• Title/Summary/Keyword: X-ray Structure Analysis

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Synthesis of YSZ Thin Films by PECVD (PECVD에 의한 YSZ(Yttria Stabilized Zirconia)박막 제조)

  • Kim, Gi-Dong;Sin, Dong-Geun;Jo, Yeong-A;Jeon, Jin-Seok;Choe, Dong-Su;Park, Jong-Jin
    • Korean Journal of Materials Research
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    • v.9 no.3
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    • pp.234-239
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    • 1999
  • A Abstract Yttria-stabilized zirconia(YSZ) thin films were synthesized by plasma enhanced chemical vapor deposition process. $Zr[TMHD]_4$ $Y[TMHD]_3$ precursors and oxygen were used with the deposition temperature of $425^{\circ}C$ and rf power ranging 0-100 watt. Effects of the deposition parameters were studied by X-ray diffraction and thickness anal­ysis. YSZ thin films have cubic crystal structure with (200) orientation. From the results of EDX analysis, the converte ed content of TEX>$Y_2O_3$ was determined to be 0-36%, and the film thickness was increased with bubbling temperature which is considered to be due to increasing TEX>$Y_2O_3$ flux. The depth profiles of Zr, Y and 0 appeared relatively $\infty$nstant through film thickness. Columnar grains of $1000~2000\AA$ grew vertical to the substrate surface for the case of Ar carri­er gas. In case of He carrier gas, the grain size was observed to be about $1000~2000\AA$. X-ray diffraction data showed the increase of lattice constant with TEX>$Y_2O_3$ content. It was that the presence of the cracks formed during film deposition, partially released the stress generated by the increase of lattice constant.

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Synthesis of ceria by combination of spray pyrolysis, postheat, and ball-milling and its characterization (분무열분해, 후소성 및 볼밀링을 조합한 방법을 이용한 세리아의 합성 및 특성연구)

  • Kim, Hyun-Ik;Kim, Sang Pil;Song, Jae-Kyung;Kim, Sang Hern
    • Journal of the Korean Applied Science and Technology
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    • v.35 no.4
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    • pp.1057-1072
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    • 2018
  • In this study, micro-sized $CeO_2$ particles were synthesized by spray pyrolysis, and EG(ethylene glycol) and CA(citric acid) as organic additives were added to obtain hollow and porous particle during spray pyrolysis, and characteristics of obtained ceria were investigated according to the amount of added organic additives. Spray pyrolysis, postheat and ball-milling were combined to give 6 paths. $CeO_2$ nano-sized particle was obtained by the path which has sequence of Spray Pyrolysis with 0.5 M of EG and CA${\rightarrow}$Post-heat${\rightarrow}$Ball-milling${\rightarrow}$Post-heat among 6 paths. The average particle size(24 nm with standard deviation of 3.8 nm) of $CeO_2$ nano-sized particle by TEM analysis is close to the primary particle size(20 nm) which was calculated by Debye-Scherrer equation. To investigate the morphological characteristics and structure of the synthesized nanoparticle powders, SEM(Scanning Electron Microscopy), XRD(X-Ray Diffractometer) and TEM(Transmission Electron Microscopy) were used.

Corrosion Behaviors of Dental Implant Alloy after Micro-sized Surface Modification in Electrolytes Containing Mn Ion

