• Title/Summary/Keyword: -energy-dispersive x-ray-

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A study on the Investigation and Removal the Cause of Blacken Effect of Waterlogged archaeological woods (수침고목재의 흑화 원인과 제거방법에 관하여)

  • Yang, Seok-jin
    • Korean Journal of Heritage: History & Science
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    • v.40
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    • pp.413-430
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    • 2007
  • This study analyzed the foreign substances in waterlogged archaeological woods and compounds in soil where waterlogged archaeological wood was buried, in order to examine the relationship between burial environment and foreign substances in waterlogged archaeological wood. The XRF(X-ray Fluorescence Spectroscopy) and EDX(Energy Dispersive X-ray) analysis were conducted to examine the effect of iron(Fe) to blacken the waterlogged wood. The XRF results showed that investigated soil contained Si, Al, and Fe. Wood ash contained more sulfur and Fe than any other elements in the EDX analysis. Cellulose and hemicellulose were significantly reduced at the surface of wood, which is the blackened part of waterlogged wood. Foreign substances changed the surface color. These problems could be solved by removal of foreign substances in waterlogged archaeological wood using EDTA(Ethylene Diamine Tetra Acetic acid). The optimum condition to remove Fe from waterlogged wood by EDTA was investigated. To do this, the concentration of Fe removed was measured with various concentration of EDTA-2Na. The optimum pH of EDTA-2Na was figured to be 4.1 to 4.3. As the concentration of EDTA increased, the extracted concentration of Fe also increased. In the case of 0.4 wt% of EDTA-2Na, about 60ppm of Fe was eliminated and was stabilized after 48 hours. In the case of EDTA-3Na, the optimum pH was 7 to 8, and about 10 ppm of Fe was eliminated at 0.4 wt% of EDTA-3Na. In the case of EDTA-4Na, the optimum pH was 10 to 11, and about 20 ppm of Fe was eliminated at 0.4 wt% of EDTA-4Na. In conclusion, the iron(Fe) in waterlogged archaeological wood was removed by EDTA treatment and it increased the whiteness of the surface.

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.

A Study on Material Characteristics and Manufacturing Techniques for Gold-granule Beads Excavated from the Neungsan-ri Temple Site in Buyeo (부여 능산리사지 출토 금제구슬의 재료학적 특성 및 제작기법 연구)

  • Yang, Soohyeon;Ro, Jihyun
    • Conservation Science in Museum
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    • v.26
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    • pp.67-82
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    • 2021
  • Two golden beads (Buyeo 5336) housed at the Buyeo National Museum were discovered in 1993 near the site of an ancient workshop in Neungsan-ri in Buyeo-gun, Chungcheongnam-do Province. These rare examples from the Baekje Kingdom of an application of granulation have maintained their original form intact, and thus serve as important materials for the investigation of production techniques applied. This study analyzed the composition of the golden beads using a portable X-ray fluorescence analyzer, a stereo microscope, and a scanning electron microscope with an energy dispersive X-ray spectrometer. The manufacturing technique was examined through the observation of the micro-shape and the surface condition and by a composition analysis of the joint part. In both beads, a hole was pierced in a hollow body and the bead was decorated with golden wires around the hole and gold granules in other parts. In some areas, golden granules had been attached to the gold plate and golden wires were then placed over the granules. The purity of both the wires and the granules was analyzed as 23.6 - 23.7K. A high copper content was detected in some of the parts where the granules were attached. The findings of a previous reproduction experiment and study of production methods suggest that the beads were made using the copper diffusion technique.

Mechanical behavior and microstructural characterization of different zirconia polycrystals in different thicknesses

  • Arcila, Laura Viviana Calvache;Ramos, Nathalia de Carvalho;Campos, Tiago Moreira Bastos;Dapieve, Kiara Serafini;Valandro, Luiz Felipe;de Melo, Renata Marques;Bottino, Marco Antonio
    • The Journal of Advanced Prosthodontics
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    • v.13 no.6
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    • pp.385-395
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    • 2021
  • PURPOSE. To characterize the microstructure of three yttria partially stabilized zirconia ceramics and to compare their hardness, indentation fracture resistance (IFR), biaxial flexural strength (BFS), and fatigue flexural strength. MATERIALS AND METHODS. Disc-shaped specimens were obtained from 3Y-TZP (Vita YZ HT), 4Y-PSZ (Vita YZ ST) and 5Y-PSZ (Vita YZ XT), following the ISO 6872/2015 guidelines for BFS testing (final dimensions of 12 mm in diameter, 0.7 and 1.2 ± 0.1 mm in thicknesses). Energy-dispersive X-ray spectroscopy (EDX), X-ray diffraction (XRD) and scanning electron microscopy (SEM) analyses were performed, and mechanical properties were assessed by Vickers hardness, IFR, quasi-static BFS and fatigue tests. RESULTS. All ceramics showed similar chemical compositions, but mainly differed in the amount of yttria, which was higher as the amount of cubic phase in the diffractogram (5Y-PSZ > 4Y-PSZ > 3Y-TZP). The 4Y- and 5Y-PSZ specimens showed surface defects under SEM, while 3Y-TZP exhibited greater grain uniformity on the surface. 5Y-PSZ and 3Y-TZP presented the highest hardness values, while 3Y-TZP was higher than 4Y- and 5Y-PSZ with regard to the IFR. The 5Y-PSZ specimen (0.7 and 1.2 mm) showed the worst mechanical performance (fatigue BFS and cycles until failure), while 3Y-TZP and 4Y-PSZ presented statistically similar values, higher than 5Y-PSZ for both thicknesses (0.7 and 1.2 mm). Moreover, 3Y-TZP showed the highest (1.2 mm group) and the lowest (0.7 mm group) degradation percentage, and 5Y-PSZ had higher strength degradation than 4Y-PSZ group. CONCLUSION. Despite the microstructural differences, 4Y-PSZ and 3Y-TZP had similar fatigue behavior regardless of thickness. 5Y-PSZ had the lowest mechanical performance.

