• 한국표면공학회지
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• 제41권2호
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• pp.57-62
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• 2008

Electrochemical properties of Ti-30Ta-$(3{\sim}15)$Nb alloys coated by HA/Ti compound layer have been studied by various electrochemical method. Ti-30Ta binary alloys contained 3, 7, 10, and 15 wt% Nb contents were manufactured by the vacuum furnace system. The specimens were homogenized for 24 hrs at $1000^{\circ}C$. The samples were cut and polished for corrosion test and coating. It was coated with HA/Ti compound layer by magnetron sputter. The HA/Ti non-coated and coated morphology of Ti alloy were analyzed by x-ray diffractometer(XRD) and filed emission scanning electron microscope(FE-SEM). The corrosion behaviors were investigated using potentiodynamic method in 0.9% NaCl solution at $36.5{\pm}1^{\circ}C$. The homoginazed Ti-30Ta-$(3{\sim}15wt%$)Nb alloys showed the ${\alpha}+{\beta}$ phase, and ${\beta}$ phase peak was predominantly appeared with increasing Nb content. The microstructure of Ti alloy was transformed from needle-like structure to equiaxed structure as Nb content increased. HA/Ti composite surface showed uniform coating layer with 750 nm thickness. The corrosion resistance of HA/Ti composite coated Ti-alloys were higher than those of the non-coated samples in 0.9% NaCl solution at $36.5{\pm}1^{\circ}C$. Especially, corrosion resistance of Ti-Ta-Nb system increased as Nb content increased.

• International Journal of Oral Biology
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• 제37권1호
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• pp.9-16
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• 2012

The aim of this study was to evaluate surface characteristics and biological properties of the dentin -derived hydroxyapatite (HA) coating on titanium substrate. Dentinderived HA was obtained from extracted human teeth using a calcination method at $850^{\circ}C$. The commercially pure titanium (cp-Ti, ASTM Grade II) was used as a metallic substrate and a radio frequency magnetron sputtering method was employed as a coating method. Scanning electron microscopy (SEM) and energy dispersive X-ray analysis (EDX) were utilized to investigate the coating aspects and composition. Atomic forced microscopy (AFM) and a surface profiler were used to assess the surface morphology and roughness. Corrosion tests were performed in phosphate-buffered saline at a $36.5{\pm}1^{\circ}C$ in order to determine the corrosion behavior of the uncoated and coated specimens. The biocompatibility of dentin-derived HA coated specimens with fetal rat calvarial cells and human gingival fibroblasts was assessed by SEM and cell proliferation analysis. The results showed that the dentin-derived HA coatings appeared to cover thinly and homogeneously the surfaces without changing of the titanium substrate. The EDX analysis of this the coating surface indicated the presence of Ca and P elements. The mean surface roughness of cp-Ti and dentin-derived coating specimens was $0.27{\mu}m$ and, $1.7{\mu}m$, respectively. Corrosion tests indicated a stable passive film of the dentin-derived HA coating specimens. SEM observations of fetal rat calvarial cells and human fibroblast cells on coated surfaces showed that the cells proliferated and developed a network of dense interconnections. The cells on all specimens proliferated actively within the culture period, showing good cell viability. At day 1 and 3, dentin-derived coating specimens showed 89% and 93% cell viability, respectively, when normalized to cp-Ti specimens. These results suggest that dentin-derived HA coating using the RF magnetron sputtering method has good surface characteristics and biocompatibility.

• Journal of Periodontal and Implant Science
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• 제40권6호
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• pp.276-282
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• 2010

Purpose: The present study was performed to evaluate the effect of erbium:yttrium-aluminium-garnet (Er:YAG) laser irradiation on the change of hydroxyapatite (HA)-coated implant surface microstructure according to the laser energy and the application time. Methods: The implant surface was irradiated by Er:YAG laser under combination condition using the laser energy of 100 mJ/pulse, 140 mJ/pulse and 180 mJ/pulse and application time of 1 minute, 1.5 minutes and 2 minutes. The specimens were examined by surface roughness evaluation and scanning electron microscopic observation. Results: In scanning electron microscope, HA-coated implant surface was not altered by Er:YAG laser irradiation under experimental condition on 100 mJ/pulse, 1 minute. Local areas with surface melting and cracks were founded on 100 mJ/pulse, 1.5 minutes and 2 minutes. One hundred forty mJ/pulse and 180 mJ/pulse group had surface melting and peeling area of HA particles, which condition was more severe depending on the increase of application time. Under all experimental condition, the difference of surface roughness value on implant surface was not statistically significant. Conclusions: Er:YAG laser on HA-coated implant surface is recommended to be irradiated below 100 mJ/pulse, 1 minute for detoxification of implant surface without surface alteration.