  • Kang, Jung-In;Son, Mee-Kyoung;Choe, Han-Cheol
    • Journal of Korean Dental Science
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    • v.11 no.2
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    • pp.71-81
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    • 2018
  • Purpose: The purpose of this study was to investigate the corrosion behaviors of dental implant alloy after microsized surface modification in electrolytes containing Mn ion. Materials and Methods: $Mn-TiO_2$ coatings were prepared on the Ti-6Al-4V alloy for dental implants using a plasma electrolytic oxidation (PEO) method carried out in electrolytes containing different concentrations of Mn, namely, 0%, 5%, and 20%. Potentiodynamic method was employed to examine the corrosion behaviors, and the alternatingcurrent (AC) impedance behaviors were examined in 0.9% NaCl solution at $36.5^{\circ}C{\pm}1.0^{\circ}C$ using a potentiostat and an electrochemical impedance spectroscope. The potentiodynamic test was performed with a scanning rate of $1.667mV\;s^{-1}$ from -1,500 to 2,000 mV. A frequency range of $10^{-1}$ to $10^5Hz$ was used for the electrochemical impedance spectroscopy (EIS) measurements. The amplitude of the AC signal was 10 mV, and 5 points per decade were used. The morphology and structure of the samples were examined using field-emission scanning electron microscopy and thin-film X-ray diffraction. The elemental analysis was performed using energy-dispersive X-ray spectroscopy. Result: The PEO-treated surface exhibited an irregular pore shape, and the pore size and number of the pores increased with an increase in the Mn concentration. For the PEO-treated surface, a higher corrosion current density ($I_{corr}$) and a lower corrosion potential ($E_{corr}$) was obtained as compared to that of the bulk surface. However, the current density in the passive regions ($I_{pass}$) was found to be more stable for the PEO-treated surface than that of the bulk surface. As the Mn concentration increased, the capacitance values of the outer porous layer and the barrier layer decreased, and the polarization resistance of the barrier layers increased. In the case of the Mn/Ca-P coatings, the corroded surface was found to be covered with corrosion products. Conclusion: It is confirmed that corrosion resistance and polarization resistance of PEO-treated alloy increased as Mn content increased, and PEO-treated surface showed lower current density in the passive region.

Effect of Low Temperature Heat Treatment on the Physical and Chemical Properties of Carbon Anode Materials and the Performance of Secondary Batteries (저온 열처리가 탄소 음극재의 물리·화학적 특성 및 이차전지 성능에 미치는 영향)

  • Whang, Tae Kyung;Kim, Ji Hong;Im, Ji Sun;Kang, Seok Chang
    • Applied Chemistry for Engineering
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    • v.32 no.1
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    • pp.83-90
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    • 2021
  • In this study, effects of the physical and chemical properties of low temperature heated carbon on electrochemical behavior as a secondary battery anode material were investigated. A heat treatment at 600 ℃ was performed for coking of petroleum based pitch, and the manufactured coke was heat treated with different heat temperatures at 700~1,500 ℃ to prepare low temperature heated anode materials. The physical and chemical properties of carbon anode materials were studied through nitrogen adsorption and desorption, X-ray diffraction (XRD), Raman spectroscopy, elemental analysis. Also the anode properties of low temperature heated carbon were considered through electrochemical properties such as capacity, initial Coulomb efficiency (ICE), rate capability, and cycle performance. The crystal structure of low temperature (≤ 1500 ℃) heated carbon was improved by increasing the crystal size and true density, while the specific surface area decreased. Electrochemical properties of the anode material were changed with respect to the physical and chemical properties of low temperature heated carbon. The capacity and cycle performance were most affected by H/C atomic ratio. Also, the ICE was influenced by the specific surface area, whereas the rate performance was most affected by true density.

Effect of Curing Solution and Pre-Rust Process on Rebar Corrosion in the Cement Composite (시멘트 복합체 내부 철근 부식에 양생 용액과 철근 사전 부식이 미치는 영향)

  • Du, Rujun;Jang, Indong;Lee, Hyerin;Yi, Chongku
    • Journal of the Korea institute for structural maintenance and inspection
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    • v.26 no.2
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    • pp.1-8
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    • 2022
  • The corrosion of reinforcement is the main reason for the performance degradation of concrete structures. The pre-rusted parts of rebar in concrete structures are vulnerable to the corrosion, especially if the structure is exposed to wet or chlorinated environments. In this study, effects of different curing solution on corrosion behavior of the pre-rusted rebars in the cement composites were investigated. HCl(3%) and CaCl2(10%) solution were utilized to accelerate the pre-rust of the rebar, and each pre-rust condition rebar including reference (RE) were placed in mortar cylinder. Three kinds of samples then were cured in CaCl2 (3%) solution and tap water respectively for 120 days. Electrochemical polarization and half-cell potential measurement were used to monitor the influence of curing water on the corrosion behavior of pre-rusted steel bar in cement composite. The surface morphology and composition of corroded steel bar were analyzed by scanning electron microscope and energy dispersive X-ray diffraction. The results show that the corrosion rates of pre-rusted samples in both curing water are higher than that of non-pre-rusted samples. The corrosion rates of RE, CaCl2 and HCl pre-rusted samples in salt water were 8.14, 4.48, 13.81 times higher than those in tap water respectively, on the 120th day.

