• Journal of the Korean Vacuum Society
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• v.7 no.s1
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• pp.50-56
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• 1998

Ion beam assisted deposition (IBAD) was successfully used to produce a dense and ultra-adherent Hydroxyapatite (HA) film on titanium alloy and alumina. Recently it is also proved that the HA coatings on alumina substrate treated with 20 ppm $AgNO_3$ had the structure of $(Ag, Ca)_10(PO_4)6(OH)_2$, which exhibited excellent antimicrobial effects. The present paper aims to morphlogically characterize the adhesion of macrophages on newly developed Ag-HA coated alumina and Ti6A14V substrates and to evaluate the biocompatibility of the coatings in vitro. It can be found that the cell number on alumina of the concentration of $AgNO_3$ in the treatment, the cell number on Ag-HA coatings decreased. Up to 20 ppm $AgNO_3$ by Ag-treatment, the morphological development of the cells on Ag-HA coating was similar to that of the cells on HA coating, suggesting the biotolerance of the Ag-HA coatings.

• Korean Journal of Materials Research
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• v.17 no.2
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• pp.100-106
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• 2007

The effects of $MgO-P_2O_5$ based sintering additive on the microstructure and material and biological properties of hydroxyapatite $(HAp,\;Ca_{10}(PO_4)_6(OH)_2)$ ceramic were investigated using XRD, SEM and TEM techniques. The $MgO-P_2O_5$ sintering additive improved the material properties and increased the grain size in the sintered HAp bodies. As the content of sintering additive increased over 4 wt%, a small amount of the HAp phase was decomposed and transformed to ${\beta}-TCP$. In the 2 wt% $MgO-P_2O_5$ content HAp sintered body, the maximum values of density and hardness were respectively about 3.10 gm/cc and 657 HV. However, the maximum fracture toughness in the HAp body containing 8 wt% $MgO-P_{2}O_{5}$ was about $1.02MPa{\cdot}m^{1/2}$ due to the crack deflection effect. Human osteoblast like MG-63 cells and osteoclast like raw 264.7 cells were well grown and fully covered all of the HAp sintered bodies. The osteoblast cells were grown with spindle-shaped and the osteoclast cells had a grape-like round shape.

• Korean Journal of Soil Science and Fertilizer
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• v.40 no.5
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• pp.405-411
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• 2007

This study was carried out to measure insoluble phosphorus fractions content fixed in different soil type and isolate a superior phosphate solublizing bacteria(PSB) producing free phosphate in citrus orchard soil. Distribution of insoluble phosphate fraction ordered Al-P>Ca-P>Fe-P in the investigated citrus orchards. Insoluble phosphate fraction such as Al-P, Ca-P, Fe-P were higher in volcanic ash than in non-volcanic ash soil. A PSB with high holo zone in PDA-P medium isolated from citrus orchard soil. This strain identificated by MIDI system as Bacillus sphaericus. The optimum growth of pH and temperature were at 4~5, $30^{\circ}C$, respectively. When Bacillus sphaericus cultured at $25^{\circ}C$, 150 rpm condition in LB broth medium included different phosphate. Bacillus sphaericus produced free phosphate in the culture broth medium from tricalcium-phosphate(207.0 ppm), aluminium phosphate(324.5 ppm) and hydroxyapatite(334.8 ppm) and Phosphatase activity of Bacillus sphaericus was higher at $35^{\circ}C$ culture condition than that of $25^{\circ}C$. Two type preparation inoculated Bacillus sphaericus made with carrier materials such as Bentonite, $CaCO_3$, Sodium alginate. Density of PSB in this preparation conserved at $10^5c.f.u.\;g^{-1}$ level during storage in different temperature condition for 7 month. It also showed that free phosphate produced at PDA-P medium.

• Proceedings of the Korean Vacuum Society Conference
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• 2010.02a
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• pp.397-397
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• 2010

Bone is considered as hierarchically organized biocomposites of organic (collagen) and inorganic (hydroxyapatite) materials. The precise structural dependence between hydroxyapatite (HAp, $Ca_{10}(PO_4)_6(OH)_2)$ crystals and collagen fibril is critical to unique characteristics of bone. To meet those conditions and obtain optimal properties, it is essential to understand and control the initial growth mechanisms of hydroxyapatite at the molecular level, such as other nano-structured materials. In this study, collagen fibrils were prepared by adsorbing native type I collagen molecules onto hydrophobic surface. Hydrophobicity was introduced on the Si wafer surface by using PECVD (plasma enhanced chemical vapor deposition) method and cyclohexane as a precursor. Biomimetic nucleation and growth of HAp on the self-assembled collagen nanofibrils were occurred through incubation of the sample in SBF (simulated body fluid). Chemical and morphological evolution of HAp nanocrystals was investigated by surface-sensitive analytical techniques such as ToF-SIMS (Time-of-Flight Secondary Ion Mass Spectrometry) and AFM (Atomic Force Microscopy) in the early growth stages (< 24 hrs). The very initial stages (< 12 hrs) of mineralization could be clearly demonstrated by ToF-SIMS chemical mapping of surface. In addition to ToF-SIMS and AFM measurement, scanning electron microscopy, energy dispersive spectroscopy and X-ray diffraction analysis were conducted to characterize the HAp layer in the late stages. This study is of great importance in the growth of real bone-like materials with a structure analogous to that of natural bones and the development of biomimetic nanomaterials.

