• 한국재료학회지
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• 제14권12호
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• pp.893-899
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• 2004

Even though Ti-6Al-4V has gained popularity as an implant material, the possible dissolution of Al and V ions in body fluids remains a matter of concern. Though commercially pure Ti (Cp-Ti) overcomes this problem, the mechanical strength of pure titanium remains very low. Thus, in this experiment Cp-Ti was processed by Equal channel angular processing (ECAP), in order to increase the mechanical strength. The biocompatibility of ECAP-Ti, Cp-Ti and Ti-6Al-4V was examined by the apatite formation on each sample surface, after treating the surface with 5M NaOH and soaking in Simulated body fluids (SBF). Initially, the samples were mechanically polished on silicone carbide paper (#2000). The polished samples were treated with 5M NaOH solution at $60^{\circ}C$ for 24 hours. The NaOH treated samples were washed gently with distill water and dried at $40^{\circ}C$ for 1 day. The dried samples were heat treated in air at $600^{\circ}C$ for 1 hour. The surface morphology of these samples were studied using SEM and XRD. The SEM studies showed network of pores in all samples. The XRD showed oxide layer formation on Cp-Ti and Ti-6Al-4V. samples. However the oxide layer in ECAP-Ti was not substantial. These samples were immersed in SBF, kept at $36.5^{\circ}C$ for seven days period. At the end of 7 days, the apatite formation was confirmed only on Cp-Ti and was not observed in Ti-6Al-4V and ECAP-Ti. These observations of apatite formation relate to the fact that Cp-Ti showed greater oxide layer than other samples. The apatite examined was confirmed as tricalcium phosphate (TCP) using EDS and XRD.

• 대한금속재료학회지
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• 제46권2호
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• pp.105-110
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• 2008

Process of the hydroxyapatite (HA) formation on bioactive titanium metal prepared by NaOH treatment in a modified-simulated body fluid (mSBF) containing bovine serum albumin (BSA) was investigated by high resolution transmission electron microscope attached with energy dispersive X-ray spectrometer (EDX). The amorphous titanate, which was formed on titanium surface by NaOH treatment, combined with the calcium ions in the liquid to form an amorphous calcium titanite. With increasing of soaking time in the liquid, an amorphous calcium titanite combined with the phosphate ions to form an amorphous calcium phosphate with low Ca/P atomic ratio, and it grows as aggregates of plate (or needle)-like substance on titanium surface. The crystalline apatite layers, which are needle-shaped with the c axis parallel to the long axis, are formed in an amorphous calcium phosphate with further increase in soaking time. The formation of needle-shaped apatite layers can be explained by electrostatic effects and difference of concentration between calcium, phosphate, and albumin ions.

• 대한금속재료학회지
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• 제47권12호
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• pp.881-886
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• 2009

Research into the replacement of injured systems and tissue in the human body is advancing rapidly. Recently, Ti-Ni shape memory alloys have shown excellent biofunctionality related to their shape memory effect and superelasticity. In this study, the effect of an acid or an alkali treatment on the bioactivity in 49Ti-Ni and 51.5Ti-48.5Ni alloys is investigated in an effort to utilize Ti-Ni alloy as a biomaterial. In addition, the biocompatibility in a SBF solution is assessed through in vitro testing. A porous surface was formed on the surface of both alloys after a chemical treatment. According to the in vitro test, apatite formed on the surfaces of both alloys. The forming rate of apatite in the Ti-rich alloy was faster that in the Ni-rich alloy. The formation of apatite provided proof of the bioactivity of the Ti-Ni alloy. A small quantity of Ni was eluted at the initial stage, whereas Ni was not found for 12 days in the Ti-rich alloy and for 8 days in the Ni-rich alloy. In the case of the treated 51.5Ti-Ni alloy, the shape memory property was worsened but the biocompatibility was improved.

• 한국결정성장학회지
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• 제19권1호
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• pp.19-24
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• 2009

생체모방법을 이용하여 표면 처리된 titanium plates 표면에 아파타이트 형성에 관하여 조사하였다. 표면 처리방법으로는 우선, titanium plate 표면에 titanium oxide층을 형성시키기 위하여 열처리온도를 $400^{\circ}C$, $600^{\circ}C$, 그리고 $800^{\circ}C$에서 전기로에서 5시간 유지하였으며, 열처리된 titanium plates 1 M를 수산화나트늄 용액에 침전시켜 표면을 화학적으로 처리하였다. 생체모방법으로 titanium plates 표면에 아파타이트를 형성시키기 위하여 표면처리된 titanium plates 를 Kokubo's recipe에 의하여 제조된 생체유사액(SBF)에 침적시켰다. SBF 용액에 1주와 3주기간 동안 침적시킨 후, 표면처리를 달리한 titanium plates 표면에 형성된 코팅층을 서로 비교 분석하였다.

