowadays goes by several names such as plasma electrolytic oxidation (PEO), micro-arc oxidation (MOA), anodic spark deposition (ASD) etc. Several startups and surface treatment companies have taken up the process and deployed it successfully in a range of products, from military grade rifles to common off road sprockets. However, there are certain limitations to this technology such as the formation of an outer porous oxide layer, especially in case of magnesium which displays a Piling Bedworth ratio of less than one and thus an inherent non protective oxide. This can be treated further but adds to the cost of the process. Overall, it can be said the PEO process offers a better solution than the conventional coating processes. It offers advantages considering the fact that he electrolyte used in PEO process is environmental friendly and the temperature control is not as strict as in case of other surface treatment processes.

• Corrosion Science and Technology
• /
• v.5 no.2
• /
• pp.77-83
• /
• 2006

The plasma electrolytic oxidation (PEO) process is a relatively new surface treatment technique that produces a chemically stable and environment-friendly electrolytic coating that can be applied to all types of magnesium alloys. In this study, the characteristics of oxide film were examined after coating the extruded AZ31 alloy through the PEO process. Hard ceramic coatings were obtained on the AZ31 alloy by changing the coating time from 10min to 60min. The morphologies of the surface and the cross-section of the PEO coatings were examined by scanning electron microscopy and optical microscopy, and the thickness of the coating was measured. The X-ray diffraction pattern of the coating shows that the coated layer consists mainly of the MgO and $Mg_2SiO_4$ phases after the oxidation reaction. The hardness of the coated AZ31 alloy increased with increasing coating time. In addition, the corrosion rates of the coated and uncoated AZ31 alloys were examined by salt spray tests according to ASTM B 117 and the results show that the corrosion resistance of the coated AZ31 alloy was superior to that of the un-coated AZ31 alloy.

• Journal of the Korean Society for Heat Treatment
• /
• v.25 no.5
• /
• pp.227-232
• /
• 2012

Magnesium alloy have good physical properties such as good castability, good vibration absorption, high strength/weight ratios. Despite the desirable properties, the poor resistance of Mg alloy impedes their use in many various applications. Therefore, magnesium alloy require surface treatment to improve hardness, corrosion and wear resistance. Plasma Electrolytic Oxidation (PEO) is one the surface treatment methods to form oxide layer on Mg alloy in alkali electrolyte. In comparison with Anodizing, there is environmental process having higher hardness and faster deposition rate. In this study, the characteristics of oxide film were examined after coating the AZ31 Mg alloy through the PEO process. We changed concentration of sodium aluminate into $K_2ZrF_6$, KF base electrolyte. The morphologies of the coating layer were characterized by using scanning electron microscopy (SEM). Corrosion resistance also investigated by potentiodynamic polarization analysis. As a result, propertiy of oxide layer were changed by concentration of sodium aluminate. Increasing with concentration of sodium aluminate in electrolyte, the oxidation layer was denser and the pore size was smaller on the surface.

• Journal of the Korean institute of surface engineering
• /
• v.52 no.3
• /
• pp.117-122
• /
• 2019

In this study, surface porosity and corrosion resistance of PEO coatings prepared on the 6061 Al alloy were investigated in terms of sodium phosphate ($Na_3PO_4$) concentrations in an alkaline solution and $NaAlO_2$ sealing. The surface morphologies of the PEO coatings clearly show that the coatings film formed in $9g\;L^{-1}$ had the lowest porosity. The $NaAlO_2$ sealing was found to remove micropores and cracks existing on the surface of PEO coatings. As a result, the $NaAlO_2$ sealing resulted in the movement of corrosion potential toward more positive value and lower corrosion current density.

• Korean Chemical Engineering Research
• /
• v.49 no.6
• /
• pp.758-763
• /
• 2011

In this work, polymer composite electrolytes were prepared by a blend of poly(methyl methacrylate) (PMMA) and poly(ethylene oxide) (PEO) as a polymer matrix, propylene carbonate as a plasticizer, $LiClO_4$ as a salt, and by containing a different content of $TiO_2$, by using the solution casting method. The crystallinity and ionic conductivity of the polymer electrolytes was evaluated using X-ray diffraction(XRD) and AC impedance method, respectively. The morphology of composite electrolyte film was analyzed by SEM method. From the experimental results, by increasing the $TiO_2$ content, crystallinity of PEO was reduced, and ionic conductivity was increased. In particular, the ionic conductivity was dependent on the content of $TiO_2$ and showed the highest value 15 wt%. However, when $TiO_2$ content exceeds 15 wt%, the ionic conductivity was decreased. According to the surface morphology, the ionic conductivity was decreased because the polymer composite electrolytes showed a heterogenous morphology of fillers due to immiscibility or aggregation of the filler within the polymer matrix.

• Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
• /
• 2006.11a
• /
• pp.230-231
• /
• 2006

In this paper, we examined effects by the binder in manufacturing titanium dioxide film for dye sensitized solar cell. Binder(PEG and PEO) was added the amount of 10-40wt% to commercial $TiO_2$ (P25), Respectively. All of $TiO_2$ film was showed porous structure owing to the addition of binders. But the difference of film's porosity could not be confirmed. The transmittance of $TiO_2$ film was decreased with the increase of binder's amount, generally. In case of 20wt%, however. The transmittance of $TiO_2$ films was showed the highest value.