• Proceedings of the Korean Vacuum Society Conference
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• 2010.02a
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• pp.386-386
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• 2010

최근 널리 보급되고 있는 치과용 임플란트는 티타늄(Ti) 또는 티타늄 합금(Ti-6Al-4V) 보철과 크라운을 연결하여 사용하고 있다. 티타늄은 생체 친화성이 우수하나, 생체 활성도가 없어 치유기간이 긴 단점이 있다. 이를 보완하기 위해 인체 경조직과 유사한 수산화아파타이트(hydroxyapatite, $Ca_{10}(PO_4)_6(OH)_2)$를 티타늄 임플란트 표면에 코팅하는 방법이 연구되고 있으나 수산화아파타이트 코팅은 티타늄과의 접착성이 나쁘기 때문에 시술 및 사용과정에서 코팅층이 임플란트로부터 박리되는 문제점이 있다. 본 연구에서는 티타늄과 수산화아파타이트 사이에서 접착력을 향상시키는 buffer layer로서 지르코니아(8YSZ, 8mol% Yttria-stabilized zirconia)를 연구하였다. 지르코니아는 고온에서 안정하며, 티타늄 합금과 수산화아파타이트 사이의 반응을 방지하며, 박막밀도와 기계적 강도가 좋은 생체세라믹스이다. 지르코니아 박막을 펄스 레이저 증착법을 이용하여 증착 온도 $600^{\circ}C$, 레이저 fluence $2\;J/cm^2$에서 산소($O_2$) 분압을 바꿔 가며 증착하였다. 그 위에 수산화아파타이트 박막을 역시 펄스 레이저 증착법으로 증착하였다. Scratch test와 Pull-off test를 통해 접착력을 평가한 결과 지르코니아 buffer layer 삽입에 의해 티타늄 합금과 수산화아파타이트 사이의 접착력이 향상되었음을 확인하였다. 또한 산소분압이 박막의 특성 및 접착력에 미치는 영향을 고찰하였다.

• Corrosion Science and Technology
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• v.17 no.3
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• pp.91-100
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• 2018

Development of biodegradable implants for treatment of complex bone fractures has recently become one of the priority areas in biomedical materials research. Multifunctional corrosion resistant and bioactive coatings containing hydroxyapatite $Ca_{10}(PO_4)_6(OH)_2$ and magnesium oxide MgO were obtained on Mg-Mn-Ce magnesium alloy by plasma electrolytic oxidation. The phase and elemental composition, morphology, and anticorrosion properties of the coatings were investigated by scanning electron microscopy, energy dispersive spectroscopy, potentiodynamic polarization, and electrochemical impedance spectroscopy. The PEO-layers were post-treated using superdispersed polytetrafluoroethylene powder. The duplex treatment considerably reduced the corrosion rate (>4 orders of magnitude) of the magnesium alloy. The use of composite coatings in inducing bioactivity and controlling the corrosion degradation of resorbable Mg implants are considered promising. We also applied the plasma electrolytic oxidation method for the formation of the composite bioinert coatings on the titanium nickelide surface in order to improve its electrochemical properties and to change the morphological structure. It was shown that formed coatings significantly reduced the quantity of nickel ions released into the organism.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.14 no.3
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• pp.83-89
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• 2004

In this work, HA/$TiO_2$ biocomposite to get high mechanical properties with biocompatibility were prepared. HA/$TiO_2$ biocomposite powders were prepared by mixing $TiO_2$ and HA powders which were synthesized through sol-gel, precipitation and hydrothermal methods. The mixing ratio was fixed at 1:1 ratio (HA/$TiO_2$, wt%). HA/$TiO_2$ biocomposite powders showed different microstructures depending on their particle size and shape. The smaller particles were coated on the surface of larger particles, whereas they were well mixed and dispersed when both $TiO_2$ and HA were nanocrystallites. HA/$TiO_2$ biocomposite powders with homogeneous microstructure showed high sintered density and good mechanical properties.

