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열산화법에 의한 티타늄 임플란트의 인산칼슘 결정의 형성 능력 증진
황규석,안준형,이선옥,윤연흠,강보안,오정선,김상복,Hwang, Kyu-Seog,An, Jun-Hyung,Lee, Seon-Ok,Yun, Yeon-Hum,Kang, Bo-An,Oh, Jeong-Sun,Kim, Sang-Bok 한국세라믹학회 2002 한국세라믹학회지 Vol.39 No.5
티타늄 임플란트의 표면을 열산화법을 이용하여 티타늄의 표면 위에 생체활성을 갖는 $TiO_2$ 박막을 생성시켜 다양한 의료분야의 응용 가능성을 검토하였다. 시판되고 있는 순수한 티타늄 디스크를 세척 공정을 거친 후, 공기와 아르곤 분위기에서 500, 550, 600, 650, 700${\circ}C$의 온도로 10분간 각각 열산화 처리를 실시하였다. 열처리된 시편의 인산칼슘 결정의 형성 능력을 시험하기 위하여 36.5${\circ}C$의 Eagle's minimum essential medium 용액에서 15일 동안 침적시험을 행하였다. 침적하기 전과 후의 시편의 표면 형상과 표면 조성을 Field Emission-Scanning Electron Microscopy(FE-SEM)와 Energy Dispersive X-ray Spectrometry(EDS)로 각각 분석하였다. In vitro 시험에서 미세한 $TiO_2$ 결정이 생성된 박막의 표면에는 탄소가 함유된 인산칼슘 결정이 생성됨을 확인하였다. Titanium oxide film was deposited on the commercially pure titanium (cp-Ti) by thermal oxidation method for its medical application. The cp-Ti disks were cleaned and then heat-treated at the temperatures of 500, 550, 600, 650, and 700${\circ}C$, respectively, for 10 min in air or Ar. To test the ability of calcium phosphate formation, the specimens were immersed in the Eagle's minimum essential medium solution at 36.5${\circ}C$ for 15 days. The morphology and chemical composition of the surfaces before and after soaking were analyzed by using FE-SEM and EDS. The in-vitro formation of carbonated calcium phosphate on the thin films containing nano-sized $TiO_2$ crystals was identified.
정전 분무법으로 제조한 β-형 PVDF 막에 미치는 니켈 질산염 첨가의 영향
황규석(Kyu-Seog Hwang),김명윤(Myung-Yoon Kim),손병래(Byeongrae Son),황보승(Seung Hwang-Bo),노형갑(Hyeonggap No) 대한전기학회 2018 전기학회논문지 Vol.67 No.10
PVDF as a semicrystal polymer, having a structure with C-F dipole moments, has been widely investigated because of its excellent chemical stability, mechanical strength, and ferroelectricity. In this study, ferroelectic β type – PVDF layer was prepared by using an electrostatic spray deposition method and the effects of the addition of Ni-nitrate in precursor solution on the properties of PVDF layer were evaluated. Crystallinity and chemical structure of the PVDF layer were analyzed by a X-ray diffraction and Fourier Transform Infrared Spectrophotometer. Surface structure and fractured cross section of the layer were examined by a field emission-scanning electron microscope. LCR meter was used to obtain the dielectric properties of the layer. As the addition of an inorganic metal salt in PVDF sol, β type – PVDF crystals were appeared in the hydrated metal salts doped-layer since the strong hydrogen bondings (O-H…F-C)n due to high polarity of OH- were formed.
티타늄 기판 위에 강유전성 BaTiO<sub>3</sub>박막 형성과 분극처리에 의한 Eagle’s MEM 용액에서의 Calcium Phosphate 생성
이용렬,정영화,황규석,송호준,박영준,Lee, Yong-Ryeol,Jeong, Young-Hwa,Hwang, Kyu-Seog,Song, Ho-Jun,Park, Yeong-Joon 한국재료학회 2002 한국재료학회지 Vol.12 No.7
Titanium (Ti) is a bioinert material and has lower elastic coefficient and better strength/volume property than other metals. Ferroelectric materials show alignment of positive and negative charges by poling treatment. This study was purposed to develop a new implant system by combining the advantages of Ti and ferroelectric property of $BaTiO_3$ (BTO). It was performed with the assumption that the $Ca^{2+ }$ ions would be easily attracted on negatively charged surface and the attracted cation might behave as nuclei for bone-like crystal growth in biological solutions. A ferroelectric BTO thin film on Ti was fabricated and the effect of poling treatment on the improvement of calcium phosphate (Ca-P) formation in biological solutions was evaluated. After immersion in Eagle’s minimum essential media (MEM) solution, NaCl was formed on Ti, and Ca-P layer containing NaCl was formed on Ti-O. Weak and sparse Ca-P layers were formed on BTO, while thick, homogeneous, and dense Ca-P layer was formed on negatively polarized BTO (N-BTO), which was confirmed by FE-SEM and EDX. In summary, these results demonstrate that poling the ferroelectric BTO surface negatively is effective for the formation of Ca-P layer in MEM solution, and that N-BTO coating on Ti could be used as a possible alternative method for enhancing the osseointegration of the implants.
