• The Journal of Advanced Prosthodontics
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• 제5권4호
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• pp.402-408
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• 2013

PURPOSE. The aim of this study was to evaluate the surface properties and in vitro bioactivity to osteoblasts of magnesium and magnesium-hydroxyapatite coated titanium. MATERIALS AND METHODS. Themagnesium (Mg) and magnesium-hydroxyapatite (Mg-HA) coatings on titanium (Ti) substrates were prepared by radio frequency (RF) and direct current (DC) magnetron sputtering.The samples were divided into non-coated smooth Ti (Ti-S group), Mg coatinggroup (Ti-Mg group), and Mg-HA coating group (Ti-MgHA group).The surface properties were evaluated using scanning electron microscopy (SEM) and X-ray photoelectron spectroscopy (XPS). The surface roughness was evaluated by atomic force microscopy (AFM). Cell adhesion, cell proliferation and alkaline phosphatase (ALP) activity were evaluated using MC3T3-E1 cells. Reverse transcription polymerase chain reaction (RT-PCR) analysis was performed. RESULTS. Cross-sectional SEM images showed that Mg and Mg-HA depositionson titanium substrates were performed successfully. The surface roughness appeared to be similaramong the three groups. Ti-MgHA and Ti-Mg group had improved cellular responses with regard to the proliferation, alkaline phosphatase (ALP) activity, and bone-associated markers, such as bone sialoprotein (BSP) and osteocalcin (OCN) mRNA compared to those of Ti-S group. However, the differences between Ti-Mg group and Ti-MgHA group were not significant, in spite of the tendency of higher proliferation, ALP activity and BSP expression in Ti-MgHA group. CONCLUSION. Mg and Mg-HAcoatings could stimulate the differentiation into osteoblastic MC3T3-E1 cells, potentially contributing to rapid osseointegration.

• 대한치과보철학회지
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• 제43권1호
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• pp.78-94
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• 2005

Purpose. The purpose of this study was to compare the effects of various surface treatments by measuring resonance frequency and histomorphometric analyses. Material and methods. In 5 adult dogs, the mandibular premolar were extracted. Six months later, 30 screw titanium implants (Dentium Co., Seoul, Korea) 6mm in length and 3.4mm in diameter, were placed in the mandibles of 5 dogs. Implants were divided into five groups following to surface treatment methods ; Group 1 is machined controls, Group 2 is sandblasted with large grit and acid-etched (SLA), Group 3 is anodized (Autoelectric Co., Korea, 660Hz, Duty10), Group 4 is hydroxyapatite(HA) coated by ion beam assisted deposition(E-beam), Group 5 is hydroxyapatite(HA) coated with Sol-gel coating process. Resonance frequency was measured implant placement immediately, and 3, 6 weeks and 10 weeks of healing perods. With the animal subject's sacrifice 10 weeks after implantation, implants were removed on bloc and histologic and computer-based histomorphometric analyses were performed. Histomorphometric analysis involved quantification of the entire bone to metal contact around the implants. Statistical analyses were performed using the SPSS for Windows (ver. 9.0 SPSS Inc.) Statistical differences were considered significant at P<0.05. Results. The results were as follows : 1) In five groups, mean value of resonance frequency analysis(RFA) were highest in group 5 (Sol-gel implant) at implantation and those of group 4 (E-beam)was highest at 10 weeks . but there was no correlation between surface treatments and RFA. 2) In all surface treatment groups, the RFA values of implants decreased until 3 weeks and increased to 10 weeks. 3) The percentage of direct bone-to-implant contact (BIC) had statistical significance between five groups in cancellous bone, (P<0.05) the percentage of bone density inside the thread had no statistical significance between five groups. (P>0.05) 4) There was a significant difference between cortical bone and cancellous bone in BIC. (P<0.05) and bone density. (P<0.05) 5) There was a correlation between the RFA value of implants at 10 weeks and BIC in cancellous bone, and between the RFA value of implants at 10 weeks and bone density in cortical bone. (P<0.05). Conclusions. These results indicate that surface treatment does not affect the implant stability in case of good bone quality.

