• 한국재료학회지
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• 제8권9호
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• pp.865-870
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• 1998

생체내에서 매식되는 타이타늄의 표면에 골의 형성과 성장을 촉진시키기 위해 칼슘이온과 인산이온을 함유하는 용액에서 타이타늄의 표면처리를 행하였다. 표면처리방법으로는 pH 5.8, 7.0, 8.0의 인산칼슘 완충용액에 10분간 침적시킨 후 유사체액에 30일간 침적시켰다. 침적시킨 후의 타이타늄 표면에 형성된 피막의 특성을 주사전자현미경, X-ray 회절장치, Fourier 변환강도계등으로 확인하고 유사체액에만 침적한 시편의 표면특성과 비교하였다. 실험결과 인산완충용액에서의 침적에 의해 타니타늄 표면에 인산칼슘 형성이 촉진됨을 알 수 있었다. 형성된 층은 입자형의 미세구조를 지닌 하이드록시아파타이트나 $\beta$-TCP의 인산칼슘 층으로 확인되었다. 형성된 층의두께는 pH 8.0, 7.0 그리고 pH 5.8의 인산완충액에서의 침적 순으로 증가하였고, 그 밀도는 pH 7.0, pH8.0그리고 pH5.8의 인산완충액에서의 침적 순으로 증가하였다.

• 한국결정성장학회지
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• 제22권2호
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• pp.99-104
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• 2012

BCP(biphasic calcium phosphate) 분말을 제조하기 위하여 $Ca(NO_3)_2{\cdot}4H_2O$, $(NH_4)_2HPO_4$를 출발 물질로 공침법(co-precipitation process)을 이용하여 합성하였다. 합성된 분말의 열처리 전 후의 HAp(Hydroxyapatite)/${\beta}$-TCP(${\beta}$-Tricalcium phosphate) 결정상 비율 및 분광학적 특성을 XRD 및 FT-IR를 이용하여 분석하였다. BCP 분말의 생체활성 거동을 평가하기 위하여 Hanks' Balanced Salt Solution(HBSS)에 침적시켜 시간에 따라 형상, 이온농도의 변화 및 결정상을 분석한 결과 낮은 결정화도의 HAp가 생성됨을 확인하였다. BCP분말의 세포독성 평가에서도 대조군에 비하여 세포성장률이 우수함을 관찰하였다.

• 한국결정성장학회지
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• 제20권5호
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• pp.243-248
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• 2010

Si-BCP(si-substituted biphasic calcium phosphate)를 제조하기 위하여 $Ca(NO_3)_2{\cdot}4H_2O$, $(NH_4)_2HPO_4$, $Si(OC_2H_5)_4$을 출발 물질로 공침법(co-precipitation process)을 이용하여 합성하였다. 합성된 분말의 HAp/${\beta}$-TCP 결정상 비율 및 Si-P 치환 거동은 X-선 회절 상 분석을 이용하여 측정하였고, silicon ion 첨가 시 나타나는 BCP의 화학적 결합거동을 측정하기 위하여 FT-IR를 사용하여 분석하였다. 또한 Si-BCP 분말의 in-vitro 생분해거동 및 생체활성도를 측정하기 위하여 제조된 분말을 SBF(simulated body fluid) solution에 침적시킨 뒤 분말의 형상과 구성 성분은 SEM과 EDS를 통하여 확인하였다.

• 한국세라믹학회지
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• 제41권12호
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• pp.921-928
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• 2004

수용액의 pH, 소성온도, 반응시간 등을 변화한 조건하에서 $Ca(OH)_2$와 $H_{3}PO_4$ 수용액을 이용하여 인산칼슘계 화합물을 제조하였다. 산성분위기(pH=5.21)에서는 ${\beta}-TCP({\beta}-tricalcium phosphate)$가, pH>7.62에서는 HAp(hydroxyapatite)가 주 결정상으로 관찰되었다. XRD 분석결과, $Ca(OH)_2$와 $H_{3}PO_4$는 빠르게 반응(5분이내)하여 HAp를 생성하였고, 반응 16시간까지 안정적으로 구조를 유지하였다. 우수한 결정성을 나타내는 소성온도는 $1200^{\circ}C$로 관찰되었다. 주사전자현미경(SEM)에 의한 미세구조 관찰 결과, pH가 5.21일 경우 침상 형태의 ${\beta}-TCP$ 입자가, pH 7.62에서는 침상 형태의 HAp가 합성되었다. 그러나 pH 9.16에서는 매우 작고 균일한 구형의 HAp 입자들이 생성되었고, 다시 작은 입자들이 침상으로 재배열된 형상을 관찰할 수 있었다. 합성된 HAp(pH 9.16)를 본차이나 소지에 일정량 혼합하여 본차이나 물성, 즉 결정성, 흡수율, 색도, 파단면의 형상을 측정${\cdot}$분석하였다.