• Journal of Periodontal and Implant Science
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• 제46권5호
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• pp.337-349
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• 2016

Purpose: The aim of this study was to compare and analyze the peri-implant tissue conditions and prospective clinical outcomes associated with 2 types of hydroxyapatite (HA)-coated implants: (1) fully HA-coated implants and (2) partially HA-coated implants with resorbable blast medium on the coronal portion of the threads. Methods: Forty-four partially edentulous patients were randomly assigned to undergo the placement of 62 HA-coated implants, and were classified as the control group (partially HA-coated, n=30) and the test group (fully HA-coated, n=32). All patients had chronic periodontitis with moderate crestal bone loss around the edentulous area. The stability and clinical outcomes of the implants were evaluated using the primary and secondary implant stability quotient (ISQ), as well as radiographic, mobility, and peri-implant soft tissue assessments around the implants. The Wilcoxon signed-rank test and the Mann-Whitney test were used to evaluate differences between and within the 2 groups, with P values <0.05 considered to indicate statistical significance. Results: The fully HA-coated implants displayed good retention of crestal bone, and insignificant differences were found in annual marginal bone loss between the 2 types of HA-coated implants (P>0.05). No significant differences were found in the survival rate (group I, 100%; group II, 100%) or the success rate (group I, 93.3%; group II, 93.8%). The fully HA-coated implants also did not significantly increase the risk of peri-implantitis (P>0.05). Conclusions: The fully HA-coated implants did not lead to an increased risk of peri-implantitis and showed good retention of the crestal bone, as well as good survival and success rates. Our study suggests that fully HA-coated implants could become a reliable treatment alternative for edentulous posterior sites and are capable of providing good retention of the crestal bone.

• 한국표면공학회지
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• 제41권5호
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• pp.181-188
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• 2008

A.C. impedance properties of HA/Ti compound layer coated Ti-30Ta-($3{\sim}15$)Nb alloys have been studied by electrochemical method. Ti-30Ta binary alloys contained 3, 7, 10 and 15 wt% Nb were manufactured by the vacuum furnace system. And then specimen was homogenized at $1000^{\circ}C$ for 24 hrs. The sample was cut and polished for corrosion test and coating. It was coated with HA/Ti compound layer by magnetron sputter. The non-coated and coated morphology of Ti alloy were analyzed by X-ray diffractometer (XRD), energy X-ray dispersive spectroscopy (EDX) and filed emission scanning electron microscope (FE-SEM). The corrosion behaviors were investigated using A.C. impedance test (PARSTAT 2273, USA) in 0.9% NaCl solution at $36.5{\pm}1^{\circ}C$. Ti-30Ta-($3{\sim}15\;wt%$)Nb alloys showed the ${\alpha}+{\beta}$ phase, and $\beta$ phase peak was predominantly appeared in the case of increasingly Nb contents. The microstructures of Ti alloy were transformed from needle-like structure to equiaxed structure as Nb content increased. From the analysis of coating surface, HA/Ti composite surface uniformed coating layer with 750 nm thickness. The growth directions of film were (211), (112), (300) and (202) for HA/Ti composite coating on the surface after heat treatment at $550^{\circ}C$, whereas, the growth direction of film was (110) for Ti coating. The polarization resistance ($R_p$) of HA/Ti composite coated Ti-alloys were higher than those of the Ti and HA coated samples in 0.9% NaCl solution at $36.5{\pm}1^{\circ}C$. Especially, corrosion resistance of Ti-Ta-Nb system increased as Nb content increased.

