• 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.

• 대한치과보철학회지
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• 제42권5호
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• pp.556-571
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• 2004

Statement of problem: Surface texture of the implant is one of the important factors of the implant success, especially in the immediate implant loading. Many methods of the surface treatment of implant have developed and introduced. Purpose : This study was to evaluate the effects of the Ca-P coating implant crystallized the hydroxyapatite on the surface by the removal torque test and the histomorphometric analysis in vivo. Material and methods: 135 screw type implants, 4.0mm in length and 3.75mm in diameter were used in this study. Implants were divided into 3 groups and treated in the different mothods. Group I was not treated, Group II was treated in the SLA method, and Group III was treated in the Ca-P coating with the anodizing method and the hydroxyapatite was crystallized on the surface with the hydrothermal treatment. Firstly, the surface roughness of each group was measured, 45 rabbits were used in this experiment. Two implants were inserted on right tibial metaphysis and one implant was inserted on left side with the alternating order. After the healing periods of 3, 5, and 12 weeks, the rabbits were sacrificed to evaluate the osseointergration by the removal torque test and the histomorphometric analysis. Results : 1. In the analysis for the surface roughness, Group II showed the highest roughness. And Group III showed higher secondly. There was a significant difference one another statistically 2. In the removal torque test, Group III and II were significantly higher than Group I. There was no statistical difference between Group III and Group II. 3. For all Groups, the removal torque values at 12th week were significantly higher than at 3rd and 5th week. 4. In histomorphometric analysis, the bone implant contact rates of Group III and II were higher than that of Group I at 3rd and 5th week. There was a significant difference at 5th week. 5. In histomorphometric analysis, the bone implant contact rate of Group III and II increased from 3rd week to 5th week, but decreased at 12th week. In Group I, the contact rate at 12th week was significantly higher than at 3rd week and 5th week.

• 한국융합학회논문지
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• 제12권12호
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• pp.145-151
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• 2021

Ti Gr4에 TPS 법을 이용하여 HA 코팅을 수행하여 코팅층에 대한 물리적특성 및 생체적합성을 판단하여 의료용 부품으로서의 활용성에 대한 평가를 하였다. 직경 25mm Ti Gr4 합금 시험편을 기계가공 후 #120, #400, #1,000 샌드페이퍼 및 바렐 연마로 표면을 연마를 하여 ASTM F1185-88로 HA 코팅은 한 후 HA 코팅층의 두께, 표면조도, 강도 및 접착력 측정 시험과 세포독성 시험을 하였다. Ti Gr4에 대한 HA 코팅 결정도는 75.51%, Ca/P 비는 1.67의 값을 얻을 수 있었다. HA 코팅층의 두께는 Ti 소재의 표면거칠기가 거칠수록 증가하고, 코팅의 강도 및 접착력은 시험장치의 지그 형상, 에폭시 성분, 크로스헤드 속도 등에 따라 변화가 있을 것으로 예측된다. 세포독성 시험은 Grade 3의 반응성으로 적합한 것으로 나타났다. 본 실험 결과 TPS에 의한 Ti Gr4 소재의 HA 코팅 두께 향상과 골융합을 촉진이 가능할 것으로 확인되어 인체삽입용으로 상용화가 가능할 것으로 판단된다.

• 대한의용생체공학회:학술대회논문집
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• 대한의용생체공학회 1996년도 춘계학술대회
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• pp.133-136
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• 1996

We investigated how hydroxyapatite (HA) coating onto a porous super stainless steel (S.S.S, 22Cr-20Ni-6Mo-0.25N) affects bone ingrowth in a dog transcortical femoral model. Implants were histologically evaluated after 4 and 48 weeks of implantation, and the bone bonding strength at the bone/implant interface was examined by employing the pull-out test. The direct osseous tissue bonding onto the HA-coated S.S.S was observed, but the uncoated stainless steels had thin fibrous tissue layers. The mean interface strength of the HA-coated S.S.S was 1.5 and 2.5 times greater than those of the S.S.S and the 316L SS after one year of implantation, respectively. In preliminary studies, no toxic responce was observed from a cytotoxicity test of the S.S.S, having similar corrosion resistance to titanium. Our results suggest that early osteoconductive nature of HA coating may induce long term osteointegration for a bioinert substrate.

