• Title/Summary/Keyword: Microstructure analysis

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Structural and Optical Properties of TiO2 Thin Films Prepared by RF Reactive Magnetron Sputtering (RF reactive magnetron sputtering으로 제조한 TiO2 박막의 구조 및 광학적 특성)

  • Gang, Gye-Won;Lee, Yeong-Hun;Gwak, Jae-Cheon;Lee, Dong-Gu;Jeong, Bong-Gyo;Park, Seong-Ho;Choe, Byeong-Ho
    • Korean Journal of Materials Research
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    • v.12 no.6
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    • pp.452-457
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    • 2002
  • Titanium oxide films were prepared by RF reactive magnetron sputtering. The effect of sputtering conditions on structural and optical properties was investigated systemically as a function of sputtering pressure(5~20 mTorr) and $O_2/Ar$ flow ratio(0.08~0.4). The results of the X-ray diffraction showed that all films had only the anatase $TiO_2$ phase. At low sputtering pressure and $O_2/Ar$ flow ratio, the films had preferred orientations along [101] and [200] directions. As the sputtering pressure and $O_2/Ar$ flow ratio increased, the intensity of the 101 and 200 diffraction peaks decreased gradually. The microstructure of the sputtered films showed the fine grain size (20nm~50nm) and columnar microcrystals perpendicular to the substrate. With increasing the sputtering pressure and decreasing $O_2/Ar$ flow ratio, the sputtered films showed the more porous columnar structure. XPS analysis showed that stoichiometric $TiO_2$ films were deposited at 7 mTorr sputtering pressure and 0.2 $O_2/Ar$ flow ratio. The results of the X-ray diffraction showed that all films had only the anatase $TiO_2$ phase. Ellipsometeric analysis showed that the refractive index increased from 2.32 to 2.46 as the sputtering pressure decreased. The packing density calculated using the refractive index varied from 0.923 to 0.976, indicating that $TiO_2$films became denser as the sputtering pressure decreased.

Study on Effect of Various Underlayer on Bilayer Agglomerlation (다양한 하지층이 이중층의 응집현상에 미치는 영향에 관한 연구)

  • Ha, J.H.;Ryu, D.H.;Im, H.W.;Jung, J.M.;Choi, H.J.;Hong, I.G.;Koh, J.H.;Koo, S.M.;Kamiko, M.;Ha, J.G.
    • Journal of the Korean Vacuum Society
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    • v.21 no.5
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    • pp.233-241
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    • 2012
  • We have deposited the bilayer consisted of the underlayer and the overlayer by using DC magnetron sputter on Single crystal MgO (001) substrate. This bilayer was fabricated at fixed annealing temperature and time. We have controlled agglomeration effect by changing of the bilayer thickness. Finally, we have made the self-organization and nano-structured film. In this processing, we have made nano-dot which consists of the underlayer and the overlayer, unlike the existing method called the agglomeration effect in the single layer. The underlayer has deposited using Ti, Cr and Co. And the overlayer has deposited with Ag. Through the analysis of Atomic force microscopy (AFM), the microstructure of underlayer is observed by AFM to confirm the formation of nano-dot. As the nano-dot through above processing, we have found that the nano-dot has the different shape. As a result, when we manufactured nano-dot through the agglomeration effect of bi-layer, the best matching material is Ti for underlayer. And also, we have found that MgO/Ti/Ag samples have been grown expitaxially toward the direction of MgO (001) by X-ray Diffraction analysis.

Composition Changes in Cement Matrix of RC Column Exposed to Fire (화재에 노출된 RC기둥 시멘트 매트릭스의 구성성분 변화)

  • Kim, Jung-Joong;Youm, Kwang-Soo
    • Journal of the Korea Concrete Institute
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    • v.26 no.3
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    • pp.369-375
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    • 2014
  • This study examined the changes of microstructural compositions in cement matrix according to the depth from the surface of a reinforced concrete (RC) column exposed to fire. The RC column was exposed to a standard fire for 180 minutes. After the fire test, core samples passing through the column section were obtained. Using the core samples, the remaining fractions of calcium-silicate-hydrates (C-S-H) and calcium hydroxide in cement matrix at the surface, the depth of 40 mm and 80 mm and the center (175 mm) were examined using thermal gravimetric analysis (TGA) and X-ray diffraction analysis (XRDA). Using nuclear magnetic resonance (NMR) technique, the silicate polymerization of C-S-H in cement matrix was also evaluated. The experimental results indicated that the amount of C-S-H loss at the center of column experiencing the transferred fire temperature of $236^{\circ}C$ has been underestimated as the TGA results showed the highest C-S-H contents are located at the depth of 80 mm, where the transferred fire temperature is $419^{\circ}C$. Moreover, the destruction of silicate connections at the center was observed as similar as that at the depth of 40 mm, where the transferred fire temperature was $618^{\circ}C$. This might be attributed to the temperature changes during cooling time after the fire test was neglected. Due to the relatively low thermal conductivity of concrete, the high temperature, which can affect the change of microstructure in cements, will hold longer at the center of the column than other depth.

