• 대한금속재료학회지
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• 제50권1호
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• pp.86-91
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• 2012

Ti-6Al-4V extra low interstitial (ELI) alloy has been widely used as an orthopedic implant material because of its excellent biocompatibility, corrosion resistance and mechanical properties. However, V-free titanium alloys such as Ti-6%Al-7%Nb and Ti-5%Al-2.5%Fe have recently been developed because of the toxicity of V. Hydroxyapatite (HA) is used as a coating material on Ti or Ti biomaterials due to its good biocompatibility. However, HA coated on Ti alloy causes a problem for tissue by peeling off during usage. Therefore, such peeling off during long time usage can be suppressed by adding HA in Ti or Ti alloy composites. The aim of this study was to manufacture an ultra fine grained (UFG) Ti-Nb-HA bulk alloy, which is usually difficult to fabricate using melting and casting technology, by rapid sintering process using high energy mechanical milled (HEMM) powder.

• Molecular & Cellular Toxicology
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• 제3권1호
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• pp.36-45
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• 2007

Several features of the implant surface, such as topography, roughness, and composition play a relevant role in implant integration with bone. This study was conducted in order to determine the effects of different-coatings on Ti surfaces on the biological responses of a human osteoblast-like cell line (MG63). MG63 cells were cultured on HA (Hydroxyapatite coating on Titanium), Ano (HA coating on anodized surface Titanium), Zr (zirconium-coating on Titanium), and control (non-coating on Titanium). The morphology of these cells was assessed by SEM. The cDNAs prepared from the total RNAs of the MG63 were hybridized into a human cDNA microarray (1,152 elements). The appearances of the surfaces observed by SEM were different on each of the three dental substrate types. MG63 cells cultured on HA, Ano, Zr, and control exhibited cell-matrix interactions. In the expression of several genes were up-, and down-regulated on the different surfaces. The attachment and expression of key osteogenic regulatory genes were enhanced by the surface morphology of the dental materials used.

• 한국표면공학회:학술대회논문집
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• 한국표면공학회 2018년도 춘계학술대회 논문집
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• pp.23-23
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• 2018

In this study, new titanium alloys were prepared by adding elements such as tantalum (Ta), zirconium (Zr) and the like to complement the biological, chemical and mechanical properties of titanium alloys. The Ti-40Ta-xZr ternary alloy was formed on the basis of Ti-40Ta alloy with the contents of Zr in the contents of 0, 3, 7 and 15 wt. %. Plasma electrolytic oxidation (PEO), which combines high-voltage sparks and electrochemical oxidation, is a novel method to form ceramic coatings on light metals such as Ti and its alloys. These oxide film produced by the electrochemical surface treatment is a thick and uniform porous form. It is also composed of hydroxyapatite and calcium phosphate-based phases, so it has the characteristics of bone inorganic, non-toxic and very high bioactivity and biocompatibility. Ti-40Ta-xZr alloys were homogenized in an Ar atmosphere at $1050^{\circ}C$ for 1 hour and then quenched in ice water. The electrochemical oxide film was applied by using a power supply of 280 V for 3 minutes in 0.15 M calcium acetate monohydrate ($Ca(CH_3COO)_2{\cdot}H_2O$) and 0.02 M calcium glycerophosphate ($C_3H_7CaO_6P$) electrolyte. A small amount of 0.0075M zinc acetate and magnesium acetate were added to the electrolyte to enhance the bioactivity. The mechanical properties of the coated surface of Ti-40Ta-xZr alloys were evaluated by Vickers hardness, roughness test, and elastic modulus using nano-indentation, and the surface wettability was evaluated by measuring the contact angle of the coated surface. In addition, cell activation and differentiation were examined by cell culture of HEK 293 (Human embryonic kidney 293) cell proliferation. Surface properties of the alloys were analyzed by scanning electron microscopy(FE-SEM), EDS, and X-ray diffraction analysis (XRD).