• 대한금속재료학회지
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• 제50권5호
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• pp.395-400
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• 2012

In this study, we have investigated the surface morphology of hydroxyapatite (HA) coated Ti alloy surface using pulsed laser plating. The HA (tooth ash) films were grown by pulsed KrF excimer laser, film surfaces were analyzed for topology, chemical composition, crystal structure and electrochemical behavior. The Ti-6Al-4V alloy showed ${\alpha}$ and ${\beta}$ phase, Cp-Ti showed ${\alpha}$ phase and the HA coated surface showed HA and Ti alloy peaks. The HA coating layer was formed with $1-2{\mu}m$ droplets and grain-like particles, particles which were smaller than the HA target particle, and the composition of the HA coatings were composed of Ca and P. From the electrochemical test, the pitting potential (1580 mV) of HA coated Ti-6Al-4V alloy was higher than those of Cp-Ti (1060 mV) and HA coated Cp-Ti (1350 mV). The HA coated samples showed a lower current density than non-HA coated samples, whereas, the polarization resistance of HA coated samples showed a high value compared to non-HA coated samples.

• 대한화학회지
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• 제57권4호
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• pp.493-498
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• 2013

리포솜은 표적 약물을 봉입하여 병소에 안전하게 전달할 수 있는 약물전달체로서 연구되고 있다. 그러나 일반적인 리포솜은 표적부위에서 약물방출이 제한적인 문제점이 있다. 따라서 본 연구에서는 리포솜의 안정성을 향상시키고 표적부위에서 외부 초음파로부터 약물의 방출을 극대화시키기 위하여 하이드록시아파타이트(hydroxyapatite, HA)가 코팅된 리포솜을 개발하였다. 대조군 리포솜은 인지질과 콜레스테롤을 이용하여 제조하였고, 대조군 리포솜의 표면에 칼슘 아세테이트, 포스포릭에시드, 그리고 25% 암모니아용액을 이용하여 HA를 코팅하였다. 모델 약물로는 독소루비신을 사용하였다. HA코팅 리포솜의 크기는 120 nm 이었고, 약물봉입효율은 95% 이상이었다. 30% 혈장용액 내에서 HA코팅 리포솜의 입자크기는 일정한 상태를 유지하였으며, 대조군 리포솜은 크기가 1.4배 증가하였다. 외부 초음파 자극에 의한 리포솜으로부터 약물 방출을 유도한 후, 방출된 약물의 세포 이입율은 HA 코팅된 리포솜이 3배 이상 대조군 리포솜에 비하여 증가하였다. 본 연구에서는 외부 초음파 자극에 의하여 리포솜으로부터 약물의 방출을 극대화시키기 위한 초음파 민감형 리포솜을 개발하였고, 본 제형은 표적부위에서 약물의 방출을 효과적으로 제어하기 위한 분야에 활용이 가능할 것이다.

• Journal of Periodontal and Implant Science
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• 제23권3호
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• pp.400-410
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• 1993

Dental implants have been widely used in the treatment of esthetic and functional problems of the mouth due to alveolar bone loss, after tooth extraction. The success of implantation strongly depends on osseointegration. For osseointegration, implant material, methodology, and design have been investigated. For materials, two popular materials at present are titanium and hydroxyapatite. For methods, immediate implantation is being used recently. The purpose of this study is to evaluate osseointegration between the unthreaded cylindrical TPS implant and the HA-coated implant by a histomorphometric analysis. For this analysis, experimental periodontits was induced on the 3, 4 premolars of adult dogs by the ligation of orthodontic threads. Thereafter, each tooth was extracted. TPS. Implants and HA-coated implants were immediately inserted in the extraction socket. In control group, TPS implants were immediately inserted, and In experimental group, HA implants were immediately inserted. The dogs were sacrificed after 12 weeks, then the specimens were prepared for LM and histomorphometric analysis. The conclusion of this study is as follows l. In both control and experimental group, no inflammatory cells were observed. 2. The results of the histomorphometric analysis showed that the total osseointegration was 48.5% in control group, and 68.8% in expermental group. The experimental group was higher than the control group, and the difference was not statistically significant (p<0.05). 3. The results of the histomorphometric analysis showed that the osseointegration in the hole was 40.6% in control group, and 70.2% in experimental group. The experimental group was higher than the control group, and the difference was statistically significant (p<0.05). In both control and experinental group, no inflammatory cells were observed. 4. The results of the histomorphometric analysis showed that the osseointegration in the lower part was 52.1% in control group, and 73.3% in experimental group. The experimental group was higher than the control group, and the difference was statistically significant (p<0.05). 5. In experimental group, the bone to HA interface seemed to be mixed of bone and HA. We could not distinguish HA from the bone. The HA coating was detached from the titanium surface.