Corrosion behaviors of Cp-Ti and Ti-6Al-4V alloys by TiN coating (TiN 코팅된 Ti 및 Ti-6Al-4V합금의 부식거동)

  • Lee, Soon-Hyun;Jung, Yoong-Hun;Choi, Han-Chul;Ko, Yeong-Mu
    • Journal of Technologic Dentistry
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    • v.30 no.1
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    • pp.25-31
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    • 2008
  • Cp-Ti and Ti-6Al-4V alloys commonly used dental implant materials, particularly for orthopaedic and osteosynthesis because of its suitable mechanical properties and excellent biocompatibility. This alloys have excellent corrosion behavior in the clinical environment. The first factor to decide the success of dental implantation is sufficient osseointegration and high corrosion resistance between on implant fixture and its surrounding bone tissue. In this study, in order to increase corrosion resistance and biocompatibility of Cp-Ti and Ti-6Al-4V alloy that surface of manufactured alloy was coated with TiN by RF-magnetron sputtering method. The electrochemical behavior of TiN coated Cp-Ti and Ti-6Al-4V alloy were investigated using potentiodynamic (EG&G Co, PARSTAT 2273. USA) and potentiostatic test (250mV) in 0.9% NaCl solution at 36.5 $\pm$ 1$^{\circ}C$. These results are as follows : 1. From the microstructure analysis, Cp-Ti showed the acicular structure of $\alpha$-phase and Ti-6Al-4V showed the micro-acicular structure of ${\alpha}+{\beta}$ phase. 2. From the potentiodynamic test, Ecorr value of Cp-Ti and Ti-6Al-4V alloys showed -702.48mV and -319.87mV, respectively. Ti-6Al-4V alloy value was higher than Cp-Ti alloy. 3. From the analysis of TiN and coated layer, TIN coated surface showed columnar structure with 800 nm thickness. 4. The corrosion resistance of TiN coated Cp-Ti and Ti-6Al-4V alloys were higher than those of the non-coated Ti alloys in 0.9% NaCl solution from potentiodynamic test, indicating better protective effect. 5. The passivation current density of TiN coated Cp-Ti and Ti-6Al-4V alloys were smaller than that of the noncoated implant fixture in 0.9% NaCl solution, indicating the good protective effect resulting from more compact and homogeneous layer formation.

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Analysis of microstructure for glass-ceramics made of silicate glasses containing EAF dust (제강분진이 첨가된 규산염계 결정화유리의 미세구조 분석)

  • Kim, H.S.;Kang, S.G.
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.16 no.5
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    • pp.227-234
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    • 2006
  • Microstructures of free surface and interior of glass-ceramics obtained by heat treating silicate glass specimen containing electric arc furnace dust(EAF dust) were observed. The crystallization temperature, $T_c$ of glassy specimen was measured around $850^{\circ}C$ from the result of different thermal analysis so heat treatment temperature to obtain glass-ceramic specimen was selected as $950^{\circ}C$ for 1 hr. Glass specimens containing 50 wt% dust were amorphous, while glass specimens containing 70 wt% dust showed spinel crystal peaks in XRD results. In case of glass-ceramic specimens, spinel crystalline phase was appeared with willemite, and willemite crystal peak intensity increased with increasing dust contents. The fractured surface of glass specimens containing 50 wt% dust was smooth like mirror surface, but that containing 70 wt% dust showed spinel crystals of 10 ${\mu}m$ size in glass matrix. In case of glass-ceramic specimens, ZnO crystal particles of $2{\sim}5{\mu}m$ size were produced in free surface and glassy phase, spinel and willemite crystal phases existed in interior. There were no crystals in glasses containing 50 wt% dust, while glass containing 70 wt% dust had 14 vol% crystals. Crystallinity of glass-ceramic specimens containing 50 and 70 wt% dust were 19 and 43%, respectively. When microstructures of glass and glass-ceramic specimens were observed through SEM after TCLP experiment, glass specimens showed flaking phenomenon while glass-ceramic specimens showed a slight corrosion evidence without any cracks.