• 한국세라믹학회지
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• 제48권1호
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• pp.26-33
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• 2011

The glass in the system of CaO-$SiO_2-P_2O_5$ and the corresponding glass-ceramics are prepared for bone cements and the behaviors of the hardening and hydroxyapatite formation were studied for the glass and glass-ceramic powders. The glass crystallized into apatite, $\alpha$-wollastonite and $\beta$-wollastonite depending on the glass composition when they were heat-treated at $950^{\circ}C$ for 4 h. A DCPD (dicalcium phosphate dihydrate : $CaHPO_4{\cdot}2H_2O$) was developed when the prepared glass and glass-ceramic powders were mixed with 3M-$H_3PO_4$ solution. The DCPD (Ca/P=1.0) transformed to HAp (Ca/P=1.67) when the bone cement was soaked in simulated body fluid (SBF), and this HAp formation strongly depended on the releasing capacity of $Ca^{2+}$ ions from the glass and glass-ceramic cements. The glass-ceramic bone cement containing $\alpha$-wollastonite crystals showed faster transformation of DCPD to HAp than other glass-ceramics containing $\alpha$- and $\beta$-wollastonite crystals. No hydroxyapatite was observed when the glass-ceramic bone cement containing apatite crystals (36P6C) was soaked in SBF even for 1 month, because no $Ca^{2+}$ ion can be released from the stable apatite crystals.

• 한국표면공학회:학술대회논문집
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• 한국표면공학회 2017년도 춘계학술대회 논문집
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• pp.79-79
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• 2017

Metallic biomaterials have been mainly used for the fabrication of medical devices for the replacement of hard tissue such as artificial hip joints, bone plates, and dental implants. Because they are very reliable on the viewpoint of mechanical performance. This trend is expected to continue. Especially, Ti and Ti alloys are bioinert. So, they do not chemically bond to the bone, whereas they physically bond with bone tissue. For their poor surface biocompatibility, the surface of Ti alloys has to be modified to improve the surface osteoinductivity. Recently, ceramic-like coatings on titanium, produced by plasma electrolytic oxidation (PEO), have been developed with calciumand phosphorus-enriched surfaces. A lso included the influences of coatings, which can accelerate healing and cell integration, as well as improve tribological properties. However, the adhesions of these coatings to the Ti surface need to be improved for clinical use. Particularly Silicon (Si) has been found to be essential for normal bone, cartilage growth and development. This hydroxyapatite, modified with the inclusion of small concentrations of silicon has been demonstrating to improve the osteoblast proliferation and the bone extracellular matrix production. Strontium-containing hydroxyapatite (Sr-HA) was designed as a filling material to improve the biocompatibility of bone cement. In vitro, the presence of strontium in the coating enhances osteoblast activity and differentiation, whereas it inhibits osteoclast production and proliferation. The objective of this work was to study Morphology of bone-like apatite formation on Sr and Si-doped hydroxyapatite surface of Ti-6Al-4V alloy after plasma electrolytic oxidation. Anodized alloys was prepared at 270V~300V voltages with various concentrations of Si and Sr ions. Bone-like apatite formation was carried out in SBF solution. The morphology of PEO, phase and composition of oxide surface of Ti-6Al-4V alloys were examined by FE-SEM, EDS, and XRD.

• 한국표면공학회:학술대회논문집
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• 한국표면공학회 2017년도 춘계학술대회 논문집
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• pp.157-157
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• 2017

Titanium and its alloys that have a good biocompatibility, corrosion resistance, and mechanical properties such as hardness and wear resistance are widely used in dental and orthopedic implant applications. They can directly connect to bone. However, they do not form a chemical bond with bone tissue. Plasma electrolytic oxidation (PEO) that combines the high voltage spark and electrochemical oxidation is a novel method to form ceramic coatings on light metals such as titanium and its alloys. This is an excellent reproducibility and economical, because the size and shape control of the nano-structure is relatively easy. Silicon (Si), manganese (Mn), and magnesium (Mg) has a useful to bone. Particularly, Si has been found to be essential for normal bone, cartilage growth and development. Manganese influences regulation of bone remodeling because its low content in body is connected with the rise of the concentration of calcium, phosphates and phosphatase out of cells. Insufficience of Mn in human body is probably contributing cause of osteoporosis. Pre-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 objective of this work was to study nucleation and growth of bone-like apatite formation on Ti-6Al-4V in solution containing Mn, Mg, and Si ions after plasma electrolytic oxidation. Anodized alloys was prepared at 270V~300V voltages. And bone-like apatite formation was carried out in SBF solution for 1, 3, 5, and 7 days. The morphologies of PEO-treated Ti-6Al-4V alloy in containing Mn, Mg, and Si ions were examined by FE-SEM, EDS, and XRD.