• 한국표면공학회:학술대회논문집
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• 한국표면공학회 2009년도 춘계학술대회 논문집
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• pp.162-163
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• 2009

마이크로플라즈마 스프레이(Microplasma spray, MPS)를 이용하여 hydroxyapatite(HA) 코팅을 수행하여, HA코팅 층에 대한 밀착력을 측정하였다. 밀착력의 측정은 ASTM C633에 의거하였으며, 실험의 설계는 다꾸치법 (L18($2^{1}3^{7}$))을 이용하였다. 본 실험에서 HA코팅 층과 모재에 대한 밀착력 측정에서 35.8MPa의 밀착력을 얻었으며, SEM을 이용하여, 표면 형상과 밀착력 실험 후의 파단면을 관찰하였다. 또한, 나노 인덴테이션을 사용하여, 탄성계수와 미소경도를 측정하였다.

• 한국진공학회지
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• 제6권S1호
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• pp.27-33
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• 1997

Recently ion beam assistant deposition (IBAD) was successfully used to produce a dense ultra-adherent and pinhole-free hydroxyapatite (HAp) layer on alumina substrate. After that the HAp-coated alumina was immersed in 20ppm and 100ppm $AgNO_3$ solution at room temperature for 48 hours to carry out the ions exchange between $Ag^+\;and\;Ca^+$ in HAp. The obvious antimicrobial effect against E.Coli, P. Aeruginosa and S. Epidermidis was observed in the samples treated with 20ppm $AgNO_3$ Solution, In contrast to this the untreated samples did not show any bactericidal effect. Scanning electron microscope(SEM) study showed that Ag homogeneously distributed on the surface. X-ray diffraction (XRD) demonstrated that the surface structure in the samples without Ag was HAp whereas with Ag is HAp and AgCaP. It appears that silver ions exchange with calcium ions in HAp does not cause significant changes in the structure of HAp coatings.

• 한국재료학회지
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• 제21권7호
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• pp.384-390
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• 2011

Ti-6Al-4V ELI (Extra Low Interstitial) alloy has been widely used as an alternative to bone due to its excellent biocompatibility. However, it still has many problems, including a high elastic modulus and toxicity. Therefore, nontoxic biomaterials with a low elastic modulus should be developed. However, the fabrication of a uniform coating is challenging. Moreover, the coating layer on Ti and Ti alloy substrates can be peeled off after implantation. To overcome these problems, it is necessary to produce bulk Ti and Ti alloy with hydroxyapatite (HA) composites. In this study, Ti, Nb, and Zr powders, which are biocompatible elements, were milled in a mixing machine (24h) and by planetary mechanical ball milling (1h, 4h, and 6h), respectively. Ti-35%Nb-7%Zr and Ti-35%Nb-7%Zr-10%HA composites were fabricated by spark plasma sintering (SPS) at $1000^{\circ}C$ under 70MPa using mixed and milled powders. The effects of HA addition and milling time on the biocompatibility and physical and mechanical properties of the Ti-35%Nb-7%Zr-(10%HA) alloys have been investigated. $Ti_2O$, CaO, $CaTiO_3$, and $Ti_xP_y$ phases were formed by chemical reaction during sintering. Vickers hardness of the sintered composites increases with increased milling time and by the addition of HA. The biocompatibilty of the HA added Ti-Nb-Zr alloys was improved, but the sintering ability was decreased.