정전분무 열분해법에 의한 나노분말의 제조 및 하이드록시 아파타이트 형성능력 평가
이영환,전경옥,전영선,이지창,황규석,Lee, Young-Hwan,Jeon, Kyung-Ok,Jeon, Young-Sun,Lee, Ji-Chang,Hwang, Kyu-Seog 한국결정성장학회 2006 韓國結晶成長學會誌 Vol.16 No.6
본 연구에서는 새로운 나노 분말 제조방법 중의 하나인 정전분무 열분해법을 이용하여 칼슘 포스페이트 나노분말을 제조하였다. 정전 분무된 분말은 공기 중에서 $400^{\circ}C$로 30분간 열처리하여 고상화하였다. 결정화된 분말의 하이드록시 아파타이트 형성능력을 평가하기 위하여 Eagle's minimum essential medium solution(MEM)을 사용하였으며, MEM 용액에 침전된 후의 분말의 특성평가를 위하여 X-선 회절 분석법, 전계 방사 주사형 전자 현미경, 에너지 분산 X-선 분광계 및 퓨리에 변환 적외선 분광계를 사용하여 분석을 행하였다. 비정질 구조를 가진 나노 분말은 MEM 용액에 15일 침전 후, 분말의 표면에 유도된 하이드록시 아파타이트 결정을 확인할 수 있었다. Electrostatic spray pyrolysis, a novel fabrication technique, has been used in this study to prepare calcium phosphate nano powders. Final annealing was done at $400^{\circ}C$ for 30min in air. The hydroxyapatite - forming ability of the annealed powder has been evaluated in Eagle's minimum essential medium solution (MEM). X-ray diffraction analysis, field emission - scanning electron microscope, energy dispersive X-ray spectroscope, and Fourier transform infrared spectroscope were used to characterized the annealed powders after immersion in MEM. The powder with an amorphous structure induced hydroxyapatite formation on their surfaces after immersion fer 15 days.
지르코늄 나프테네이트를 이용한 나노결정질 ZrO<sub>2</sub> 박막의 제조와 칼슘 포스페이트 형성 능력의 평가
오정선,안준형,윤연흠,강보안,김상복,황규석,심연아,Oh, Jeong-Sun,Ahn, Jun-Hyung,Yun, Yeon-Hum,Kang, Bo-An,Kim, Sang-Bok,Hwang, Kyu-Seog,Shim, Yeon-A 한국세라믹학회 2002 한국세라믹학회지 Vol.39 No.9
In order to investigate the calcium phosphate forming ability of nanocrystalline $ZrO_2$ film, we prepared $ZrO_2/Si$ structure by using a chemical solution deposition with a zirconium naphthenate as a starting material. Precursor sol was spin-coated onto the (100)Si substrate and prefired at 500$^{\circ}C$ for 10 min in air, followed by final annealing at 800$^{\circ}C$ for 30 min in air. Crystallinity of the annealed film was examined by X-ray diffraction analysis. Surface morphology and surface roughness of the film were characterized by field emission-scanning electron microscope and atomic force microscope. After annealing, nanocrystalline $ZrO_2$ grains were obtained on the surface of the film with a homogeneous interface between the film and substrate. After immersion for 1 or 5 days in a simulated body fluid, formation of calcium phosphate was observed on $ZrO_2$ film annealed at 800$^{\circ}C$ by energy dispersive X-ray spectrometer. The fourier transform infrared spectroscopy revealed that carbonate was substituted into the calcium phosphate. 나노 결정질 $ZrO_2$ 박막을 제조하여 박막의 표면에서 인산칼슘을 유도하는 능력을 편가하기 위하여, 지르코늄 나프테네이트를 출발물질로 사용하고 화학적 용액법을 이용하여, $ZrO_2/Si$ 구조를 제작하였다. 코팅용액을 (100)Si 기판 위에 스핀코팅한 후, 500$^{\circ}C$에서 10분간 전열처리와 800$^{\circ}C$에서 30분간 최종열처리를 행하였고, 모든 열처리는 공기분위기에서 실시하였다. X-ray diffraction analysis를 이용하여 열처리된 박막의 결정화도를 조사하였고, 표면의 미세구조와 표면 거칠기를 field emission-scanning electron microscope와 atomic force microscope를 이용하여 관찰하였다. 열처리 후의 박막은 표면에 미세한 $ZrO_2$ 나노 결정이 생성되어 있었으며, 박막의 계면은 매우 균질 하였다. 유사생채용액에 1일 및 5일간 침적된 샘플의 표면위에 형성된 인산칼슘을 energy dispersive X-ray spectrometer를 이용하여 관찰하였고, fourier transform infrared spectroscopy를 이용하여 인산칼슘에 카본이 치환되어 있음을 확인하였다.