• 한국재료학회지
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• 제24권12호
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• pp.671-676
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• 2014

It is known that bones get damaged by accidents and aging. Since the discovery of Bioglass, various kinds of ceramics have been also found to bond to living bone; some of these ceramics are already being clinically used as bone-repairing materials. In the present study, antibacterial calcium silicate gel ($Ag-30CaO{\cdot}70SiO_2$ gel) was prepared by sol-gel method in order to control the microstructure, which is related to the dissolution rate and induction period of apatite formation in body environment. In addition, biological $Ag-30CaO{\cdot}70SiO_2$ is tested. This was done to impart antimicrobial activity to the $30CaO{\cdot}70SiO_2$. Ag ion was added during sol-gel synthesis to replace the $H_2O$ added during the making of the $30CaO{\cdot}70SiO_2$ gel, which has silver solutions of various concentration. After the sol-gel process, 1N-$HNO_3$ solution was used to wash the gel when synthesizing the gel, in order to maintain the porous structure and remove PEG, water soluble polymers. Then, the apatite forming ability of the sol-gel derived CaO-$SiO_2$ gels was investigated using simulated body fluid (SBF), which had almost the same ion concentration as that of human blood plasma. The gels were analyzed by FT-IR spectroscopy, SEM observation, XRD, and fluorescent microscopy. The apatite was successfully created even after washing the gel; apatite is present in an amorphous state, and was found to affect the concentration of the Ag ion in cells in MC3T3 live & dead assay results. From these results, it is suggested that a good material that can be used to repair defects of nature bone is $Ag-30CaO{\cdot}70SiO_2$ gel.

• 공학논문집
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• 제6권2호
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• pp.23-32
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• 2004

현재까지 사용되어가지고 있는 임플란트 재료 중 commercially pure titanium (순수티탄; Cp-Ti)과 Ti-alloy들은 생체재료로 폭넓게 사용되어지고 있는데, Ti 금속들은 경도가 강하고 점도가 높기 때문에, 치과나 정형외과 등의 하중에 잘 견디는 곳에 이용되어지고 있다고 한다. 이것들은 생체적합성과 부식에 대한 저항성도 좋은 것으로 알려져 있다. 일반적으로 Ti은 4종류의 Grade로 강도의 차이에 의하여 분류되고 Ti의 강도에 영향을 미치는 것으로는 산소, 철, 질소등이 있다. 따라서 본 연구에서는 O와 Fe의 함량을 달리한 Ti alloy시편을 사용하여 생체적합성 실험을 하였다. 먼저 실험은 시편을 micropolishing하고 5M NaOH에서 $60^{\circ}C$에서24시간 처리하여서 비표면적을 넓혔으며, 표면의 $TiO_2$을 만들어주기 위하여 $600^{\circ}C$에서 열처리하였다. 그런 시편을 $36.5^{\circ}C$의 SBF에 넣어 1~14일까지 침적한 후에 표면에 형성된 apatite를 SEM과 EDAX로 조사하였다. 조사 결과 모든 시편에서 apatite가 생성되었지만, 시편의 조성에 따라서 apatite의 형성양이 다름을 확인하였다.

• 한국세라믹학회지
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• 제45권10호
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• pp.638-643
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• 2008

Biomimetic apatite formation and deposition behaviors of Ti-6Al-7Nb and Ti-6Al-4V plates in simulated body fluids(SBF) under various conditions were examined. In case of regular samples without collagen treatments the weight gain due to apatite precipitation on the surface in Ti-6Al-4V was found to be higher than in Ti-6Al-7Nb. In case of collagen-coated samples, the weight gain in Ti-6Al-4V continued to be higher than in Ti-6Al-7Nb, but the difference between the two became smaller. Both Ti-6Al-7Nb and Ti-6Al-4V samples with collagen coating exhibited an appreciable increase of weight gain, which may be caused by the interaction between collagen and $Ca^{+2}$ ions. The weight gain was found to be not much affected by the addition of collagen to SBF. The ill-defined granular structure in the presence of collagen can be associated with the increasing volume fraction of amorphous calcium phosphate.