Characterization of Calcium Lactate Prepared from Butter Clam Saxidomus purpuratus Shell Powder (개조개(Saxidomus purpuratus) 패각분말로부터 젖산칼슘의 제조 및 특성)

  • Yoon, In Seong;Lee, Gyoon-Woo;Lee, Hyun Ji;Park, Sung Hwan;Park, Sun Young;Lee, Su Gwang;Kim, Jin-Soo;Heu, Min Soo
    • Korean Journal of Fisheries and Aquatic Sciences
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    • v.49 no.3
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    • pp.301-309
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    • 2016
  • To facilitate the effective use of butter clam shell as a natural calcium resource, we determined the optimal conditions for calcium lactate (BCCL) preparation with high solubility using response surface methodology (RSM). The polynomial models developed by RSM for pH, solubility and yield were highly effective in describing the relationships between factors (P<0.05). Increased molar ratios of calcined powder (BCCP) from butter clam shell led to reduced solubility, yield, color values and overall quality. The critical values of multiple response optimization to independent variables were 1.75 M and 0.94 M for lactic acid and BCCP, respectively. The actual values (pH 7.23, 97.42% for solubility and 423.22% for yield) under optimization conditions were similar to the predicted values. White indices of BCCLs were in the range of 86.70–90.86. Therefore, organic acid treatment improved color value. The buffering capacity of BCCLs was strong, at pH 2.82 to 3.80, upon the addition of less than 2 mL of 1 N HCl. The calcium content and solubility of BCCLs were 6.2–16.7 g/100 g and 93.6-98.5%, respectively. Fourier transform analysis of infrared spectroscopy data identified BCCL as calcium lactate pentahydrate, and the analysis of microstructure by field emission scanning electron microscopy revealed an irregular form.

A Study on Conservation and Material Characteristics of Outdoor Bronze Sculpture : Kim Chan Shik's 'Feeling' (야외 청동 조각작품의 보존과 재질특성 연구 - 김찬식 '정(情)'을 중심으로 -)

  • Kwon, Hee Hong;Kim, Ye Seung;Kim, Beom Jun;Choi, Nam Young;Park, Hye Sun;Kim, Jung Suk
    • Journal of Conservation Science
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    • v.33 no.3
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    • pp.155-165
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    • 2017
  • As interest in the public display of art and outdoor sculptures is increasing, the conservation and treatment of these sculptures is becoming increasingly crucial. Long-term exposure to the natural elements and atmospheric pollution can cause corrosion and deterioration in outdoor sculptures. In the case of Kim Chan Shik's "Feeling", which was exhibited in the outdoor sculpture park at the National Museum of Modern and Contemporary Art (MMCA), the patina of the sculpture was damaged during a long outdoor exhibition. Therefore, the treatment process was as follows: recording of condition, sanding, repatination, and wax coating. Consequently, the sculpture was restored similar to the original. Chemical analysis revealed that the sculpture was crafted from bronze and was cast from a quaternary alloy of Cu-Pb-Sn-Zn. The welding is lower in Zn, Sn, and Pb content than the metal used in the sculpture itself. Bright strains contain about 13.0 wt% Sn and 10.5 wt% Pb. The strains are higher in Sn and Pb content than the rest of the metal in the sculpture (7.0 wt% Sn and 4.4 wt% Pb). As a result of component analysis and microstructure observation, the material is estimated to have been made by casting without artificial treatment.

A Micro Finite Element Analysis on Effects of Altering Monomer-to-Powder ]Ratio of Bone Cement During Vertebroplasty (골 시멘트 중합 비율 변경이 척추성형술 치료에 미치는 영향에 대한 비교 분석)