Durability Evaluation of Cement Concrete Using Ferrosilicon Industrial Byproduct (페로실리콘 산업부산물 활용 시멘트 콘크리트의 내구성능 평가)

  • Chang-Young Kim;Ki Yong Ann
    • Journal of the Korean Recycled Construction Resources Institute
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    • v.11 no.1
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    • pp.89-96
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    • 2023
  • In this paper, a ferrosilicon by-product was evaluated to confirm the feasibility of recycling it as supplementary cementitious material of ordinary Portland cement in concrete. Three different levels of replacement ratio (10 %, 20 % and 30 % of total binder) were applied to find which is the most beneficial to be used as a binder. Ferrosilicon concrete was initially assessed at setting time and compressive strength. Durability was evaluated by the resistance to chloride penetration test(RCPT) and alkali-silica reaction(ASR) with a comparison to silica fume concrete due to their similarity in chemical composition. The porosimetry and X-ray diffraction analysis along with energy dispersive X-ray spectroscopy give information on the microstructural characteristics of the ferrosilicon concrete. It was found that 10 % ferrosilicon concrete has higher strength while 20 %, 30 % have lower strength than OPC concrete. However, chemical resistance to chloride attack is higher when replacement is increased. Compared to silica fume, the durability of ferrosilicon might be less efficient however, it is obviously beneficial than OPC. High SiO2 content in ferrosilicon results in producing more C-S-H gel which could make denser pore structure. Most of the risk of alkali silica reaction to silicate binders through length change tests was less than 0.2 %, and both mortar using ferrosilicon and silica fume showed better resistance to alkali silica reaction as the substitution rate increased.Reuse of industrial waste rather than producing highly refined additives might reduce environmental load during manufacture and save costs.

Characterization of TMA-A zeolite incorporated by ZnO nanocrystals (ZnO 나노결정을 담지한 TMA-A 제올라이트의 특성분석)

  • Lee, Seok Ju;Lim, Chang Sung;Kim, Ik Jin
    • Analytical Science and Technology
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    • v.21 no.1
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    • pp.58-63
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    • 2008
  • Nano-sized ZnO crystals were successfully incorporated using ion exchange method in TMA-A zeolite synthesized by the hydrothermal method. The optimal composition for the synthesis of TMA-A zeolite was resulted in a solution of $Al(i-pro)_3$ : 2.2 TEOS : 2.4 TMAOH : 0.3 NaOH : 200 $H_2O$. 0.3 g of TMA-A zeolite and 5 mol of $ZnCl_2$ solution were employed for the preparation of ZnO incorporated TMA-A zeolite. The crystallization process of ZnO incorporated TMA-A zeolite was analyzed by X-ray diffraction (XRD). The incorporated nano-sized ZnO crystals and the crystallinity of TMA-A zeolite were evaluated by transmission electron microscopy (TEM) and high resolution transmission electron microscopy (HRTEM). The size of the incorporated nano-sized ZnO crystals was 3~5 nm, while the TMA-A zeolite was 60~100 nm. The bonding structure and absorption of the ZnO incorporated TMA-A zeolite were compared with the ZnO and TMA-A zeolite by the FT-IR analysis. Subsequentlly, the ZnO incorporated TMA-A zeolite showed the photoluminescent characteristics on the wavelengths of 330~260 nm and 260~230 nm by measurement of UV spectrophotometer.

Study on Ti-doped LiNi0.6Co0.2Mn0.2O2 Cathode Materials for High Stability Lithium Ion Batteries (고안정성 리튬이온전지 양극활물질용 Ti 치환형 LiNi0.6Co0.2Mn0.2O2 연구)

  • Jeon, Young Hee;Lim, Soo A
    • Journal of the Korean Electrochemical Society
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    • v.24 no.4
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    • pp.120-132
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    • 2021
  • Although the development of high-Nickel is being actively carried out to solve the capacity limitation and the high price of raw cobalt due to the limitation of high voltage use of the existing LiCoO2, the deterioration of the battery characteristics due to the decrease in structural stability and increase of the Ni content. It is an important cause of delaying commercialization. Therefore, in order to increase the high stability of the Ni-rich ternary cathod material LiNi0.6Co0.2Mn0.2O2, precursor Ni0.6Co0.2Mn0.2-x(OH)2/xTiO2 was prepared using a nanosized TiO2 suspension type source for uniform Ti substitution in the precursor. It was mixed with Li2CO3, and after heating, the cathode active material LiNi0.6Co0.2Mn0.2-xTixO2 was synthesized, and the physical properties according to the Ti content were compared. Through FE-SEM and EDS mapping analysis, it was confirmed that a positive electrode active material having a uniform particle size was prepared through Ti-substituted spherical precursor and Particle Size Analyzer and internal density and strength were increased, XRD structure analysis and ICP-MS quantitative analysis confirmed that the capacity was effectively maintained even when the Ti-substituted positive electrode active material was manufactured and charging and discharging were continued at high temperature and high voltage.

