• Title/Summary/Keyword: microstructure, SEM-EDS

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Magnetic Susceptibility depending on the Thermal Degradation of HK-40 Steel (HK-40강의 열화도에 따른 자화율의 변화)

  • Kim, Jeong-Min;Son, De-Rac;Park, Jong-Seo;Nahm, Seung-Hoon;Kim, Dong-Gyun;Han, Sang-In;Choi, Song-Chun;Ryu, Dae-Hyun
    • Journal of the Korean Society for Nondestructive Testing
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    • v.24 no.1
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    • pp.22-28
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    • 2004
  • Since the used materials of furnace heater tube with different kinds of thermal degradation were not commonly available, the HK-40 steel specimens were heat-treated isothermally at elevated temperature to simulate the microstructure at the service temperature. HK-40 steel specimens with five different aging time were prepared by isothermal heat treatment at $1050^{\circ}C$. The characteristics of the magnetic susceptibility have been investigated for the degradation evaluation of HK-40 steel. The magnetic susceptibility at room temperature increases as the extent of degradation of the materials increases. The variation of magnetic susceptibility was compared with the variation of tensile properties and Vickers hardness. To investigate the effect of the microsturctural change on the characteristics of tensile properties, hardness and magnetic susceptibility, the microstructures were examined by a scanning electron microscope(SEM) and the chemical compositions were analyzed by a energy spectrometer of SEM. As a result, the magnetic susceptibility method can be suggested as one of the nondestructive evaluation methods for the degradation of the HK-40 steel.

Manufacturing Techniques of Bronze Seated Bodhisattva Statue of Goseongsa Temple in Gangjin (강진 고성사 청동보살좌상의 제작기술 연구)

  • LEE Seungchan;BAE Gowoon;CHUNG Kwangyong
    • Korean Journal of Heritage: History & Science
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    • v.57 no.1
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    • pp.146-159
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    • 2024
  • In this study, a study on the production technology of the Buddha statue and the production of raw material origin was conducted through scientific analysis on the Bronze seated Bodhisattva Statue of Goseongsa Temple, a treasure. As a result of microstructure analysis through a metal microscope, it was confirmed that the microstructure of the Bronze seated Bodhisattva Statue of Goseongsa Temple was a process-type dendritic structure, and the casting structure of bronze was well represented, so it was manufactured through casting. Subsequently, as a result of analyzing the alloy composition ratio through SEM-EDS, it was identified as a ternary alloy with 81.26 wt% of copper (Cu) and 16.42 wt% of tin (Sn) and 1.72 wt% of lead (Pb). The results of the analysis of lead isotope ratios using a thermal ionization mass spectrometer (TIMS) were substituted into the distribution of lead isotope ratios on the Korean Peninsula, it was shown in corresponding to Jeolla-do and Chungcheong-do regions and North and South Gyeongsang Province. This suggests that the raw materials used in their production were likely sourced from the mines around Goseong Temple in Gangjin. Despite the fact that the statue is a medium and large Buddha with a total height of 51 centimeters, 1.72 wt% of lead (Pb) was found as a result of alloy composition ratio analysis, which showed a similar composition to the lead content ratio of small bronze and gilt-bronze Buddha statues. Therefore, we compared and analyzed the results of the analysis of the composition ratio of the alloys of bronze and gilt bronze statues, which has been scientifically analyzed with a compositional age similar to that of the Bronze seated Bodhisattva Statue of Goseongsa Temple. Comparison results, Various factors, such as the size of the Buddha statue as well as its stylistic characteristics and the age of composition, may exist in determining the alloy composition ratio of the bronze and gilt bronze Buddha statues, and it was confirmed that the alloy composition ratio or casting technology was properly adjusted when the Buddha statue was created. In other words, it is judged that a more comprehensive system of Buddha statue production technology should be investigated by conducting archaeological and art history studies on stylistic characteristics and age of composition, as well as scientific analysis results such as observation of internal structure, microstructure observation, and analysis of alloy composition ratio using radiation transmission irradiation.