  • 김형도;탁계래;김한성
    • Journal of Biomedical Engineering Research
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    • v.23 no.6
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    • pp.451-458
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    • 2002
  • Osteoporosis is a systemic skeletal disease caused by low bone mass and the decrease of bone density in the microstructure of trabecular bone. Drug therapy(PTH Parathyroid hormone) may increase the trabecular thickness and thus bone strength. Vertebroplasty is a minimally invasive surgery foy the treatment of osteoporotic vertebral compression fracture. This Procedure includes Puncturing vertebrae and filling with Polymethylmethacrylate(PMMA). Although altering recommended monomer-to-Powder ratio affects material properties of bone cement, clinicians commonly alter the mixture ratio to decrease viscosity and increase the working time. The Purposes of this study were to analyze the effect of 4he monomer-to-powder ratio on the mechanical characteristics of trabecular. In this paper, the finite element model of human vertebral trabecualr bone was developed by modified Voronoi diagram, to analyze the relative effect of hormone therapy and vertebroplasty at the treatment of osteoporotic vertebrae. Trabeuclar bone models for vertebroplasty with varied monomer-to-Powder ratio(0.40∼1.07 ㎖/g) were analyzed. Effective modulus and strength of bone cement-treated models were approximately 60% of those of intact models and these are almost twice the values of hormone-treated models. The bone cement models with the ratio of 0.53㎖/g have the maximum modulus and strength. For the ratio of 1.07㎖/g, the modulus and strength were minimum(42% and 49% respectively) but these were greater than those for drug therapy. This study shows that bone cement treatment is more effective than drug therapy. It is found that in vertebroplasty, using a monomer-to-powder ratio different from that recommended by manufacturer nay significantly not only reduce the cement's material Properties but also deteriorate the mechanical characteristics of osteoporotic vertebrae.

A Study on the High Frequency Ultrasonic Attenuation Characterization in Artificially Aging Degraded 2.25Cr-1Mo Steel (2.25Cr-1Mo 강 인공 열화재의 고주파수 초음파 감쇠특성에 관한 연구)

  • Park, Ik-Keun;Park, Un-Su;Kim, Chung-Seok;Kim, Hyun-Mook;Kwun, Sook-In;Byeon, Jai-Won
    • Journal of the Korean Society for Nondestructive Testing
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    • v.21 no.4
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    • pp.439-445
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    • 2001
  • The destructive method is reliable and widely used lot the estimation of material degradation but, it have time-consuming and a great difficulty in preparing specimens from in-service industrial facilities. Therefore, the estimation of degraded structural materials used at high temperature by nondestructive evaluation such as electric resistance method, replica method, Barkhausen noise method, electro-chemical method and ultrasonic method are strongly desired. Ultrasonic nondestructive evaluation technique has been reported good to attain efficiency of measurement, high sensitivity of measurement, and rapidity and reliability of result interpretation. In this study, it was verified experimentally the feasibility of the evaluation of degraded 2.25Cr-1Mo steel specimens which were prepared by the isothermal aging heat treatment at $630^{\circ}C$ by high frequency longitudinal wave method investigating the change of attenuation coefficient by FFT analysis and wavelet transform. Because of carbide precipitation increase and spheroidization near grain boundary of microstructure to aging degradation, attenuation coefficient had a tendency to increase as degradation proceeded. It was identified possibly to evaluate degradation using the characteristics of high-frequency ultrasonics. Frequency dependence of ultrasonic attenuation coefficient to aging degradation appeared large, which made sure that attenuation coefficient is an important parameter for evaluation of aging degradation.

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Microstructural analysis of sintered brick made of recycled wastes (폐기물을 재활용한 소성벽돌의 미세구조 분석)

  • 엄태호;김유택;이기강;강승구;김정환
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.13 no.4
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    • pp.199-204
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    • 2003
  • Microstructure and chemical analysis of sintered bricks containing recycled wastes were investigated by SEM and EDS. The recycled wastes for which substitute ceramic raw materials were EAF (electric arc furnace) dust, fly ash and stone ash. Yellowish and brownish regions on the surface and brownish and blackish regions in the inside of bricks were observed. Main component of yellowish region on the surface turned out to be Zn. No chemical difference between the black-core region and brownish matrix. Mullite crystallites of 1 fm size were distributed in the inside of bricks and enclosed by glass phases. It seems that alumine-silicate mixtures of kaolin and fly ash were transformed to mullite crystallites during the sintering. Relatively large pores ot several ten fm size were observed in the black-core region in the inside of bricks. The main components of the inside of brick were Al and Si. The minor components were C, Na, Mg, K, Ca, and Fe. Particularly, the precipitates of Fe-rich crystallites were observed in the amorphous matrix. These precipitates were formed due to the local reduction atmosphere in the inside of bricks. Zn-rich covers were found on the surface of bricks because Zn diffused from the inside of bricks to the surface under the reduction atmosphere.