• 대한치과보철학회지
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• 제41권3호
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• pp.271-287
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• 2003

Statement of problem: Resonance frequency analysis (RFA) has been increasingly served as a non-invasive and objective method for clinical monitoring of implant stability. Many clinical studies must be required for standardized baseline data using RFA. Purpose: This study was performed to evaluate RFA value changes in two stage surgery group and one stage surgery group in patients. Material and method: Forty-seven mandibles in consecutively implant installed patients were selected for this study and 141 fixtures were installed. Ninety-three fixtures were double threaded, machined surface design ($Br{\aa}anemark^{(R)}$ MK III, Nobel Biocare AB, Goteborg, Sweden) and 48 fixtures were root form, threaded, HA-coated surface one ($Replace^{TM}$, Steri-Oss/Nobel Biocare AB, USA). Among those, each 10 fixture was installed in one stage group patients. ISQ values were measured using $Osstell^{TM}$ (Integration Diagnostics Ltd. Sweden) during fixture installation, at healing abutment connection and in the loading period for two stage surgery group patients and during at each 4, 6, 8, 10, 12week and in the loading phase for one stage surgery group patients and evaluated the changes according to the time and fixture type. Results: In two stage surgery group, mean and SO of ISQ values of machined surface implants were $76.85{\pm}3.74,\;75.76{\pm}5.04,\;75.73{\pm}4.41$ and those of HA-coated surface implant were $75.05{\pm}6.23,\;77.58{\pm}5.23,\;78.32{\pm}4.29$ during fixtures installation, at healing abutment connection and in the loading period, respectively. In one-stage surgery group, the ISQ values of machined surface and HA-coated surface implants decreased until 4 or 6 week and maintained at plateau for 1-3 week and increased to the loading period. Conclusions: Machined and HA-coated surface implants showed minimal ISQ changes with time if they were installed at the sites showing at least intact cortical plate and good bone qualities. And HA-coated implants had a tendency to show somewhat increased ISQ values with time.

• 한국표면공학회지
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• 제51권3호
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• pp.164-171
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• 2018

In this study, we have fabricated pure titanium (Ti)/hydroxyapatite (HA) double layer coating on medical grade PEEK from magnetron sputtering system, an investigation was performed whether the surface can be had more improve bio-active for orthopedi/dental applications than that of non-coated one. Pure Ti and HA coating layer were obtained by a radio-frequency and direct current power magnetron sputtering system. The microstructures surface, mechanical properties and wettability of the pure Ti/HA double layer deposited on the PEEK were analyzed by scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDS), X-ray diffraction (XRD), nano-indentation, and contact angle test. According to the EDS and XRD results, the composition and crystal structure of pure Ti and HA coated surface were verified. The elastic modulus and hardness value were increased by pure Ti and HA coating, and the pure Ti/HA double layer coating surface has the highest value. The contact angle showed higher value for pure Ti/HA double layered coating specimens than that of non-coated (PEEK) surface.

• Journal of Periodontal and Implant Science
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• 제24권1호
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• pp.131-143
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• 1994

