• Corrosion Science and Technology
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• v.6 no.6
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• pp.316-321
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• 2007

The effect of annealing on the pitting corrosion resistance of anodized Al-Mg alloy (AA5052) processed by equal-channel angular pressing (ECAP) was investigated by electrochemical techniques in a solution containing 0.2 mol/L of $AlCl_3$ and also by surface analysis. The Al-Mg alloy was annealed at a fixed temperature between 473 and 573 K for 120 min in air after ECAP. Anodizing was conducted for 40 min at $100-400A/m^2$ at 293 K in a solution containing 1.53 mol/L of $H_2SO_4$ and 0.0185 mol/L of $Al_2(SO_4)_3$. The internal stress generated in anodic oxide films during anodization was measured with a strain gauge to clarify the effect of ECAP on the pitting corrosion resistance of anodized Al-Mg alloy. The time required to initiate the pitting corrosion of anodized Al-Mg alloy was shorter in samples subjected to ECAP, indicating that ECAP decreased the pitting corrosion resistance. However, the pitting corrosion resistance was greatly improved by annealing after ECAP. The time required to initiate pitting corrosion increased with increasing annealing temperature. The strain gauge attached to Al-Mg alloy revealed that the internal stress present in the anodic oxide films was compressive stress, and that the stress was larger with ECAP than without. The compressive internal stress gradually decreased with increasing annealing temperature. Scanning electron microscopy showed that cracks occurred in the anodic oxide film on Al-Mg alloy during initial corrosion and that the cracks were larger with ECAP than without. The ECAP process of severe plastic deformation produces large internal stresses in the Al-Mg alloy; the stresses remain in the anodic oxide films, increasingthe likelihood of cracks. It is assumed that the pitting corrosion is promoted by these cracks as a result of the higher internal stress resulting from ECAP. The improvement in the pitting corrosion resistance of anodized AlMg alloy as a result of annealing appears to be attributable to a decrease in the internal stresses in anodic oxide films

• Corrosion Science and Technology
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• v.6 no.6
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• pp.275-281
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• 2007

The effect of annealing on the pitting corrosion resistance of anodized Al-Mg alloy (AA5052) processed by equal-channel angular pressing (ECAP) was investigated by electrochemical techniques in a solution containing 0.2 mol/L of $AlCl_3$ and also by surface analysis. The Al-Mg alloy was annealed at a fixed temperature between 473 and 573 K for 120 min in air after ECAP. Anodizing was conducted for 40 min at $100-400A/m^2$ at 293 K in a solution containing 1.53 mol/L of $H_2SO_4$ and 0.0185 mol/L of $Al_2(SO_4)_3$. The internal stress generated in anodic oxide films during anodization was measured with a strain gauge to clarify the effect of ECAP on the pitting corrosion resistance of anodized Al-Mg alloy. The time required to initiate the pitting corrosion of anodized Al-Mg alloy was shorter in samples subjected to ECAP, indicating that ECAP decreased the pitting corrosion resistance. However, the pitting corrosion resistance was greatly improved by annealing after ECAP. The time required to initiate pitting corrosion increased with increasing annealing temperature. The strain gauge attached to Al-Mg alloy revealed that the internal stress present in the anodic oxide films was compressive stress, and that the stress was larger with ECAP than without. The compressive internal stress gradually decreased with increasing annealing temperature. Scanning electron microscopy showed that cracks occurred in the anodic oxide film on Al-Mg alloy during initial corrosion and that the cracks were larger with ECAP than without. The ECAP process of severe plastic deformation produces large internal stresses in the Al-Mg alloy; the stresses remain in the anodic oxide films, increasingthe likelihood of cracks. It is assumed that the pitting corrosion is promoted by these cracks as a result of the higher internal stress resulting from ECAP. The improvement in the pitting corrosion resistance of anodized AlMg alloy as a result of annealing appears to be attributable to a decrease in the internal stresses in anodic oxide films

• Proceedings of the Korean Institute of Surface Engineering Conference
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• 2016.11a
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• pp.197-197
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• 2016