The Study on Material Characteristics of Slags Excavated from Iron Making Site (제철 유적 출토 철재(鐵滓)의 재료학적 특성 연구)

  • Kang, Yoon-Hee;Cho, Nam-Chul;Song, Hyeon-Jeong;Go, Hyeong-Sun
    • Journal of Conservation Science
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    • v.26 no.2
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    • pp.171-182
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    • 2010
  • The slag excavated from Gyesil-ri in Gongju, Yeonje-ri in Cheongwon and Beopcheonsaji (temple) site in Wonju are analyzed by X-ray Fluorescence Analyzer, metallurgical microscope, SEM-EDS etc., for chemical composition and microstructure to figure out the raw material and the iron manufacturing technique. First of all, as a result of principal component analysis, the total Fe-content of slag from Gyesil-ri is 39 to 44% and the modified rate is 15 to 21%, which is common in ancient iron slag. Yeonje-ri site is found the ancient iron-smelting furnace. The total Fe-content of slag from Yeonje-ri is 41 to 43% and modified rate is 18~30%, which is also the general value in the ancient slag. However only slag is excavated in the residential area at Beopcheonsaji site and there is no iron making relic. In addition, the result of principal component analysis contains that the total Fe-content of Beopcheonsaji site is 52 to 57%, and modified rate is 8 to 14%. It shows that the total Fe-content of Beopcheonsaji site is higher than relic from Gyesil-ri and Yeonje-ri and the modified rate is lower than other sites. This results mean that recollecting rate of Fe in Beopcheonsaji site is lower than other sites. Also, as a result of minor elements analysis, the slag from Gyesil-ri has the higher level of Ti, V and Zr than other sites and the microstructure are observed as magnetite and ulvospinel, so that the raw material of slag is iron sand. But the slag from Yeonje-ri and Beopcheonsaji site are identified to use iron ore. As a result of microstructure observation, fayalite, gray-columnar crystal, is found in the slag from Yeonje-ri and big wustite as main phase is observed in the slag from Beopcheonsaji site. This study show that the slag from Yeonje-ri is made of smelt ash produced during smelting works and the slag from Beopcheonsaji site is made of forging ash produced during forging work concerning the excavated location and the microstructure.

A Study of the Material Properties of Steel Used to Repair the Stupa of State Preceptor Jigwang from Beopcheonsa Temple, Wonju in 1957 (1957년 원주 법천사지 지광국사탑 수리에 사용된 철물(鐵物)의 재료학적 특성 연구)

  • You, Harim;Lee, Jaesung;Lee, Taejong;Park, Heejeoung
    • Korean Journal of Heritage: History & Science
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    • v.53 no.4
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    • pp.100-117
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    • 2020
  • National Treasure no. 101, the stupa of State Preceptor Jigwang from the Beopcheonsa Temple Site in Wonju has been transferred from place to place and reassembled several times since it was built. In particular, overall dismantling and repair was carried out in 1957 to restore parts damaged by bombing during the Korean War. Documented information on the repair process and materials used at that time does not exist. However, various types of metal materials used for this stupa have been identified during conservation work. Besides clamps anchor bolts, 9mm-thick circular rebars were mainly used for joining the parts of this stupa, while circular rebars and wires of various thicknesses were used for joining the parts with mortar restoration materials. Although deformed bars are typically used for stone pagodas classified as architectural structures, smooth circular rebars were used in this case. In terms of restoration using mortar, material shapes were transformed, bound alternately, and twisted irregularly to improve bonding strength and coherence in order to insert restoration materials and to bolster structural weaknesses. In addition, metallographic analysis showed the material to be hypo-eutectoid steel with low carbon content. Many non-metallic inclusions in the shape of drops of different sizes were included, which do not affect the whole elemental composition due to the very small quantities involved. Qualitative and EPMA analysis of Mn and S, which were not identified by SEM-EDS area analysis, established an even distribution of MnS in crystal grains of the microstructure, regardless of the shape of the samples. It is presumed that secondary homogenization and softening might have been conducted after manufacturing to facilitate the working process. Furthermore, in consideration of properties indicating that the thinner the steel is, the less carbon content contained and the greater the elasticity and elongation, it is judged that restoration work was ordered.

