• Corrosion Science and Technology
• /
• v.22 no.3
• /
• pp.193-200
• /
• 2023

Titanium alloy (grade-4) is commonly used in industrial and medical applications. To improve its corrosion resistance and biocompatibility for medical use, it is necessary to form a titanium oxide film. In this study, the morphology of the oxide film formed by anodizing Ti-grade 4 using different electrolytes was analyzed. Wetting properties before and after surface modification with SAM coating were also observed. Electrolytes used were categorized as A, B, and C. Electrolyte A consisted of 0.3 M oxalic acid and ethylene glycol. Electrolyte B consisted of 0.1 M NH₄F and 0.1 M H₂O in ethylene glycol. Electrolyte C consisted of 0.07 M NH₄F and 1 M H₂O in ethylene glycol. Samples B and C exhibited a porous structure, while sample A formed a thickest oxide film with a droplet-like structure. AFM analysis and contact angle measurements showed that sample A with the highest roughness exhibited the best hydrophilicity. After surface modification with SAM coating, it displayed superior hydrophobicity. Despite having the thickest oxide film, sample A showed the lowest insulation resistance due to its irregular structure. On the other hand, sample C with a thick and regular porous oxide film demonstrated the highest insulation resistance.

• Journal of the Korean Institute of Electrical and Electronic Material Engineers
• /
• v.34 no.1
• /
• pp.68-72
• /
• 2021

Aluminum is a lightweight metal and has excellent properties with regard to conductivity, workability, and strength. It has been used in various industries owing to its economic benefits. To improve upon the mechanical properties and processability by adding various alloying elements to aluminum, improving the corrosion resistance and heat resistance by electrochemically forming a porous anodic film having a thickness and hardness on the surface of the aluminum alloy is crucial. In this study, the aluminum 6061 alloy was controlled by an anodization process in a 0.3M oxalic acid electrolyte at room temperature to investigate the oxide film parameters such as porosity and thickness depending on the modulating applied voltage and time. The anodizing experiment was performed by increasing the time from 1 h to 9 h at 2-h intervals at applied voltages of 50 V and 60 V.

• Journal of the Korean institute of surface engineering
• /
• v.51 no.1
• /
• pp.34-39
• /
• 2018

Steel crucible used for molten Al has a problem of very limited lifetime because of the interaction between Fe and molten Al. This study was performed to improve the lifetime of steel crucible for molten Al by coating metallic Al and by further anodizing treatment to form thick and uniform anodic oxide films. The lifetime of the steel crucible was improved slightly by Al coating from 30 to 40 hours by metallic Al coating and largely to 120 hours by coating the surface with anodic oxide film. The improved lifetime was attributed to blocking of the reaction between Fe and molten Al with the help of anodic oxide layer with more than 20 um thickness on the crucible surface. The failure of the steel crucible arises from the formation of intermetallic compounds and pores at the steel/Al interface.

• Korean Journal of Materials Research
• /
• v.17 no.5
• /
• pp.244-249
• /
• 2007

The properties of anodized films on aluminum 6061 alloy in single electrolyte of sulfuric acid and mixed electrolyte of sulfuric-boric acid and sulfuric-boric-nitric acid have been studied. Polarization tests in NaC solution were used to investigate the corrosion performance. Characteristics of film formation and surface morphology were examined by optical microscopy, FE-SEM and EDS. The results obtained have indicated that oxide films growth have been promoted by nitric acid and anodized films in mixed electrolyte have superior corrosion resistance. In case of anodic films formed in mixed electrolyte, some grooves and numerous crazings were also observed at the surface.