구강내 노출된 임프란트를 건강한 상태로 유지하기 위해서는 임프란트 매식체 표면을 처치하여 주위조직과 잘 적합할 수 있는 표면구조를 만들어 주어야 한다. 실패한 임프란트의 처리방법으로 구연산이나 air-abrasive system과 같은 여러 가지 방법이 소개 되었으나 HA 피막 처치된 임프란트와 같은 거친 표면이 구강내로 노출된 경우에는 구연산이나 air-abrasive system을 이용한 표면 처리방법을 세균독소 제거에는 효과적이나 HA 피막 처리된 매식체의 거친 표면 제거는 어렵기 때문에 계속되는 치태침착을 방지하기에는 효과적이지 못하므로 세균독소를 제거하는 한편 표면성상을 변화시키지 않고 평활한 표면을 만들기 위한 처리방법들을 알아보고자 하였다. IMZ사에서 제작한 HA 피막 처리된 disc에 high speed diamond bur, low speed diamond bur, stone bur, rubber point, jetpolisher를 처치하고 표면평활도를 알아보기 위하여 표면조도측정 및 주사전자현미경으로 표면상태를 관찰하고 표면성분 변화 유무를 알아보기 위하여 EDX를 이용하여 표면성분을 분석한 결과 다음과 같은 결과를 얻었다. 각 시편에 대한 표면조도 측정 결과는 실험 I군 $2.11{\mu}m$, 실험 II군 $4.17{\mu}m$, 실험 III군 $7.28{\mu}m$, 실험 IV군 $8.61{\mu}m$, 실험 V군 $39.44{\mu}m$의 최대높이값을 나타내므로써, I, II, III, IV, V군 순으로 표면이 평활하게 나타났다. 주사전자현미경 관찰에서는 실험 I군은 비교적 평활한 면을 보였고, 실험 II군은 HA 입자가 거의 삭제되었으나 잔존하는 일부의 HA 입자로 인하여 I군보다 약간 거친 표면을 보였다. 실험 III군과 IV군은 삭제되지 않고 잔존하는 HA 입자가 많아 거친 양상을 보였으며 실험 V군인 HA 피막 처리된 면의 경우는 깊은 홈과 돌출된 부분을 가진 매우 불규칙한 표면 구조를 보였다. 시편의 단면 관찰에서는 실험 I군은 균일한 면을 보였으며 실험 III군과 IV군에서는 삭제되지 않고 잔존하는 다량의 HA 입자로 인해 거친 표면을 보였으나 HA 피막의 두께는 상당량 감소되어 나타났다. 또한 실험 II군과 I군과 유사한 양상을 보였다. 실험 V군의 경우는 일정하지는 않지만 약 $40{\mu}m$의 두께를 보였다. EDX에 의한 표면성분 분석 결과, 삭제가 가장 우수한 실험 II군에서는 calcium과 phosphorus가 소량 나타났고, 삭제가 완전하지 않은 실험 III, IV군에서는 calcium peak와 phosphorus peak를 보였다. 모든 군에 나타난 aluminum은 제조과정 중의 혼입으로 사료된다. 모든 실험군에서 titanium, aluminum, calcium, phosphorus 이외의 다른 성분은 나타나지 않았다.

• The Journal of Advanced Prosthodontics
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• 제6권2호
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• pp.96-102
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• 2014

PURPOSE. This study was performed to characterize the effects of zirconia coated with calcium phosphate and hydroxyapatite compared to smooth zirconia after bone marrow-derived osteoblast culture. MATERIALS AND METHODS. Bone marrow-derived osteoblasts were cultured on (1) smooth zirconia, (2) zirconia coated with calcium phosphate (CaP), and (3) zirconia coated with hydroxyapatite (HA). The tetrazolium-based colorimetric assay (MTT test) was used for cell proliferation evaluation. Scanning electron microscopy (SEM) and alkaline phosphatase (ALP) activity was measured to evaluate the cellular morphology and differentiation rate. X-ray photoelectron spectroscopy (XPS) was employed for the analysis of surface chemistry. The genetic expression of the osteoblasts and dissolution behavior of the coatings were observed. Assessment of the significance level of the differences between the groups was done with analysis of variance (ANOVA). RESULTS. From the MTT assay, no significant difference between smooth and surface coated zirconia was found (P>.05). From the SEM image, cells on all three groups of discs were sporadically triangular or spread out in shape with formation of filopodia. From the ALP activity assay, the optical density of osteoblasts on smooth zirconia discs was higher than that on surface treated zirconia discs (P>.05). Most of the genes related to cell adhesion showed similar expression level between smooth and surface treated zirconia. The dissolution rate was higher with CaP than HA coating. CONCLUSION. The attachment and growth behavior of bone-marrow-derived osteoblasts cultured on smooth surface coated zirconia showed comparable results. However, the HA coating showed more time-dependent stability compared to the CaP coating.

• 한국표면공학회:학술대회논문집
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• 한국표면공학회 2012년도 춘계학술발표회 논문집
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• pp.126-126
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• 2012

In this study, adhesion of plasma spray coated hydroxyapatite film on the two-step anodized dental implant was investigated. The plasma spray was carried out on the dental implant after two step anodization. The adhesion of coated HA film was investigated by FE-SEM after fatigue test. In the case of two-step anodized implant showed a good adhesion between implant and coated film.