Si and Mg doped Hydroxyapatite Film Formation by Plasma Electrolytic Oxidation

  • Park, Seon-Yeong;Choe, Han-Cheol
    • Proceedings of the Korean Institute of Surface Engineering Conference
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    • 2016.11a
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    • pp.195-195
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    • 2016
  • Titanium and its alloys are widely used as implants in orthopedics, dentistry and cardiology due to their outstanding properties, such as high strength, high level of hemocompatibility and enhanced biocompatibility. Hence, recent works showed that the synthesis of new Ti-based alloys for implant application involves more biocompatible metallic alloying element, such as, Nb, Hf, Zr and Mo. In particular, Nb and Hf are one of the most effective Ti ${\beta}-stabilizer$ and reducing the elastic modulus. Plasma electrolyte oxidation (PEO) is known as excellent method in the biocompatibility of biomaterial due to quickly coating time and controlled coating condition. The anodized oxide layer and diameter modulation of Ti alloys can be obtained function of improvement of cell adhesion. Silicon (Si) and magnesium (Mg) has a beneficial effect on bone. Si in particular has been found to be essential for normal bone and cartilage growth and development. In vitro studies have shown that Mg plays very important roles in essential for normal growth and metabolism of skeletal tissue in vertebrates and can be detected as minor constituents in teeth and bone. The aim of this study is to research Si and Mg doped hydroxyapatite film formation by plasma electrolytic oxidation. Ti-29Nb-xHf (x= 0, 3, 7 and 15wt%, mass fraction) alloys were prepared Ti-29Nb-xHf alloys of containing Hf up from 0 wt% to 15 wt% were melted by using a vacuum furnace. Ti-29Nb-xHf alloys were homogenized for 2 hr at $1050^{\circ}C$. Each alloy was anodized in solution containing typically 0.15 M calcium acetate monohydrate + 0.02 M calcium glycerophosphate at room temperature. A direct current power source was used for the process of anodization. Anodized alloys was prepared using 270V~300V anodization voltage at room. A Si and Mg coating was produced by RF-magnetron sputtering system. RF power of 100W was applied to the target for 1h at room temperature. The microstructure, phase and composition of Si and Mg coated oxide surface of Ti-29Nb-xHf alloys were examined by FE-SEM, EDS, and XRD.

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Morphology of RF-sputtered Mn-Coatings for Ti-29Nb-xHf Alloys after Micro-Pore Form by PEO

  • Park, Min-Gyu;Park, Seon-Yeong;Choe, Han-Cheol
    • Proceedings of the Korean Institute of Surface Engineering Conference
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    • 2016.11a
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    • pp.197-197
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    • 2016
  • Commercially pure titanium (CP Ti) and Ti-6Al-4V alloys have been widely used for biomedical applications. However, the use of the Ti-6Al-4V alloy in biomaterial is then a subject of controversy because aluminum ions and vanadium oxide have potential detrimental influence on the human body due to vanadium and aluminum. Hence, recent works showed that the synthesis of new Ti-based alloys for implant application involves more biocompatible metallic alloying element, such as, Nb, Hf, Zr and Mo. In particular, Nb and Hf are one of the most effective Ti ${\beta}-stabilizer$ and reducing the elastic modulus. Plasma electrolyte oxidation (PEO) is known as excellent method in the biocompatibility of biomaterial due to quickly coating time and controlled coating condition. The anodized oxide layer and diameter modulation of Ti alloys can be obtained function of improvement of cell adhesion. Manganese(Mn) plays very important roles in essential for normal growth and metabolism of skeletal tissue in vertebrates and can be detected as minor constituents in teeth and bone. Radio frequency(RF) magnetron sputtering in the various PVD methods has high deposition rates, high-purity films, extremely high adhesion of films, and excellent uniform layers for depositing a wide range of materials, including metals, alloys and ceramics like a hydroxyapatite. The aim of this study is to research the Mn coatings on the micro-pore formed Ti-29Nb-xHf alloys by RF-magnetron sputtering for dental applications. Ti-29Nb-xHf (x= 0, 3, 7 and 15wt%, mass fraction) alloys were prepared Ti-29Nb-xHf alloys of containing Hf up from 0 wt% to 15 wt% were melted by using a vacuum furnace. Ti-29Nb-xHf alloys were homogenized for 2 hr at $1050^{\circ}C$. Each alloy was anodized in solution containing typically 0.15 M calcium acetate monohydrate + 0.02 M calcium glycerophosphate at room temperature. A direct current power source was used for the process of anodization. Anodized alloys was prepared using 270V~300V anodization voltage at room. Mn coatings was produced by RF-magnetron sputtering system. RF power of 100W was applied to the target for 1h at room temperature. The microstructure, phase and composition of Mn coated oxide surface of Ti-29Nb-xHf alloys were examined by FE-SEM, EDS, and XRD.

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Investigation of physicochemical properties, sustainability and environmental evaluation of metakaolin- granulated blast furnace slag geopolymer concrete