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.

Identification of the Materials of the Decorative Pieces Excavated from Geumnyeongchong Tomb (금령총 출토 장식편 재질 규명)

  • Lee Gyuhye;Shin Seungchul;Gwak Hongin;Yang Seokjin
    • Conservation Science in Museum
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    • v.30
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    • pp.89-100
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    • 2023
  • Museum collections are comprised of a variety of materials, and different scientific examinations are being conducted according to the types and production properties of the materials, but insufficient research has been carried out on ultra-small artifacts. To identify the material characteristics of the white ultra-small materials excavated from Geumnyeongchong tomb, this study carried out a wide range of non-destructive analyses (specific gravity, microscopy, nano-computed tomography (Nano-CT), scanning electron microscopy-energy dispersive X-ray spectroscopy (SEM-EDS), X-ray diffraction (XRD), and Raman spectroscopy) and compared the said artifacts with the Goryeo-era burial accessories examined in prior research. Non-destructive analysis confirmed the presence of aragonite, which mainly consists of calcium carbonate (CaCO3) as the constituent mineral, and identified the material used for the ornaments as the gemstone pearl based on its growth lines. This study concludes that pearls began to be used in the ancient Korean Peninsula in the 6th century. It is expected that scientific examinations of the white ultra-small artifacts will yield information about the social culture of the time.

Decomposition Behavior of Secondary Solidification Phase During Heat Treatment of Squeeze Cast Al-Cu-Si-Mg (용탕단조 Al-Cu-Si-Mg합금의 열처리시 제2응고상의 분해거동)

  • Kim, Yu-Chan;Kim, Do-Hyang;Han, Yo-Sub;Lee, Ho-In
    • Journal of Korea Foundry Society
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    • v.17 no.6
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    • pp.560-568
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    • 1997
  • The dissolution behavior of secondary solidification phases in squeeze cast Al-3.9wt%Cu-1.5wt%Si-1.0wt%Mg has been studied using a combination of optical microscope, image analyzer, scanning electron microscope(SEM), energy dispersive spectrometer(EDS), X-ray diffractometer(XRD) and differential thermal analyzer (DTA). Special emphasis was placed on the investigation of the effects of the nonequilibrium heat treatment on the dissolution of the second solidification phases. Ascast microstructure consisted of primary solidification product of ${\alpha}-Al$ and secondary solidification products of $Al_2Cu$, $Mg_2Si$ and $Al_2CuMg$. Equilibrium and non-equilibrium solution treatments were carried out at the temperatures of $495^{\circ}C$, $502^{\circ}C$ and $515^{\circ}C$ for 3 to 5 hours. The amount of the dissolved secondary phases increased with increasing solution treatment temperature, for example, area fractions of $Al_2Cu$, $Mg_2Si$ and $Al_2CuMg$ were approximately 0%, 1.6% and 4.2% after solution treatment at $495^{\circ}C$ for 5hours, and were approximately 0%, 0.36% and 2% after solution treatment at $515^{\circ}C$ for 5hours. The best combination of tensile properties was obtained when the as-cast alloy was solution treated at $515^{\circ}C$ for 3hours followed by aging at $180^{\circ}C$ for 10 hours. Detailed DTA and TEM study showed that the strengthening behavior during aging was due to enhanced precipitation of the platelet type fine ${\theta}'$ phase.

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Production of Porous Metallic Glass Granule by Optimizing Chemical Processing

  • Kim, Song-Yi;Guem, Bo-Kyung;Lee, Min-Ha;Kim, Taek-Soo;Eckert, Jurgen;Kim, Bum-Sung
    • Journal of Powder Materials
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    • v.21 no.4
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    • pp.251-255
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    • 2014
  • In this study, we optimized dissolution the dissolution conditions of porous amorphous powder to have high specific surface area. Porous metallic glass(MG) granules were fabricated by selective phase dissolution, in which brass is removed from a composite powder consisting of MG and 40 vol.% brass. Dissolution was achieved through various concentrations of $H_2SO_4$ and $HNO_3$, with $HNO_3$ proving to have the faster reaction kinetics. Porous powders were analyzed by differential scanning calorimetry to observe crystallization behavior. The Microstructure of milled powder and dissolved powder was analyzed by scanning electron microscope. To check for residual in the dissolved powder after dissolution, energy dispersive X-ray spectroscory and elemental mapping was conducted. It was confirmed that the MG/brass composite powder dissolved in 10% $HNO_3$ produced a porous MG granule with a relatively high specific surface area of $19.60m^2/g$. This proved to be the optimum dissolution condition in which both a porous internal granule structure and amorphous phase were maintained. Consequently, porous MG granules were effectively fabricated and applications of such structures can be expanded.

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.