Commercially pure titanium (CP Ti) and Ti-6Al-4V alloys have been widely used for biomedical applications. However, the use of the Ti-6Al-4V alloy in biomaterial is then a subject of controversy because aluminum ions and vanadium oxide have potential detrimental influence on the human body due to vanadium and aluminum. Hence, recent works showed that the synthesis of new Ti-based alloys for implant application involves more biocompatible metallic alloying element, such as, Nb, Hf, Zr and Mo. In particular, Nb and Hf are one of the most effective Ti ${\beta}-stabilizer$ and reducing the elastic modulus. Plasma electrolyte oxidation (PEO) is known as excellent method in the biocompatibility of biomaterial due to quickly coating time and controlled coating condition. The anodized oxide layer and diameter modulation of Ti alloys can be obtained function of improvement of cell adhesion. Manganese(Mn) plays very important roles in essential for normal growth and metabolism of skeletal tissue in vertebrates and can be detected as minor constituents in teeth and bone. Radio frequency(RF) magnetron sputtering in the various PVD methods has high deposition rates, high-purity films, extremely high adhesion of films, and excellent uniform layers for depositing a wide range of materials, including metals, alloys and ceramics like a hydroxyapatite. The aim of this study is to research the Mn coatings on the micro-pore formed Ti-29Nb-xHf alloys by RF-magnetron sputtering for dental applications. Ti-29Nb-xHf (x= 0, 3, 7 and 15wt%, mass fraction) alloys were prepared Ti-29Nb-xHf alloys of containing Hf up from 0 wt% to 15 wt% were melted by using a vacuum furnace. Ti-29Nb-xHf alloys were homogenized for 2 hr at $1050^{\circ}C$. Each alloy was anodized in solution containing typically 0.15 M calcium acetate monohydrate + 0.02 M calcium glycerophosphate at room temperature. A direct current power source was used for the process of anodization. Anodized alloys was prepared using 270V~300V anodization voltage at room. Mn coatings was produced by RF-magnetron sputtering system. RF power of 100W was applied to the target for 1h at room temperature. The microstructure, phase and composition of Mn coated oxide surface of Ti-29Nb-xHf alloys were examined by FE-SEM, EDS, and XRD.

• Proceedings of the Korean Institute of Surface Engineering Conference
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• 2017.05a
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• pp.77-77
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• 2017

Titanium and its alloys offer attractive properties in a variety of applications. These are widely used for the field of biomedical implants because of its good biocompatibility and high corrosion resistance. Titanium anodizing is often used in the metal finishing of products, especially those can be used in the medical devices with dense oxide surface. Based on SAE/AMS (Society of Automotive Engineers/Aerospace Material Specification) 2488D, it has the specification for industrial titanium anodizing that have three different types of titanium anodization as following: Type I is used as a coating for elevated temperature forming; Type II is used as an anti-galling coating without additional lubrication or as a pre-treatment for improving adherence of film lubricants; Type III is used as a treatment to produce a spectrum of surface colours on titanium. In this study, we have focused on Type II anodization for the medical (dental and orthopedic) application, the anodized surface was modified with gray color under alkaline electrolyte. The surface characteristics were analyzed with Focused Ion Beam (FIB), Scanning Electron Microscopy (SEM), surface roughness, Vickers hardness, three point bending test, biocompatibility, and corrosion (potentiodynamic) test. The Ti-6Al-4V alloy was used for specimen, the anodizing procedure was conducted in alkaline solution (NaOH based, pH>13). Applied voltage was range between 20 V to 40 V until the ampere to be zero. As results, the surface characteristics of anodic oxide layer were analyzed with SEM, the dissecting layer was fabricated with FIB method prior to analyze surface. The surface roughness was measured by arithmetic mean deviation of the roughness profile (Ra). The Vickers hardness was obtained with Vickers hardness tester, indentation was repeated for 5 times on each sample, and the three point bending property was verified by yield load values. In order to determine the corrosion resistance for the corrosion rate, the potentiodynamic test was performed for each specimen. The biological safety assessment was analyzed by cytotoxic and pyrogen test. Through FIB feature of anodic surfaces, the thickness of oxide layer was 1.1 um. The surface roughness, Vickers hardness, bending yield, and corrosion resistance of the anodized specimen were shown higher value than those of non-treated specimen. Also we could verify that there was no significant issues from cytotoxicity and pyrogen test.