  • Anas Driouich;Safae El Alami El Hassani;Zakia Zmirli;Slimane El Harfaoui;Nadhim Hamah Sor;Ayoub Aziz;Jong Wan Hu;Haytham F. Isleem;Hadee Mohammed Najm;Hassan Chaair
    • Computers and Concrete
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    • v.34 no.4
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    • pp.489-501
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    • 2024
  • Geopolymers are part of a class of materials characterized by properties combining polymers, ceramics, and cement. These include exceptionally high thermal and chemical stability, excellent mechanical strength and durability in aggressive environments. This work deals with the synthesis, characterization, and sustainability evaluation of GPGBFS-MK geopolymers by alkaline activation of a granulated blast furnace slag-metakaolin mixture. In the first step, elemental and oxide analyses by XRF and EDS showed that the main constituents of GPGBFS-MK geopolymers are silicon, sodium, and aluminium oxides. The structural analyses by XRD and FTIR confirmed that the geopolymerization for GPGBFS-MK geopolymers did occur, accompanied by the formation of disordered networks from the blends and a modification to the microstructure by the geopolymerization process. Similarly, the microstructural study made by SEM showed that the GPGBFS-MK geopolymers are constituted by aluminosilicates in the form of dense clusters on which are adsorbed particles of unreacted GBFS in the form of spheroids and white residues of the alkaline activating solution. In addition, the study of the sustainability evaluation of GPGBFS-MK geopolymers showed that the water absorption of geopolymeric materials is lower than that of OPC cement. As for the elevated temperature resistance, the analyses indicated an excellent elevated temperature resistance of GPGBFS-MK. In the same way, the study of the resistance to chemical aggressions showed that the GPGBFS-MK geopolymeric materials are unattackable, contrary to the OPC cement-based materials which are strongly altered.

Research of Diffusion Bonding of Tungsten/Copper and Their Properties under High Heat Flux

  • Li, Jun;Yang, Jianfeng
    • Proceedings of the Materials Research Society of Korea Conference
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    • 2011.05a
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    • pp.14-14
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    • 2011
  • W (tungsten)-alloys will be the most promising plasma facing armor materials in highly loaded plasma interactive components of the next step fusion reactors due to its high melting point, high sputtering resistance and low deuterium/tritium retention. The bonding technology of tungsten to Cu alloy was one of the key issues. In this paper, W/CuCrZr diffusion bonding has been performed successfully by inserting pure metal interlay. The joint microstructure, interfacial elements migration and phase composition were analyzed by SEM, EDS, XRD, and the joint shear strength and micro-hardness were investigated. The mock-ups were fabricated successfully with diffusion bonding and the cladding technology respectively, and the high heat flux test and thermal fatigue test were carried out under actively cooling condition. When Ni foil was used for the bonding of tungsten to CuCrZr, two reaction layers, Ni4W and Ni(W) layer, appeared between the tungsten and Ni interlayer with the optimized condition. Even though Ni4W is hard and brittle, and the strength of the joint was oppositely increased (217 MPa) due primarily to extremely small thicknesses (2~3 ${\mu}m$). When Ti foil was selected as the interlayer, the Ti foil diffused quickly with Cu and was transformed into liquid phase at $1,000^{\circ}C$. Almost all of the liquid was extruded out of the interface zone under bonding pressure, and an extremely thin residual layer (1~2 ${\mu}m$) of the liquid phase was retained between the tungsten and CuCrZr, which shear strength exceeded 160 MPa. When Ni/Ti/Ni multiple interlayers were used for bonding of tungsten to CuCrZr, a large number of intermetallic compound ($Ni_4W/NiTi_2/NiTi/Ni_3T$) were formed for the interdiffusion among W, Ni and Ti. Therefore, the shear strength of the joint was low and just about 85 MPa. The residual stresses in the clad samples with flat, arc, rectangle and trapezoid interface were estimated by Finite Element Analysis. The simulation results show that the flat clad sample was subjected maximum residual stress at the edge of the interface, which could be cracked at the edge and propagated along the interface. As for the rectangle and trapezoid interface, the residual stresses of the interface were lower than that of the flat interface, and the interface of the arc clad sample have lowest residual stress and all of the residual stress with arc interface were divided into different grooved zones, so the probabilities of cracking and propagation were lower than other interfaces. The residual stresses of the mock-ups under high heat flux of 10 $MW/m^2$ were estimated by Finite Element Analysis. The tungsten of the flat interfaces was subjected to tensile stresses (positive $S_x$), and the CuCrZr was subjected to compressive stresses (negative $S_x$). If the interface have a little microcrack, the tungsten of joint was more liable to propagate than the CuCrZr due to the brittle of the tungsten. However, when the flat interface was substituted by arc interfaces, the periodical residual stresses in the joining region were either released or formed a stress field prohibiting the growth or nucleation of the interfacial cracks. Thermal fatigue tests were performed on the mock-ups of flat and arc interface under the heat flux of 10 $MW/m^2$ with the cooling water velocity of 10 m/s. After thermal cycle experiments, a large number of microcracks appeared at the tungsten substrate due to large radial tensile stress on the flat mock-up. The defects would largely affect the heat transfer capability and the structure reliability of the mock-up. As for the arc mock-up, even though some microcracks were found at the interface of the regions, all microcracks with arc interface were divided into different arc-grooved zones, so the propagation of microcracks is difficult.

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