Analysis Corrosion Products Formed on the Great Buddha Image of Kotokuin Temple in Kamakura (고덕원 국보 동조아미타여래좌상의 표면에 생성한 부식생성물의 해석)

  • Matsuda Shiro;Aoki Shigeo;Kang, Dai-il
    • 보존과학연구
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    • s.17
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    • pp.161-182
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    • 1996
  • In natural atmosphere, copper and copper alloy have been used to make buddha statues and ornaments of historic buildings since the abovementioned metals have corrosion resistance in some extent, and the patinaformed on the surface of the metals has provided the people aesthetic satisfaction with its beauty. But in atmosphere polluted by $SO_x$and $NO_x$, the patina layer does not work as a protective film, and it allows damages of the metal. Since 1992, Tokyo National Research Institute of Cultural Properties(TNRICP)has conducted studies on the influence of atmospheric pollution on metal cultural property held under open air. The Great Buddha Image which is located in Kamakura about 50km west from Tokyo, has been selected as one of the objects to study because it is made by copper alloy and it has stood exposed in the air for about a few hundreds years. Furthermore it is also the reason to study on it that there are many cultural properties in the surroundings of it. We have analysed the components and the structure of the corrosion products formed on the surface of the Buddha, have carried out exposure tests using the alloy samples which have simulated the components of the Great Image, and have observed climated and polluted air in order to discuss the relation between corrosion of metals in open air and conditions of the atmosphere. In this paper, the authors have described the components and the structure of the corrosion product formed on the surface of the Great Image by means of X-ray fluorescence spectroscopy and X-ray diffraction. The conclusions are as follows. (1) Sulfate patina composed mainly with brochantite were detected on the all sides of the Image and the amount of the patina is found more on the back of the Image facing to north. (2) Antlerite were detected on the back and a park of the left side facing to west, and formation of it was considered to have close relation with malignant atmosphere. (3) A big amount of chloride patina which mainly composed of atacamite were observed on the front facing to south. (4) Carbonate patina mainly composed of malachite were detected on the area where brochantite was often detected as well. It suggested that malachite had been transformed into brochantite by deteriorated atmosphere. (5) On the all sides of the Image, patina were observed together with copper oxides mainly composed of cuprous oxide. It showed that the surface layer of the Image consists of two layers : inner layer of oxide and outer layer of patina. (6) Corrosion products of lead which was a component of copperalloy were detected on the all sides : the main lead product found on the front was chlorophosphate whereas the one on the back was sulfate.

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Morphology and Chemical Composition Analysis of Human Cremated Ash by SEM/EDS (SEM/EDS를 이용한 화장 분골의 형태와 성분 분석)

  • Hwang, Kyu-Sung;An, Woo-Hwan;Kim, Jeong-Lae
    • The Journal of the Convergence on Culture Technology
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    • v.1 no.2
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    • pp.65-69
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    • 2015
  • Teeth and bones are very resistance to high temperatures and remain recognizable even after prolonged exposures to heat. The effects of heating and burning on teeth have been studied with the aim of discerning a characteristic signature withstanding high temperature, but there have been few studies about a human cremated ash, especially Korea. We are recognizable by elemental composition and can be detected in human cremated ash samples by Scanning electromicroscopy/Energy dispersive X-ray spectrometry analysis(SEM/EDS), cremated, at $800{\sim}900^{\circ}C$ for 1 hour. In this temperature range, different crystals morphologies(spherical, irregular and hexagonal) are observed in SEM. Calcium(Ca) and oxygen(O) increases steadily after cremation in EDS. We suggest that cremated bone have been provided with calcium oxide(CaO) formation at temperature above $900^{\circ}C$. This study offers basic data to assess the structure and elemental compositions of human ash and to determine if these remain identifiable after exposure to extreme temperatures.