• The Journal of Korean Academy of Prosthodontics
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• v.47 no.1
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• pp.39-45
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• 2009

Statement of problem: Recently precalcification treatment has been studied to shorten the period of the implant. Purpose: This study was performed to evaluate the effect of precalcification treatment of $TiO_2$ Nanotube formed on Ti-6Al-4V Alloy. Material and methods: Specimens of $20{\times}10{\times}2\;mm$ in dimensions were polished sequentially from #220 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. The nanotubular layer was processed by electrochemical anodic oxidation in electrolytes containing 0.5 M $Na_2SO_4$ and 1.0 wt% NaF. Anodization was carried out using a regulated DC power supply (Kwangduck FA, Korea) at a potential of 20 V and current density of $30\;㎃/cm_2$ for 2 hours. Specimens were heat-treated at $600^{\circ}C$ for 2 hours to crystallize the amorphous $TiO_2$ nanotubes, and precalcified by soaking in $Na_2HPO_4$ solution for 24 hours and then in saturated $Ca(OH)_2$ solution for 5 hours. To evaluate the bioactivity of the precalcified $TiO_2$ nanotube layer, hydroxyapatite formation was investigated in a Hanks' balanced salts solution with pH 7.4 at $36.5^{\circ}C$ for 2 weeks. Results: Vertically oriented amorphous $TiO_2$ nanotubes of diameters 48.0 - 65.0 ㎚ were fabricated by anodizing treatment at 20 V for 2 hours in an 0.5 M $Na_2SO_4$ and 1.0 NaF solution. $TiO_2$ nanotubes were composed with strong anatase peak with presence of rutile peak after heat treatment at $600^{\circ}C$. The surface reactivity of $TiO_2$ nanotubes in SBF solution was enhanced by precalcification treatment in 0.5 M $Na_2HPO_4$ solution for 24 hours and then in saturated $Ca(OH)_2$ solution for 5 hours. The immersion in Hank's solution for 2 weeks showed that the intensity of $TiO_2$ rutile peak increased but the surface reactivity decreased by heat treatment at $600^{\circ}C$. Conclusion: This study shows that the precalcified treatment of $TiO_2$ Nanotube formed on Ti-6Al-4V Alloy enhances the surface reactivity.

• Journal of the Korean Institute of Electrical and Electronic Material Engineers
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• v.17 no.6
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• pp.592-597
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• 2004

Porous silicon(PS) has received much attention as a sensitive material of chemical sensors because of its large internal surface area. In this work, we fabricated gas-sensing devices based on the porous silicon layer which could be applicable to the measurement of blood alcohol content(BAC), and estimated their electrical properties. The structure of the sensor is similar to an MIS (metal-insulator-semiconductor) diode and consists of thin Au/oxidized PS/PS/p-Si/Al, where the p-Si substrate is etched anisotropically to reduce the thickness. We measured C-V curves from two types of the samples with the PS layer treated by the different anodization current density of 60 or 100 mA/cm$^2$, in order to compare the sensitivity. As a result, the magnitude and variation of capacitances from the devices with the PS formed under the current density of 100 mA/cm$^2$ were found to be more detectable due to the larger internal surface.

• Journal of the Korean Society of Manufacturing Process Engineers
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• v.18 no.7
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• pp.14-21
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• 2019

Large-diameter hydraulic devices such as the hydraulic reservoir in aircraft that serves to balance the hydraulic pressure in the various hydraulic devices in the cabin and to store hydraulic oil are operated by the internal piston systems. However, since this operates in an environment with high temperature and humidity, it may cause the inner surface to flake during its operation. Therefore, an anodizing surface treatment is applied to improve the corrosion resistance, abrasion resistance, and smooth operation. However, anodizing increases the surface roughness. Accordingly, the polishing process that improves the surface roughness after anodizing is important. However, the existing polishing process is performed manually, which results in an inefficient process. Therefore, in this study, we selected the optimum polishing conditions for effective polishing using the experimental design to improve the polishing process for the $Al_2O_3$ film that forms after anodization. Through experiments, we confirmed that the surface uniformity after polishing was superior as the feed rate was slower when the same polishing time had been applied.

