• Journal of the Korean Ceramic Society
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• v.50 no.6
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• pp.489-494
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• 2013

Nano-sized titanium oxide powders were synthesized by a polymer matrix technique using pulp and Titanium tetraisopropoxide (TTIP) as starting materials. The synthesized powders were characterized by XRD and FE-SEM. The particle size of the powders was controlled by preparation conditions, such as heat treatment temperature and time. After investigating various drying and heat treatment conditions, 50-100 nm sized homogeneous titanium oxide particles were obtained by treating at $600^{\circ}C$ for 1 h. The crystallization and rapid growth of particles was accelerated by increasing heat treatment temperature and time. Anatase phase generated below $600^{\circ}C$ transformed to the rutile phase with increasing heat treatment temperature. Moreover, above $800^{\circ}C$, heat treatment time had a very large influence on particle growth, and changing the heating condition also had a large influence on crystal growth.

• Proceedings of the Korean Vacuum Society Conference
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• 2000.02a
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• pp.107-107
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• 2000

최근 반도체 소자의 고집적화 및 대용량화의 경향에 다라 MOSFET 소자 제작에 이동되는 게이트 산화막의 두께가 수 nm 정도까지 점점 얇아지는 추세이고 Giga-DRAM급 차세대 UNSI소자를 제작하기 위해 5nm이하의 게이트 절연막이 요구된다. 이런 절연막의 두께감소는 게이트 정전용량을 증가시켜 트랜지스터의 속도를 빠르게 하며, 동시에 저전압동작을 가능하게 하기 때문에 게이트 산화막의 두께는 MOS공정세대가 진행되어감에 따라 계속 감소할 것이다. 따라서 절연막 두께는 소자의 동작 특성을 결정하는 중요한 요소이므로 이에 대한 정확한 평가 방법의 확보는 공정 control 측면에서 필수적이다. 그러나, 절연막의 두께가 작아지면서 게이트 산화막과 crystalline siliconrksm이 계면효과가 박막의 두께에 심각한 영향을 주기 때문에 정확한 두께 계측이 어렵고 계측방법에 따라서 두께 계측의 차이가 난다. 따라서 차세대 반도체 소자의 개발 및 양산 체계를 확립하기 위해서는 산화막의 두께가 10nm보다 작은 1nm-5nm 수준의 박막 시료에 대한 두께 계측 방법이 확립이 되어야 한다. 따라서, 본 연구에서는 습식 산화 공정으로 제작된 3nm-7nm 의 게이트 절연막을 현재까지 알려진 다양한 두께 평가방법을 비교 연구하였다. 절연막을 MEIS (Medim Energy Ion Scattering), 0.015nm의 고감도를 가지는 SE (Spectroscopic Ellipsometry), XPS, 고분해능 전자현미경 (TEM)을 이용하여 측정 비교하였다. 또한 polysilicon gate를 가지는 MOS capacitor를 제작하여 소자의 Capacitance-Voltage 및 Current-Voltage를 측정하여 절연막 두께를 계산하여 가장 좋은 두께 계측 방법을 찾고자 한다.다. 마이크로스트립 링 공진기는 링의 원주길이가 전자기파 파장길이의 정수배가 되면 공진이 일어나는 구조이다. Fused quartz를 기판으로 하여 증착압력을 변수로 하여 TiO2 박막을 증착하였다. 그리고 그 위에 은 (silver)을 사용하여 링 패턴을 형성하였다. 이와 같이 공진기를 제작하여 network analyzer (HP 8510C)로 마이크로파 대역에서의 공진특서을 측정하였다. 공진특성으로부터 전체 품질계수와 유효유전율, 그리고 TiO2 박막의 품질계수를 얻어내었다. 측정결과 rutile에서 anatase로 박막의 상이 변할수록 유전율은 감소하고 유전손실은 증가하는 결과를 나타내었다.의 성장률이 둔화됨을 볼 수 있다. 또한 Silane 가스량이 적어지는 영역에서는 가스량의 감소에 의해 성장속도가 둔화됨을 볼 수 있다. 또한 Silane 가스량이 적어지는 영역에서는 가스량의 감소에 의해 성장속도가 줄어들어 성장률이 Silane가스량에 의해 지배됨을 볼 수 있다. UV-VIS spectrophotometer에 의한 비정질 SiC 박막의 투과도와 파장과의 관계에 있어 유리를 기판으로 사용했으므로 유리의투과도를 감안했으며, 유리에 대한 상대적인 비율 관계로 투과도를 나타냈었다. 또한 비저질 SiC 박막의 흡수계수는 Ellipsometry에 의해 측정된 Δ과 Ψ값을 이용하여 시뮬레이션한 결과로 비정질 SiC 박막의 두께를 이용하여 구하였다. 또한 Tauc Plot을 통해 박막의 optical band gap을 2.6~3.7eV로 조절할 수 있었다. 20$0^{\circ}C$이상으로 증가시켜도 광투과율은 큰 변화를 나타내지 않았다.부터 전분-지질복합제의 형성 촉진이 시사되었다.이것으로 인하여 호화억제에 의한 노화 방지효과가 기대되었지만 실제로 빵의 노화는 현저히 진행되었다

• The Journal of Korean Academy of Prosthodontics
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• v.43 no.6
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• pp.751-763
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• 2005