• Journal of the Korea Institute of Information and Communication Engineering
• /
• v.14 no.4
• /
• pp.923-928
• /
• 2010

Anodic aluminum oxide (AAO) nanotemplates for nano electronic device applications have been attracting increasing interest because of ease of fabrication, low cost process, and possible fabrication in large area. The size and density of the nanostructured materials can be controlled by changing the pore diameter and the pole density of AAO nanotemplate. In this paper, nano porous alumina films AAO nanotemplate was fabricated by second anodization method using sputterd Al films. In addition, effects of electrolyte temperature and anodization voltate on the microstructure of porous alumina films were investigated. As the electrolyte temperature was increased from $8^{\circ}C$ to $20^{\circ}C$, the growth rate of nanoporous alumina films was increased from 86.2 nm/min to 179.5 nm/min. The AAO nanotemplate fabricated with optimal condition had the mean pore diameter of 70 nm and the pore depth of $1\;{\mu}m$.

• Korean Journal of Materials Research
• /
• v.12 no.7
• /
• pp.528-532
• /
• 2002

Anodic $TiO_2$film on Ti substrate was fabricated at 180V in sulfuric acid solutions containing phosphoric acid and hydrogen peroxide. Effects of the anodizing conditions on the morphology of the oxide layers, and chemical states of the component elements of the layers were studied primarily using SEM, XRD, AFM, and XPS. The pores in the oxide layer was not uniform in size, shape, and growth direction particularly near the interface between the substrate and the oxide layer, compared with those of the surface layer. The formation of irregular type of pores seemed to be attributed to spark discharge phenomena which heavily occurred during increasing the anodic voltage. The pore diameter and the cell size increased, and the number of cells per unit area decreased with the increasing time. From the XPS results, it was shown that component elements of the electrolytes, P and S, existed in the chemical states of $PO_4^{-3}$ , $P_2$$O_{5}$, $SO_4^{-2}$ , $SO_3^{-2}$ , P, S, etc., which were penetrated from the electrolytes into the oxide layer during anodization.

• Corrosion Science and Technology
• /
• v.17 no.2
• /
• pp.45-53
• /
• 2018

A new 80Ti-15Ta-5Zr wt% alloy surface was protected by anodic oxidation in phosphoric acid solution. The protective oxide layer (TiO2, ZrO2 and Ta suboxides and thickness of 15.5 nm) incorporated $PO{_4}^{3-}$ ions from the solution, according to high resolution XPS spectra. The AFM analysis determined a high roughness with SEM detected pores (20 - 50 nm). The electrochemical studies of bare and anodically oxidized Ti-15Ta-5Zr alloy in Carter-Brugirard saliva of different pH values and saliva with 0.05M NaF, pointed to a nobler surface for the protected alloy, with a thicker electrodeposited oxide layer acting as a barrier against aggressive ions. The oxidized alloy significantly decreased corrosion current densities and total quantity of ions released into the oral environment in comparison with the bare one, at higher polarisation resistance and protective capacity of the electrodeposited layer. The impedance data revealed a bi-layered oxidation film formed by: a dense, compact, barrier layer in contact with the metallic substrate, decreasing the potential gradient across the metal/oxide layer/solution interface, reducing the anodic dissolution and a more permissive, porous layer in contact with the electrolyte. The open circuit potential for protected alloy shifted to nobler values, with thickening of the oxidation film signifying long-term protection.

• Journal of Dental Rehabilitation and Applied Science
• /
• v.21 no.1
• /
• pp.33-42
• /
• 2005

This study was performed to investigate the surface properties and in vitro biocompatibility of electrochemically oxidized Ti-6Al-7Nb alloy by anodic spark discharge technique. Discs of Ti-6Al-7Nb alloy of 20 mm in diameter and 2 mm in thickness were polished sequentially from #300 to 1000 SiC paper, ultrasonically washed with acetone and distilled water for 5 min, and dried in an oven at $50^{\circ}C$ for 24 hours. Anodizing was performed using a regulated DC power supply. The applied voltages were given at 240, 280, 320, and 360 V and current density of $30mA/cm^2$. Hydrothermal treatment was conducted by high pressure steam at $300^{\circ}C$ for 2 hours using a autoclave. Samples were soaked in the Hanks' solution with pH 7.4 at $36.5^{\circ}C$ during 30 days. The results obtained were summarized as follows; 1. The oxide films were porous with pore size of $1{\sim}5{\mu}m$. The size of micropores increased with increasing the spark forming voltage. 2. The main crystal structure of the anodic oxide film was anatase type as analyzed with thin-film X-ray diffractometery. 3. Needle-like hydroxyapatite (HA) crystals were observed on anodic oxide films after hydrothermal treatment at $300^{\circ}C$ for 2 hours. The precipitation of HA crystals was accelerated with increasing the spark forming voltage. 4. The precipitation of the fine asperity-like HA crystals were observed after being immersed in Hanks' solution at $37^{\circ}C$. The precipitation of HA crystals was accelerated with increasing the spark forming voltage and the time of immersion in Hanks' solution. 5. The Ca/P ratio of the precipitated HA layer was equivalent to that of HA crystal as increasing the spark forming voltage and the time of immersion in Hanks' solution.