• Journal of Electrochemical Science and Technology
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• v.12 no.2
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• pp.188-203
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• 2021

The specific benefits of the modified films formed on preliminary anodized aluminum, including the versatility of their potential applications impose the need for evaluation of the exploitation reliability of these films. In this aspect, the durability of Cu and Ni modified anodized aluminum oxide (AAO) films on the low-doped AA1050 alloy was assessed through extended exposure to a 3.5% NaCl model corrosive medium. The electrochemical measurements by means of electrochemical impedance spectroscopy (EIS) and potentiodynamic scanning (PDS) after 24 and 720 hours of exposure have revealed that the obtained films do not change their obvious barrier properties. In addition, supplemental analyses of the coatings were performed, in order to elucidate the impact of the AC-deposition of Cu and Ni inside the pores. The scanning electron microscopy (SEM) images have shown that the surface topology is not affected and resembles the typical surface of an etched metal. The subsequent energy dispersive X-ray spectroscopy (EDX) tests have revealed a predominance of Cu in the combined AAO-Cu/Ni layers, whereas additional X-ray photoelectron (XPS) analyses showed that both metals form oxides with different oxidation states due to alterations in the deposition conditions, promoted by the application of AC-polarization of the samples.

• Journal of the Korean Ceramic Society
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• v.33 no.5
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• pp.572-582
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• 1996

The porous silicon was prepared in the condition of 70mA/cm2 and 5.10 sec and then oxidized at 800~110$0^{\circ}C$ MOS(Metal Oxide Semiconductor) structure was prepared by Al electrode deposition and analyzed by C-V (Capacitance-Voltage) characteristics. Dielectric constant of oxidized porous silicon was large in the case of low temperature (800, 90$0^{\circ}C$) and short time(20-30min) oxidation and was nearly the same as thermal SiO2 3.9 in the case of high temperature (110$0^{\circ}C$) and long time (above 60 min) It is though to be caused byunoxidized silicon in oxidized porous silicon film and capacitance increase due to surface area increment effect.

• The Journal of Korean Academy of Prosthodontics
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• v.44 no.5
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• pp.617-627
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• 2006

Statement of problem: HA has been used as a coating material on Ti implants to improve osteoconductivity. However. it is difficult to form uniform HA coatings on implants with complex surface geometries using a plasma spraying technique. Purpose : To determine if Ti6Al4V sintered porous-surfaced implants coated with HA sol-gel coated and hydrothermal treated would accelerate osseointegration. Materials and Methods : Porous implants which were made by electric discharge were used in this study. Implants were anodized and hydrothermal treatment or HA sol-gel coating was performed. Hydrothermal treatment was conducted by high pressure steam at $300^{\circ}C$ for 2 hours using a autoclave. To make a HA sol, triethyl phosphite and calcium nitrate were diluted and dissolved in anhydrous ethanol and mixed. Then anodized implant were spin-coated with the prepared HA sols and heat treated. Samples were soaked in the Hanks solution with pH 7.4 at $37^{\circ}C$ for 6 weeks. The microstructure of the specimens was observed with a scanning electron microscope (SEM), and the composition of the surface layer was analyzed with an energy dispersive spectroscope (EDS). Results : The scanning electron micrographs of HA sol-gel coated and hydrothermal treated surface did not show any significant change in the size or shape of the pores. After immersion in Hanks' solution the precipitated HA crystals covered macro- and micro-pores The precipitated Ca and P increased in Hanks' solution that surface treatment caused increased activity. Conclusion : This study shows that sol-gel coated HA and hydrothermal treatment significantly enhance the rate of HA formation due to the altered surface chemistry.