• The Journal of Engineering Research
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• v.3 no.1
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• pp.181-187
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• 1998

Hydroxyapatite was used as implant materials, because it has a good biocompatibility and is similar to human bone. However it is not expected to have a high strength as implant materials because of a low fracture strength after sintering of HAp. Alumina ($\alpha$-alumina) shows a stable chemical properties and high strength in physiological environments. Thus it was tried to use a HAp coatings on Alumina substrate as implant materials. In this study, HAp was coated on Alumina substrate by lon Beam Assisted Deposition(IBAD). Then Ag was impregnated on HAp coating layer, which showed antimicrobial effects. To carry out the ion exchange of $Ag^+$ with $Ca^{2+}$ in HAp on the surface, HAp coated alumina substrate was immersed in 20ppm, 100ppm $AgNO_3$ solution at room temperature for 48 hours. Antimicrobial test was studied by using bacteria, which normally caused periprosthetic infections. The follwing bacteria was used in antimicrobial test. Escherichia coli, Pseudomonas aeruginosa (gram negative) and staphylococcus epidermidis (gram positive). Ag impregnated HAp shows very good antimicrobial effects against these bacteria. The surface structure of sample, which was treated in $AgNO_3$ solution was studied by SEM, XRD. Ag release curve was studied in Simulated Body Fluid (SBF) solution.

• Journal of Biosystems Engineering
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• v.39 no.3
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• pp.227-234
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• 2014

Purpose: The aim of this research was to develop and evaluate natural hydroxyapatite (HA) ceramics produced from the heat treatment of pig bones. Methods: The properties of natural HA ceramics produced from pig bones were assessed in two parts. Firstly, the raw materials were characterized. A temperature of $1,200^{\circ}C$ was chosen as the calcination temperature. Fine bone powders (BPs) were produced via calcinations and a milling process. Sintered BPs were then characterized using field emission scanning electron microscopy (FE-SEM), X-ray diffraction (XRD), X-ray fluorescence spectroscopy (XRF), energy dispersive X-ray spectroscopy (EDX), Fourier transform infrared (FTIR) spectroscopy, and a 2-year in vitro degradability test. Secondly, an indirect cytotoxicity test was conducted on human osteoblast-like cells, MG63, treated with the BPs. Results: The average particle size of the BPs was $20{\pm}5{\mu}m$. FE-SEM showed a non-uniform distribution of the particle size. The phase obtained from XRD analysis confirmed the structure of HA. Elemental analysis using XRF detected phosphorus (P) and calcium (Ca) with the Ca/P ratio of 1.6. Functional groups examined by FTIR detected phosphate ($PO{_4}^{3-}$), hydroxyl ($OH^-$), and carbonate ($CO{_3}^{2-}$). The EDX, XRF, and FTIR analysis of BPs indicated the absence of organic compounds, which were completely removed after annealing at $1,200^{\circ}C$. The BPs were mostly stable in a simulated body fluid (SBF) solution for 2 years. An indirect cytotoxicity test on natural HA ceramics showed no threat to the cells. Conclusions: In conclusion, the sintering temperature of $1,200^{\circ}C$ affected the microstructure, phase, and biological characteristics of natural HA ceramics consisting of calcium phosphate. The Ca-P-based natural ceramics are bioactive materials with good biocompatibility; our results indicate that the prepared HA ceramics have great potential for agricultural and biological applications.

• Proceedings of the Materials Research Society of Korea Conference
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• 2009.11a
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• pp.41.1-41.1
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• 2009

Aerosol Deposition (AD) is anovel way to fabricate bioactive ceramic coatings in biomedical implants and prostheses applications. In the present work, silicon-substituted hydroxyapatite (HA) coatings on commercially pure titanium were prepared by aerosol deposition using Si-HA powders. The incorporation of silicon in the HA lattice is known to improve the bioactivity of the HA, makingsilicon-substitute HA an attractive alternative to pure HA in biomedical applications. Si-HA powders with the chemical formula $Ca_{10}(PO_4)_6-x(SiO_4)x(OH)_2-x$, having silicon contents up to x=0.5 (1.4 wt%), were synthesized by solid-state reaction of $Ca_2P_2O_7$, $CaCO_3$, and $SiO_2$. The Si-HA powders were characterized by X-ray diffraction (XRD), X-ray fluorescence spectrometry (XRF), and Fourier transform infrared spectroscopy(FT-IR). The corresponding coatings were also analyzed by XRD, scanning electron microscopy (SEM), and electron probe microanalyzer (EPMA). The results revealed that a single-phase Si-HA was obtained without any secondary phases such as $\alpha$- or $\beta$-tricalcium phosphate (TCP) for both the powders and the coatings.The Si-HA coating was about $5\;{\mu}m$ thick, had a densemicrostructure with no cracks or pores. In addition, the proliferation and alkaline phosphatase (ALP) activity of MC3T3-E1 preosteoblast cells grown on the Si-HA coatings were significantly higher than those on the bare Ti and pure HA coating. These results revealed the stimulatory effects induced by siliconsubstitution on the cellular response to the HA coating.