• Journal of the Korean Society for Heat Treatment
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• v.31 no.1
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• pp.6-11
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• 2018

The anodic oxidation behavior of Si-containing aluminum alloy for diecasting was investigated. Especially, the property changes during anodization both on aluminum 1050 and 9 weight percentage silicon containing aluminum (Al-9Si) alloys were analyzed by the static current test. In order to fabricate a uniform anodic oxidation film by effect of Al-Si compound, nitric acid containing hydrofluoric acid had been used as a desmutter for aluminum alloy after alkaline etching. It was found that the level of voltage of Al-9Si alloy during the static current test was almost as double as higher than aluminum 1050 through anodization. By adding hydrofluoric acid in the nitric acid electrolyte, the silicon compound on the surface was removed, and the optimum amount of added hydrofluoric acid could be derived. It was also observed that the size of silicon compound formed on the surface could be refined by heat treatment at $500^{\circ}C$ and followed water quenching.

• Korean Journal of Materials Research
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• v.14 no.12
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• pp.876-884
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• 2004

This study was to investigate whether the bioactivity of the anodized and hydrothermally treated Ti-6Al-7Nb alloy were affected by the time of hydrothermal treatment. Anodizing was performed at current density 30 $mA/cm^2$ up to 300 V in electrolyte solutions containing $DL-{\alpha}-glycerophosphate$ disodium salt hydrate $(DL-{\alpha}-GP)$ and calcium acetate (CA). Hydrothermal treatment was done at $300^{\circ}C$ for 30 min, 1 hr, 2 hrs, and 4 hrs to produce a thin film layer of hydroxyapatite (HA). The bioactivity was evaluated from HA formation on the surfaces in a Hanks' solution with pH 7.4 at $36.5^{\circ}C$ for 10, 20, and 30 days. Anodic oxide films were porous with pore size of $1\sim4{\mu}m\;and\;3\sim4{\mu}m$ thickness. The anodic oxide films composed with strong anatase peak with presence of rutile peak, and showed the increase in intensity of anatase peak after hydrothermal treatment. It was shown that the intensity of anatase peak increased with increasing the time of hydrothermal treatment but was no difference in rutile peak. The corrosion voltage was the highest in the group of hydrothermal treatment for 2 hrs (Ecorr: -338.6 mV). The bioactivity in Hank's solution was accelerated with increasing the time of hydrothermal treatment.

• The Journal of Korean Academy of Prosthodontics
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• v.43 no.5
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• pp.684-693
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• 2005

Statement of problem: Ti-6Al-7Nb alloy is used instead of Ti-6Al-4V alloy that was known to have toxicity. Purpose: This study was performed to investigate the effect of electrolyte concentration on the surface characteristics of anodized and hydrothermally-treated Ti-6Al-7Nb alloy Materials and methods: Discs of Ti-6Al-7Nb alloy of 20 mm in diameter and 2 mm in thickness were polished sequentially from #300 to 1,000 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 at current density $30mA/cm^2$ up to 300 V in electrolyte solutions containing $\beta-glycerophosphate$ disodium salt hydrate $(\beta-GP)$ and calcium acetate (CA). Hydrothermal treatment was conducted by high pressure steam at $300^{\circ}C$ for 2 hours using a autoclave. All samples were soaked in the Hanks' solution with pH 7.4 at $36.5^{\circ}C$ for 30 days. Results and conclusion: The results obtained were summarized as follows: 1. After hydrothermal treatment, the precipitated HA crystals showed the dense fine needle shape. However, with increasing the concentration of electrolyte they showed the shape of thick and short rod. 2. When the dense fine needle shape crystals was appeared after hydrothermal treatment, the precipitation of HA crystals in Hanks' solution was highly accelerated. 3. The crystal structures of $TiO_2$ in anodic oxide film were composed of strong anatase peak and weak rutile peak as analyzed with thin-film X-ray diffractometery. 4. The Ca/P ratio of the precipitated HA layer was equivalent to that of HA crystal in Hanks' solution.