• 대한치과재료학회지
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• 제44권3호
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• pp.263-272
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• 2017

본 연구에서는 타이타늄 상에 항균제 클로르헥시딘(chlorhexidine; CHX)이 함유된 수산화인회석을 코팅하고 그 특성을 규명하였다. CHX를 혼합한 개조된 생체유사용액(modified simulated body fluid; mSBF)에 타이타늄 디스크를 침적하여 Ti-mSBF-CHX 시편군을 준비하였다. CHX를 함유하지 않은 mSBF에 침적하여 코팅한 Ti-mSBF 시편군을 다시 CHX 용액에 침적하여 Ti-mSBF-adCHX 시편군을 준비하였다. Ti-mSBF 시편 표면에 나노 형태의 결정들로 구성된 구형의 클러스터들이 균일하게 코팅되었다. Ti-mSBF-CHX 시편에서는 이러한 클러스터들과 함께 리본형상의 결정들이 관찰되었으며, 이 결정들에서 높은 CHX 조성이 측정되었다. 두 시편 모두 HAp 결정구조가 지배적이었으며, ${\beta}-TCP$ (tricalcium phosphate)와 OCP (octacalcium phosphate) 결정구조가 Ti-mSBF-CHX 시편에서 관찰되었다. FT-IR 스펙트럼은 Ti-mSBF-adCHX와 Ti-mSBF-CHX 시편군에서 CHX의 피크가 강하게 관찰되었다. 그러나 인산완충식염수(phosphate buffered saline;PBS)에 침적한 후, CHX가 Ti-mSBF-CHX 시편에서는 천천히 용출된 반면, Ti-mSBF-adCHX 시편에서는 빠르게 용출되었다. 따라서 Ti-mSBF-CHX 시편은 골과 유사한 HAp 구조를 가지며 함유된 CHX가 지속적으로 방출될수 있기 때문에 향후 임플란트 시술에서 염증을 방지할 수 있는 코팅법으로 기대된다.

• 한국표면공학회:학술대회논문집
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• 한국표면공학회 2016년도 추계학술대회 논문집
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• pp.195-195
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• 2016

Titanium and its alloys are widely used as implants in orthopedics, dentistry and cardiology due to their outstanding properties, such as high strength, high level of hemocompatibility and enhanced biocompatibility. 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. Silicon (Si) and magnesium (Mg) has a beneficial effect on bone. Si in particular has been found to be essential for normal bone and cartilage growth and development. In vitro studies have shown that Mg 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. The aim of this study is to research Si and Mg doped hydroxyapatite film formation by plasma electrolytic oxidation. 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. A Si and Mg coating 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 Si and Mg coated oxide surface of Ti-29Nb-xHf alloys were examined by FE-SEM, EDS, and XRD.

• 공학논문집
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• 제3권1호
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• pp.189-197
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• 1998

생체적합성이 뛰어난 Hydroxyapatite(HAp)를 Wet Chemical Process로 만든 후 Ion Beam Assisted Deposition (IBAD)를 이용하여 Ti-6Al-4V의 표면에 coating 시켰다. 그런후 5ppm, 10ppm, 20ppm, 100ppm의 $AgNO_3$용액으로 HAp의 Ca이온과 Ag이온을 치환시켰다. 본 논문에서는 Ag-HAp로 coating된 Ti-6Al-4V를 만들어 항균효과와 생체적합성을 연구하였다. 먼저 생체 대체재료 이식수술시 감염이 큰 2가지 종류의 bacteria (P. Aeruginosa, S. Epidermidis)로 항균 test를 하였고, 그 결과 20ppm의 $AgNO_3$로 처리한 Ti-6Al-4V에서 우수한 항균성이 관찰되었다. 또한 생체적합성 연구을 위해 osteoblast와 macrophages로 생체적합성 실험을 하여 SEM으로 관찰한 결과, 5ppm과 10ppm의 $AgNO_3$로 처리한 Ti-6Al-4V 에서 좋은 생체적합성을 보였다. HAp의 Ca 이온에 치환된 Ag 이온의 항균원리를 관찰하기 위하여, 가장 일반적인 bacteria인 E. coli를 Ag-HAp로 처리한 후 transmission electron microscope (TEM)으로 관찰하였다. Ag-HAp로 처리한 E. coli에서 cell wall과 cytoplasm이 파괴된 것이 관찰되었고, cytoplasm에서는 검은점이 발견되었다. 이 검은점을 Energy dispersive analysis X-ray (EDAX)로 분석한 결과 미량의 Ag이온이 검출되었다. 이로써 Ag 이온이 효과적으로 Bacteria를 파괴하여 항균효과를 나타내는 것을 알 수 있었다.