Statement of problem. To improve a direct implant fixation to the bone, various strategies have been developed focusing on the surface of materials. The surface quality of the implant depends on the chemical, physical, mechanical and topographical properties of the surface. The different properties will interact with each other and a change in thickness of the oxide layer may also result in a change in surface energy, the surface topography and surface, chemical composition. However, there is limited the comprehensive study with regard to changed surface and biologic behavior of osteoblast by anodization. Purpose of study. The aim of this study was to analyze the characteristics of an oxide layer formed and to evaluate the cellular biologic behaviors on titanium by anodic oxidation (anodization) by cellular proliferation, differentiation, ECM formation and gene expression. And the phospholipase activity was measured on the anodized surface as preliminary study to understand how surface properties of Ti implant are transduced into downstream cellular events. Methods and Materials. The surface of a commercially pure titanium(Grade 2) was modified by anodic oxidation. The group 1 samples had a machined surface and other three experimental specimens were anodized under a constant voltage of 270 V(Group 2), 350 V(Group 3), and 450 V(Group 4). The specimen characteristics were inspected using the following five categories; the surface morphology, the surface roughness, the thickness of oxide layer, the crystallinity, and the chemical composition of the oxide layer. Cell numbers were taken as a marker for cell proliferation. While the expression of alkaline phosphatase and Runx2 (Cbfa1) was used as early differentiation marker for osteoblast. The type I collagen production was determined, which constitutes the main structural protein of the extracellular matrix. Phospholipase $A_2$ and D activity were detected. Results. (1) The anodized titanium had a porous oxide layer, and there was increase in both the size and number of pores with increasing anodizing voltage. (2) With increasing voltage, the surface roughness and thickness of the oxide film increased significantly (p<0.01), the $TiO_2$phase changed from anatase to rutile. During the anodic oxidization, Ca and P ions were more incorporated into the oxide layer. (3) The in vitro cell responses of the specimen were also dependant on the oxidation conditions. With increasing voltage, the ALP activity, type I collagen production, and Cbfa 1 gene expression increased significantly (p<0.01), while the cell proliferation decreased. (4) In preliminary study on the relation of surface property and phospholipase, PLD activity was increased but $PLA_2$ activity did not changed according to applied voltage. Conclusion. The anodized titanium shows improved surface characteristics than the machined titanium. The surface properties acquired by anodization appear to give rise more mature osteoblast characteristics and might result in increased bone growth, and contribute to the achievement of a tight fixation. The precise mechanism of surface property signaling is not known, may be related to phospholipase D.

• Journal of Periodontal and Implant Science
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• v.37 no.sup2
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• pp.427-445
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• 2007

To improve osseointegration at the boneto-implant interface, several studies have been carried out to modify titanium surface. Variations in surface texture or microtopography may affect the cellular response to an implant. Osteoblast-like cells attach more readily to a rougher titanium surface, and synthesis of extracellular matrix and subsequent mineralization were found to be enhanced on rough or porous coated titanium. However, regarding the effect of roughened surface by physical and mechanical methods, most studies carried out on the reactions of cells to micrometric topography, little work has been performed on the reaction of cells to nanotopography. The purpose of this study was to examme the response of osteoblast-like cell cultured on blasted surfaces and alkali treated surfaces, and to evaluate the influence of surface texture or submicro-scaled surface topography on the cell attachment, cell proliferation and the gene expression of osteoblastic phenotype using ROS 17/2.8 cell lines. In scanning electron micrographs, the blasted, alkali treated and machined surfaces demonstrated microscopic differences in the surface topography. The specimens of alkali treatment had a submicro-scaled porous sur-face with pore size about 200 nm. The blasted surfaces showed irregularities in morphology with small(<10 ${\mu}m$) depression and indentation among flatter-appearing areas of various sizes. Based on profilometry, the blasted surfaces was significantly rougher than the machined and the alkali treated surfaces (p$TiO_2$) were observed on alkali treated surfaces, whereas not observed on machined and blasted surfaces. The attachment morphology of cells according to time was observed by the scanning electron microscope. After 1 hour incubation, the cells were in the process of adhesion and spreading on the prepared surfaces. After 3 hours, the cells on all prepared surfaces were further spreaded and flattened, however on the blasted and alkali treated surfaces, the cells exhibited slightly irregular shapes and some gaps or spaces were seen. After 24 hours incubation, most cells of the all groups had a flattened and polygonal shape, but the cells were more spreaded on the machined surfaces than the blasted and alkali treated surfaces. The MTT assay indicated the increase on machined, alkali treated and blasted surfaces according to time, and the alkali treated and blasted surfaces showed significantly increased in optical density comparing with machined surfaces at 1 day (p<0.01). Gene expression study showed that mRNA expression level of ${\alpha}\;1(I)$ collagen, alkaline phosphatase and osteopontin of the osteoblast-like cells showed a tendency to be higher on blasted and alkali treated surfaces than on the machined surfaces, although no siginificant difference in the mRNA expression level of ${\alpha}\;1(I)$ collagen, alkaline phosphatase and osteopontin was observed among all groups. In conclusion, we suggest that submicroscaled surfaces on osteoblast-like cell response do not over-ride the one of the surface with micro-scaled topography produced by blasting method, although the microscaled and submicro-scaled surfaces can accelerate osteogenic cell attachment and function compared with the machined surfaces.