• Corrosion Science and Technology
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• v.8 no.4
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• pp.143-147
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• 2009

In biomedical implants and dental fields, titanium has been widely utilized for excellent corrosion resistance and biocompatibility. However, Ti and its alloys are nonbioactive after being implanted in bone. In this study, for the purpose of improvement in biocompatibility the anodic $TiO_2$ layer on Ti-xNb alloys were fabricated by electrochemical method in phosphate solution, and the effect of Nb content on the pore size, the morphology and crystallinity of Ti oxide layer formed by the anodic oxidation method was investigated. The Ti containing Nb up to 3 wt%, 20 wt% and 40 wt% were melted by using a vacuum furnace. The sample were cut, polished, and homogenized for 24 hr at $1050^{\circ}C$ for surface roughness test and anodizing. Titanium anodic layer was formed on the specimen surface in an electrolytic solution of 1 M phosphoric acid at constant current densities ($30mA/cm^2$) by anodizing method. Microstructural morphology, crystallinity, composition, and surface roughness of oxide layer were observed by FE-SEM, XRD, EDS, and roughness tester, respectively. The structure of alloy was changed from $\alpha$-phase to $\beta$-phase with increase of Nb content. From XRD results, the structure of $TiO_2$ formed on the Ti-xNb surface was anatase, and no peaks of $Nb_2O_5$ or other Nb oxide were detected suggesting that Nb atoms are dispersed in $TiO_2$-based solid solution. Surface roughness test and SEM results, pore size formed on surface and surface roughness decreased as Nb content increased. From the line analysis results, intensity of Ti peak was high in the center of pore, whereas, intensity of O peak was high in the outside of pore center.

• Journal of the Korean Chemical Society
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• v.57 no.5
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• pp.547-553
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• 2013

Zirconium oxide ($ZrO_2$) nano porous membranes were fabricated by electrochemical two-step anodization with an electropolished zirconium substrate in inorganic water-based and organic electrolyte systems containing small amounts of fluoride. Using two-step anodization and organic electrolytes, highly regular and ordered nanotubular $ZrO_2$ oxide layers can be compared with aqueous electrolytes. The morphology and size of the nano porous layers were characterized by FE-SEM (field emission scanning electron microscopy), XRD (X-ray diffraction), and EDS (energy dispersive spectroscopy). Luminescence properties were investigated by photoluminescence measurements.

• Proceedings of the Korean Vacuum Society Conference
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• 2010.02a
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• pp.329-329
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• 2010

반도체 및 디스플레이의 진공부품은 알루미늄 모제에 전해연마법(electrolytic polishing), 양극산화피막법(Anodizing), 플라즈마 용사법(Plasma spray) 등을 사용하여 $Al_2O_3$ 피막을 성장시켜 사용되고 있다. 반도체 제조공정 중 30~40% 이상의 비중을 차지하는 식각(etching) 및 증착(deposition) 공정은 대부분 플라즈마를 사용하고 있다. 플라즈마에 의해 화학적, 물리적 침식이 발생하여 코팅막에 손상을 일으켜 코팅막이 깨지거나 박리되면서 다량의 Particle을 생성함으로써 생산수율에도 문제를 야기 시킨다고 알려져 있다. 하지만 이들 코팅막을 평가하는 방법은 거의 전무하여 산업계에서 많은 애로를 겪고 있다. 이러한 코팅부품의 내플라즈마 성능평가 방법과 기준이 없어 적절한 교체시기를 파악하기 위한 코팅부품의 손상정도를 정량화 및 평가 방법의 표준화를 구축하는 연구를 수행하였다. 본 연구에서는 이러한 소재의 특성평가를 위해 공정에서 사용 중 손상되어 교체된 샘플의 모폴로지 관찰하고 내전압 측정으로 전기적 특성을 분석하여 손상 전, 후의 변화를 관찰하였다. 또한 플라즈마의 영향에 따른 코팅 막 형태 변화 및 전기적 특성의 변화를 알아보기 위하여 양극산화피막법(Anodizing)으로 $Al_2O_3$를 성장시킨 평가용 샘플을 제작한 후, Plasma chamber 장비를 이용하여 플라즈마 처리에 따른 코팅막의 내전압, 식각율, 표면 미세구조의 변화를 측정하였고 이를 종합적으로 고려하여 진공 장비용 코팅부품의 공정영향에 의한 내플라즈마 특성평가방법 개발에 관하여 연구하였다. 이러한 실험을 통해 플라즈마 처리 후 코팅 막에 크랙이 발생되는 것을 확인할 수 있었고 코팅 막의 손상으로 전기적 특성이 감소를 것을 확인할 수 있었다. 또한 ISPM 장비를 이용하여 진공 장비용 코팅부품이 플라즈마 공정에서 발생하는 오염 입자를 측정할 수 있는 방법을 연구하였다. 이러한 결과를 이용하여 진공공정에서 사용되는 코팅부품이 플라즈마에 의한 손상정도를 정량화 하고 평가방법을 개발하여 부품 양산업체의 진공장비용 코팅부품 개발 신뢰성 향상이 가능할 것으로 본다.