• 한국표면공학회:학술대회논문집
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• 한국표면공학회 2016년도 추계학술대회 논문집
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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.

• Journal of Periodontal and Implant Science
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• 제47권4호
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• pp.219-230
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• 2017

Purpose: The purpose of this study was to compare the characteristics of single- and dualspecies in vitro oral biofilms made by static and dynamic methods. Methods: Hydroxyapatite (HA) disks, 12.7 mm in diameter and 3 mm thick, were coated with processed saliva for 4 hours. The disks were divided into a static method group and a dynamic method group. The disks treated with a static method were cultured in 12-well plates, and the disks in the dynamic method group were cultured in a Center for Disease Control and Prevention (CDC) biofilm reactor for 72 hours. In the single- and dual-species biofilms, Fusobacterium nucleatum and Porphyromonas gingivalis were used, and the amount of adhering bacteria, proportions of species, and bacterial reduction of chlorhexidine were examined. Bacterial adhesion was examined with scanning electron microscopy (SEM) and confocal laser scanning microscopy (CLSM). Results: Compared with the biofilms made using the static method, the biofilms made using the dynamic method had significantly lower amounts of adhering and looser bacterial accumulation in SEM and CLSM images. The proportion of P. gingivalis was higher in the dynamic method group than in the static method group; however, the difference was not statistically significant. Furthermore, the biofilm thickness and bacterial reduction by chlorhexidine showed no significant differences between the 2 methods. Conclusions: When used to reproduce periodontal biofilms composed of F. nucleatum and P. gingivalis, the dynamic method (CDC biofilm reactor) formed looser biofilms containing fewer bacteria than the well plate. However, this difference did not influence the thickness of the biofilms or the activity of chlorhexidine. Therefore, both methods are useful for mimicking periodontitis-associated oral biofilms.

• 치위생과학회지
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• 제11권5호
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• pp.405-410
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• 2011

본 연구의 목적은 표면 거칠기를 증가시키기 위하여 알루미나와 하이드록시아파타이트를 이용하여 각각 블라스팅 처리한 뒤 염화나트륨을 전해액 내에 섞어 양극산화 방법을 이용하여 염소가 함유된 표면을 만들고 항균력을 평가하는데 있다. 그리고 표면 특성과 항균력을 평가하여 다음과 같은 결과를 얻었다. 1. SEM 표면 관찰에서는 블라스팅 처리 후 양극산화한 결과 실험군 2와 3에서 연마처리한 실험군 1에 비해 거친 요철구조를 관찰할 수 있었다. 2. EDS 조성분석 결과 실험군 2에서는 칼슘, 인, 염소 성분과 더불어 알루미늄이 관찰된 반면, 실험군 3에서는 칼슘, 인과 염소 성분만을 관찰할 수 있었다. 3. 표면 거칠기 분석 결과 평균 표면 거칠기의 값이 실험군 2, 실험군 3, 실험군 1순으로 작았으며, 실험군 2와 3 간에는 유의한 차이가 없었다(p>0.05). 4. 항균력 평가 결과 실험군 2가 가장 적은 세균수를 보여 우수한 항균력을 보였으나 이는 실험군 3과 유의한 차이가 없었다(p>0.05). 알루미나와 하이드록시아파타이트를 이용하여 각각 블라스팅 처리한 뒤 염화나트륨을 전해액 내에 섞어 양극산화 방법을 이용하여 염소가 함유된 표면을 만들 수 있었으며, 그 결과 연마처리한 시편에 비해 높은 표면 거칠기와 우수한 항균력을 보였다. 그러나 그 재료의 효과와 안정성을 입증하기 위해서는 추가적인 in vitro와 in vivo 실험이 수행되어야겠다.