• Journal of Periodontal and Implant Science
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• 제39권sup2호
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• pp.223-230
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• 2009

Purpose: Synthetic bone products such as biphasic calcium phosphate (BCP) are mixtures of hydroxyapatite (HA) and ${\beta}$-tricalcium phosphate (${\beta}$- TCP). In periodontal therapies and implant treatments, BCP provides to be a good bone reconstructive material since it has a similar chemical composition to biological bone apatites. The purpose of this study was to compare bone regeneration capacity of two commercially available BCP. Methods: Calvarial defects were prepared in sixteen 9-20 months old New Zealand White male rabbits. BCP with HA and ${\beta}$- TCP (70:30) and BCP with Silicon-substituted hydroxyapatite (Si-HA) and ${\beta}$-TCP (60:40) particles were filled in each defect. Control defects were filled with only blood clots. Animals were sacrificed at 4 and 8 week postoperatively. Histomorphometric analysis was performed. Results: BCP with HAand ${\beta}$- TCP 8 weeks group and BCP with Si-HA and ${\beta}$- TCP 4 and 8 weeks groups showed statistically significant in crease (P <0.05) in augmented area than control group. Newly formed bone area after 4 and 8 weeks was similar among all the groups. Residual materials were slightly more evident in BCP with HA and ${\beta}$- TCP 8 weeks group. Conclusions: Based on histological results, BCP with HA and ${\beta}$- TCP and BCP with Si-HA and ${\beta}$- TCP appears to demonstrate acceptable space maintaining capacity and elicit significant new bone formation when compared to natural bone healing in 4 and 8 week periods.

• Journal of Biosystems Engineering
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• 제39권3호
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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.

• Restorative Dentistry and Endodontics
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• 제37권1호
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• pp.16-23
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• 2012

Objectives: Present study was undertaken to investigate the crystal growth onto synthetic hydroxyapatite (HA) seeds in pH 4.3 and pH 7.0 supersaturated solutions with different fluoride concentrations. Materials and Methods: 8 groups of pH 4.3 and 7.0 calcium phosphate supersaturated solutions were prepared with different fluoride concentrations (0, 1, 2 and 4 ppm). Calcium phosphate precipitates yield crystal growth onto the HA seed surface while solutions flow. For evaluation of crystallizing process, the changes of $Ca^{2+}$, $PO{_4}^{3-}$, $F^-$ concentrations of the inlet and outlet solutions were determined. The recovered solid samples were weighed to assess the amount of minerals precipitated, and finally determined their composition to deduce characteristics of crystals. Results: During the seeded crystal growth, there were significantly more consumption of $Ca^{2+}$, $PO{_4}^{3-}$, $F^-$ in pH 4.3 solutions than pH 7.0 (p < 0.05). As fluoride concentration increased in pH 4.3 solution, $Ca^{2+}$, $PO{_4}^{3-}$, $F^-$ consumption in experimental solutions, weight increment of HA seed, and fluoride ratio in crystallized samples were increased. There were significant differences among the groups (p < 0.05). But in pH 7.0 solution, these phenomena were not significant. In pH 7.0 solutions, analyses of crystallized samples showed higher Ca/P ratio in higher fluoride concentration. There were significant differences among the groups (p < 0.05). But in pH 4.3 solution, there were not significant differences in Ca/P ratio. Conclusions: Crystal growth in pH 4.3 solutions was superior to that in pH 7.0 solutions. In pH 4.3 solutions, crystal growth increased with showed in higher fluoride concentration up to 4 ppm.