• 한국표면공학회:학술대회논문집
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• 한국표면공학회 2003년도 추계학술발표회초록집
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• pp.134-135
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• 2003

The dental implant materials required good mechanical properties, such as fatigue strength, combined with a high resistance to corrosion. For increasing fatigue resistance and delaying onset of stress corrosion cracking, shot peening has been used for > 50 years to extend service life of metal components. However, there is no information on the electrochemical behavior of shot peened and hydroxyapatite(HA) coated Ti-6Al-4V alloys. To increase fatigue strength, good corrosion resistance, and biocompatibility, the electrochemical characteristics of Ti/TiN/HA coated and shot peened Ti-6Al-4V alloys by electron beam physical vapor deposition(EB-PVD) have been researched by various electrochemical method in 0.9%NaCl. Ti-6Al-4V alloys were prepared under the condition of hydrogen and vacuum arc furnace. The produced materials were quenched at 1000$^{\circ}C$ under high purity dried Ar atmosphere and were hold at 500$^{\circ}C$ for 2 hrs to achieve the fatigue strength(1140㎫) of materials. Ti-6Al-4V alloys were prepared under the condition of hydrogen and vacuum arc furnace. Shot peening(SP) and sand blasting treatment was carried out for 1, 5, and 10min. On the surface of Ti-6Al-4V alloys using the steel balls of 0.5mm and alumina sand of 40$\mu\textrm{m}$ size. Ti/TiN/HA multilayer coatings were carried out by using electron-beam deposition method(EB-PVD) as shown Fig. 1. Bulk Ti, powder TiN and hydroxyapatite were used as the source of the deposition materials. Electrons were accelerated by high voltage of 4.2kV with 80 - 120mA on the deposition materials at 350$^{\circ}C$ in 2.0 X 10-6 torr vacuum. Ti/TiN/HA multilayer coated surfaces and layers were investigated by SEM and XRD. A saturated calomel electrode as a reference electrode, and high density carbon electrode as a counter electrode, were set according to ASTM GS-87. The potentials were controlled at a scan rate of 100 mV/min. by a potentiostat (EG&G Co.273A) connected to a computer system. Electrochemical tests were used to investigate the electrochemical characteristics of Ti/TiN/HA coated and shot peened materials in 0.9% NaCl solution at 36.5$^{\circ}C$. After each electrochemical measurement, the corrosion surface of each sample was investigated by SEM.

• Maxillofacial Plastic and Reconstructive Surgery
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• 제23권5호
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• pp.396-405
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• 2001

Osseointegrated implants are used for the fixation of dental prosthesis with good long-term clinical results. In an attempt to improve the quantity and quality of the bone-implant interface, numerous implant modification have been used. Implants surface modifications have been used such as titanium-plasma sprayed, hydroxyapatite-coating, sandblasted, sandblasted and acid-etched, acid-etched. Rough surface implants have greater implant surface area and enhance the bone-implant interface and improve stabilization. The purpose of present study was to evaluate light microscopic and scanning microscopic examinations and removal torque value of newly developed calcium phosphate blast and acid-etched implant in the femur of rabbits. Titanium plasma sprayed(TPS) implant served as controls. After 12 weeks of healing of the femurs of 12 rabitts, the implant-containing segments of femur were removed on bloc and bone block including sections. Histologic examination and histomorphometric and removal torque values comparision were made for two implants. Obtained results are follows: 1. Newly developed calcium phosphate blasted and acid-etched implants were in close contact with bone under light microscopic examinations. 2. New implants showed mean bone-to implant contact 59.8%, whereas TPS implants showed mean bone-to implant contact 54.5% (statistically no difference p<0.05). 3. New implants showed mean bone density 56.7%, whereas TPS implants showed mean bone density 49.2% (statistically difference p<0.05). 4. New implants demonstrated mean removal torque values 40.5Ncm, whereas the mean removal torque values of TPS implants ranged 39.3Ncm. No statistical differences(p<0.05) were observed between two groups of implants nor was there any difference between the two implants at the clinical level.

• 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.

• 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.

• 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.

• 대한치과보철학회지
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• 제45권1호
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• pp.131-143
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• 2007

Statement of the problem: In case of poor bone quality or immediately loaded implant, various strategies have been developed focusing on the surface of materials to improve direct implant fixation to the bone. The microscopic properties of implant surfaces play a major role in the osseous healing of dental implant. Purpose of study: This study was undertaken to evaluate bone response of ion beam-assisted deposition(IBAD) of hydroxyapatite(HA) on the anodized surface of subperiosteal titanium implants. Material and methods: Two half doughnut shape subperiosteal titanium implants were made. The control group was treated with Anodized surface treatment and the test group was treated with IBAD of HA on control surface. Then two implants inserted together into the subperiosteum of the skull of 30 rats and histological response around implant was observed under LM(light microscope) and TEM(transmission electron microscope) on 4th, 6th and 8th week. Results: Many subperiosteal implants were fixed with fibrous connective tissue not with bony tissue because of weak primary stability. The control group observed poor bone response and there was no significant change at any observation time. However the test group showed advanced bone formation and showed direct bone to implant contact under LM on 8th week. The test group observed much rER in the cell of osteoblast but the control group showed little rER under TEM. Conclusions: The test group showed better bone formation than the control group at the condition of weak primary stability. With these results IBAD surface treatment method on Anodized surface, may be good effect at the condition of weak primary stability.