• Korean Journal of Materials Research
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• v.24 no.5
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• pp.259-265
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• 2014

$ZrO_2$ films were coated on aluminum etching foil by the sol-gel method to apply $ZrO_2$ as a dielectric material in an aluminum(Al) electrolytic capacitor. $ZrO_2$ films annealed above $450^{\circ}C$ appeared to have a tetragonal structure. The withdrawal speed during dip-coating, and the annealing temperature, influenced crack-growth in the films. The $ZrO_2$ films annealed at $500^{\circ}C$ exhibited a dielectric constant of 33 at 1 kHz. Also, uniform $ZrO_2$ tunnels formed in Al etch-pits $1{\mu}m$ in diameter. However, $ZrO_2$ film of 100-200 nm thickness showed the withstanding voltage of 15 V, which was unsuitable for a high-voltage capacitor. In order to improve the withstanding voltage, $ZrO_2$-coated Al etching foils were anodized at 300 V. After being anodized, the $Al_2O_3$ film grew in the directions of both the Al-metal matrix and the $ZrO_2$ film, and the $ZrO_2$-coated Al foil showed a withstanding voltage of 300 V. However, the capacitance of the $ZrO_2$-coated Al foil exhibited only a small increase because the thickness of the $Al_2O_3$ film was 4-5 times thicker than that of $ZrO_2$ film.

• Korean Journal of Metals and Materials
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• v.50 no.2
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• pp.164-170
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• 2012

Nanotubular structure formation on the Ti-6Al-4V and Ti-Ta alloy surfaces by electrochemical methods has been studied using the anodizing method. A nanotube layer was formed on Ti alloys in 1.0 M $H_3PO_4$ electrolyte with small additions of $F^-$ ions. The nanotube nucleation and growth of the ${\alpha}$-phase and ${\beta}$-phase appeared differently, and showed different morphology for Cp-Ti, Ti-6Al-4V and Ti-Ta alloys. In the ${\alpha}$-phase of Cp-Ti and martensite ${\alpha}^{\prime}$ and in the ${\alpha}^{{\prime}{\prime}}$ and ${\beta}$-phase of the Ti-Ta alloy, the nanotube showed a clearly highly ordered $TiO_2$ layer. In the case of the Ti-Ta alloy, the pore size of the nanotube was smaller than that of the Cp-Ti due to the ${\beta}$-stabilizing Ta element. In the case of the Ti-6Al-4V alloy, the ${\alpha}$-phase showed a stable porous structure; the ${\beta}$-phase was dissolved entirely. The nanotube with two-size scale and high order showed itself on Ti-Ta alloys with increasing Ta content.

• Journal of the Microelectronics and Packaging Society
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• v.26 no.1
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• pp.35-39
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• 2019

To date, porous alumina structures have been implemented by electrochemical anodization technique. The anodizing methods can easy to make a porous aluminum oxide film with a regular arrangement, but oxide film with complex structure type such as pillar-on-pore is relatively difficult to implement. Therefore, this study aims to observe the change of anodized oxide pore size, thickness, and structure in a phosphoric acid solution according to applied anodization voltage conditions. For the implementation of hybrid composite oxide structures, it is possible to create by modulating anodization voltage. The experimental conditions were performed at the applied anodization voltage of 100 V and 120 V in 10% phosphoric acid solution, respectively. The experimental results were able to observe the structure of oxides in the form of porous and composite structures (pillar-on-pore), depending on each condition.

• Korean Journal of Metals and Materials
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• v.46 no.11
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• pp.747-754
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• 2008

Recently, the requirement for the ultra thin copper foil increases with smaller and miniaturized electronic components. Therefore, it is important to examine the surface state of substrate depending on the processing parameter during the anodic oxidation. This study investigated the effect of the various electrolyte concentrations on anodizing of titanium anode prior to copper electrodeposition. Different surface morphology of anodized titanium was obtained at different electrolytic concentration 0.5 M to 3.0 M. In addition, the effect that the surfaces and the electrical characteristics on the electrodeposited copper layer was observed. In this study, surface anodized in the group containing 0.5M $H_2SO_4$ shows more uniform copper crystals with low surface roughness. the surface roughness and sheet resistance for 0.5M $H_2SO_4$ group were $1.353{\mu}m$ and $0.104m{\Omega}/sq$, respectively.