• Journal of Periodontal and Implant Science
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• 제27권2호
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• pp.363-377
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• 1997

The main goal of periodontal therapy is the regeneration of periodontal tissue which has been lost due to destructive periodontal diseases. Although conventional forms of periodontal therapy show sound clinical results, the healing results in long junctional epithelium. There have been numerous materials and surgical techniques developed for new attachment and bone regeneration. Bone grafts can be catagorized into: autografts, allografts, xenografts and bone substitutes. Synthetic bone substitute materials include hydroxyapatite, tricalcium phosphate, calcium carbonate, and Plaster of Paris. Calcium sulfate has found its use in dental practice for the last 30 years. Recent animal studies suggest that periodontal regeneration in 3 wall intrabony defect may be enhanced by the presence of calcium sulfate. And it is well known that 2 wall & 1 wall defect have less osteogenic potential, So we need to study the effect of calcium sulfate in 1 wall intrabony defect in dogs. The present study evaluates the effects of calcium sulfate on the epithelial migration, alveolar bone regeneration and cementum formation in intrabony defects of dogs. Four millimeter-deep one-wall intrabony defects were surgically created in the mesial aspect of anterior teeth and mesial & distal aspects of premolars. The test group received calcium sulfate grafts with a flap procedure. The control underwent flap procedure only. Histologic analysis following 8 weeks of healing revealed the following results: 1. The lengths of junctional epithelium were: 2.52mm in the control, and 1.89mm in the test group. There was no statistical significance between the two groups. 2. Alveolar bone formation were: 0.61mm in the control, and 1.88mm in the test group. There was a statistically significant difference between the two groups (p<0.05). 3. Cementum formations were: l.lmm in the control, and 2.46mm in the test group. There was a statistically significant difference between the two groups (p<0.05). 4. The length of CT adhesion were: O.97mm in the control, and 0.17mm in the test group. There was no statistically significant differences between the two groups These results suggest that the use of calcium sulfate in intrabony defects has little effect on junctional epithelium migration, but has significant effects on new bone and new cementum formations.

• 한국결정성장학회지
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• 제22권6호
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• pp.279-285
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• 2012

BCP, Mg-BCP, Si-BCP 분말을 공침법(co-precipitation process)을 이용하여 합성하였다. 제조된 분말을 X-선 회절 분석(XRD), 적외선분광분석(FTIR)을 이용하여 특성을 분석하였다. Ca/P 몰 비율이 1.602인 칼슘 결손 아파타이트 공침물을 제조하여 $1000^{\circ}C$ 열처리 과정을 통하여 HAp와 ${\beta}$-TCP 상이 혼재된 BCP, Mg-BCP, Si-BCP을 합성할 수 있었다. 제조된 분말의 생체활성 거동을 평가하기 위하여 Hanks' Balanced Salt Solution(HBSS)에 침적시켜 시간에 따라 형상의 변화 및 결정상을 분석한 결과, BCP 분말에 비하여 금속 이온이 치환된 BCP 분말에서 빠른 생체활성을 관찰할 수 있었다. MTT assay를 통한 세포 성장률 평가에서모든 분말에서 시간 경과에 따라 독성을 나타내지 않았으며, 세포의 활성이 증가하였다.

• 한국재료학회:학술대회논문집
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• 한국재료학회 2009년도 추계학술발표대회
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• pp.42.2-42.2
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• 2009

인체의 치아 및 뼈는 무기질 성분과 단백질로 구성되어 있다. 생체세라믹스의 일종인 수산화아파타이트(Hydroxyapatite, HA; $Ca_{10}(PO_4)_6(OH)_2$)는 결정학적, 화학적으로뼈의 무기질 성분과 거의 유사하여 실제 체내에 들어가면 주위 뼈와 화학적 반응을 하여 단단한 결합을 이루는 생체활성(bioactive)을 가진 것으로 알려져 있다. 또한, 인산삼칼슘(Tri-Calcium Phosphate, TCP; $Ca_3(PO_4)_2$)은 체내에 이식 시 체액에 용해되어 신생골을 유도하는 생체흡수성(bioresorbable) 세라믹스로 알려져 있다. 상기 2종류를 포함한 인산칼슘계 화합물은 우수한 생체친화성에도 불구하고 역학 특성이 낮아, 하중을 거의 받지 않는 분야에만 사용되고 있는 실정이며, 하중을받는 분야(load-bearing part)에 적용하기 위해서는 고강도/고인성의 세라믹스와의 micro-composite이나 인산칼슘계화합물을 금속 표면에 코팅한 macro-composite의 형태로 사용되고 있다. 하중을 거의 받지 않는 분야, 예를 들어 치아 결손부를 보충할 dental shot과 같은 인산칼슘계 다공질 골충전재의 경우에도 취급 시 잘게 파손되는 문제점이 있어 치과의사들이 어려움을 호소하고 있는 실정이다. 본 연구에서는 HA, TCP의 역학특성을 증진시키고자 소결 공정 제어를 통하여 미세조직을 변화시켰으며, 미세조직 변화에 따른 세포반응성을 골포세포주를 이용하여 평가하였다.