• Journal of Dental Rehabilitation and Applied Science
• /
• v.22 no.1
• /
• pp.101-110
• /
• 2006

This study was performed to investigate the surface properties and in vitro biocompatibility of electrochemically oxidized Ti-6Al-7Nb alloy by anodic spark discharge technique. Discs of Ti-6Al-7Nb alloy of 20 mm in diameter and 2 mm in thickness were polished sequentially from #300 to 1000 SiC paper, ultrasonically washed with acetone and distilled water for 5 min, and dried in an oven at $50^{\circ}C$ for 24 hours. Anodizing was performed using a regulated DC power supply. The applied voltages were given at 240, 280, 320, and 360 V and current density of $30mA/cm^2$. Hydrothermal treatment was conducted by high pressure steam at $300^{\circ}C$ for 2 hours using a autoclave. Samples were soaked in the Hanks' solution with pH 7.4 at $36.5^{\circ}C$ during 30 days. The results obtained were summarized as follows; 1. The oxide films were porous with pore size of $1{\sim}5{\mu}m$. The size of micropores increased with increasing the spark forming voltage. 2. The main crystal structure of the anodic oxide film was anatase type as analyzed with thin-film X-ray diffractometery. 3. Needle-like hydroxyapatie (HA) crystals were observed on anodic oxide films after hydrothermal treatment at $300^{\circ}C$ for 2 hours. The precipitation of HA crystals was accelerated with increasing the spark forming voltage. 4. The precipitation of the fine asperity-like HA crystals were observed after being immersed in Hanks' solution at $37^{\circ}C$. The precipitation of HA crystals was accelerated with increasing the spark forming voltage and the time of immersion in Hanks' solution. 5. The Ca/P ration of the precipitated HA layer was equivalent to that of HA crystal as increasing the spark forming voltage and the time of immersion in Hanks' solution.

• Nuclear Engineering and Technology
• /
• v.5 no.1
• /
• pp.30-37
• /
• 1973

The Nishitani's equations for impedance of anodic oxide films have been derived based on a p-i-n model under the assumption of $\omega$$\varepsilon$$\rho$$_{ο}$<<4$\pi$<<$\omega$$\varepsilon$$\rho$$_{\omega}$, where $\omega$ is angular frequency, $\varepsilon$ is dielectric constant, and $\rho$$_{ο}$ and $\rho$$_{\omega}$ are the resistivity of the interface region and the intrisic region of the anodic oxide film, respectively. Since it is not possible to evaluate all parameters in the equations, however, any clear physical picture cannot be obtained from the equations. Therefore, the equations are modified under the assumption of $\omega$$\tau$$_{\omega}$>>1 and In(1+$\omega$$^2$$\tau$$_{ο}$$^2$)<<1, where $\tau$$_{\omega}$=$\varepsilon$$\rho$$_{\omega}$(4$\pi$) and $\tau$$_{ο}$=$\varepsilon$$\rho$$_{ο}$/(4$\pi$). The modified equations are then used to explain the change in the frequency characteristics of anodic oxide films when they are heated. The change in impedance of anodic oxide films when they are heated is attributed mainly to the increase in the diffusion layer and to the decrease in the resistivity of anodic oxide films.s.