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

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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.

Impedance Spectroscopy Analysis of the Screen Printed Thick Films (스크린 프린트된 후막의 Impedance Spectroscopy 특성 분석)

  • Ham, Yong-Su;Moon, Sang-Ho;Nam, Song-Min;Lee, Young-Hie;Koh, Jung-Hyuk;Jyoung, Soon-Jong;Kim, Min-Soo;Cho, Kyung-Ho
    • Journal of the Korean Institute of Electrical and Electronic Material Engineers
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    • v.23 no.6
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    • pp.477-480
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    • 2010
  • In this study, we fabricate 3 wt% $Li_2CO_3$ doped $(Ba,Sr)TiO_3$ thick films on the Ag/Pd bottom electrode printed $Al_2O_3$ substrates for the LTCCs (low temperature co-fired ceramics) applications. From the X-ray diffraction analysis, 3 wt% $Li_2CO_3$ doped BST thick films on the Ag/Pd printed $Al_2O_3$ substrates, which sintered at $900^{\circ}C$, showed perovskite structure without any pyro phase. The dielectric properties of 3 wt% $Li_2CO_3$ doped BST thick films are measured from 1 kHz to 1 MHz. To investigate the electrical properties of 3 wt% $Li_2CO_3$ doped BST thick films, we employ the impedance spectroscopy. The complex impedance of 3 wt% $Li_2CO_3$ doped BST thick films are measured from 20 Hz to 1 MHz at the various temperatures.

Influence of Alumina on Hydrothermal Synthesis of 11Å Tobermorite (알루미나가 11Å Tobermorite의 수열합성에 미치는 영향)

  • Yim Going;Yim Chai Suk
    • Korean Journal of Materials Research
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    • v.15 no.2
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    • pp.97-105
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    • 2005
  • [ $11\AA$ ] tobermorite$(5CaO{\cdot}6SiO_2{\cdot}5H_2O)$ is synthesized from the mixtures of calcium hydroride and quartz using alumina in a molar ratio $Ca(OH)_2/SiO_2$ of 0.8 at $180^{\circ}C$ for 8 and 24 hrs under saturated steam pressure. The influence of alumina on the formation of $11\AA$ tobermorite was investigated by X-ray diffraction, differential thermal analysis and infrared spectroscopy. $11\AA$ tobermorite containing increasingly larger amounts of aluminum showed a shift of the basal spacing from 11.3 to $11.6\AA$. In general, there was a direct linear relation between the basal spacing and added content of alumina. The differential thermal analysis curves showed that $11\AA$ tobermorite with increasing alumina contents exhibited the exothermic peak at high temperature, namely $11\AA$ tobermorite containing aluminum gave a sharp exothermic peak at temperature around $850\~860^{\circ}C$ in the case of $S_3\~S_5$. The absorption band at $1607\~1620cm^{-1}$ is attributed to the bending vibration of water, and the position of the main O-H stretching and Si-O lattice vibration of $11\AA$ tobermorite at 3500 and $965cm^{-1}$ respectively is not altered. Consequently the existence of alumina accelerates the crystallization of $11\AA$ tobermorite, and that the aluminum ion appears to substitute for the silicon ion in $11\AA$ tobermorite structure. Al-containing tobermorite is distinguished from Al-free tobermorite.

Cr(III)-Tetraaza Macrocyclic Complexes Containing Auxiliary Ligands (Part II); Synthesis and Characterization of Cr(III)-Citrato Macrocyclic Complex

  • Byun, Jong-Chul;Park, Yu-Chul;Youn, Jeung-Su;Han, Chung-Hun;Lee, Nam-Ho
    • Bulletin of the Korean Chemical Society
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    • v.26 no.4
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    • pp.634-640
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    • 2005
  • The reaction of cis-[Cr([14]-decane)(OH$_2)_2]^+$ ([14]-decane = rac-5,5,7,12,12,14-hexamethyl-1,4,8,11-teraazacyclotetradecane) with auxiliary ligands {$L_a$ = citrate(cit)} leads to a new dimeric complex cis-[{Cr([14]-decane)($\mu$-cit)}$_2](ClO_4)_2$. This binuclear complex has been structurally characterized by a combination of elemental analysis, conductivity, IR and Vis spectroscopy, mass spectrometry, and X-ray crystallography. Analysis of the crystal structure of cis-[{Cr([14]-decane)($\mu$-cit)})($_2]^+$ reveals that each chromium has a distorted octahedral coordination environment and citrato ligands are monodentate to the two chromium atoms via the carboxyl groups. For dimeric complex the bridging geometry is as follows: Cr$\ldots$Cr = 7.361 $\AA$; Cr-O(average) = 1.958 (8) $\AA$; Cr-N range = 2.108 (9)-2.147(9) $\AA$; N(1)-Cr-N(3) (equatorial position) = 98.0(4)$^{\circ}$; N(2)-Cr-N(4) (axial position) = 166.4(4)$^{\circ}$; O(1)-Cr-N(2) = 98.1(4)$^{\circ}$; O(3)-Cr-N(4) = 96.6(3)$^{\circ}$; O(1)-Cr-O(3) = 90.4$^{\circ}$. The FAB mass spectrum of the dimeric complex displays peak due to the molecular ions cis-[{Cr([14]-decane)($\mu$-cit)})($_2]^+$ at m/z 1053.

Surface Transition by Solvent Washing Effects and Biological Properties of Metal Treated Activated Carbons

  • Oh, Won-Chun
    • Bulletin of the Korean Chemical Society
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    • v.25 no.5
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    • pp.639-646
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    • 2004
  • Metal treated activated carbons are prepared using various metals. Adsorption behaviors, morphologies, as well as antibacterial effects of metal treated samples are compared before and after solvent washing. Adsorption isotherms are used to characterize the porous structure of metal treated activated carbons before and after the solvent washing with acetone or ethyl alcohol. From these data, it is noticed that the changes in physicochemical properties of metal treated activated carbons depend on the solvents employed. Similar results are observed from BET data obtained from nitrogen adsorption isotherms. From scanning electron microscopy (SEM) studies, the changes in shape and size of metal particles are observed after the samples are washed with solvents. These changes result in different blocking effects, which, in turn, affect the adsorption behavior of metal treated activated carbons. X-ray diffraction (XRD) patterns of the samples treated with different metals are different each other. High intense sharp peaks attributed to metals are observed from silver treated samples, while the peaks are not observed from copper treated samples. To compare thermodynamic behavior of metal treated activated carbons washed with different type of solvents, differential scanning calorimetric (DSC) analysis is carried out. The analysis shows similar endothermic curves for all of the samples. Finally, antibacterial effects of metal treated activated carbon against Escherichia coli are discussed. Comparing the effects among the metals employed, highest effects are obtained from Cd, while lowest effects are obtained from Cu. Antibacterial activity becomes higher with the increase of the amount of metals treated, Optimum concentrations of metals to treat activated carbons, obtained from a shake flask test, are known to be 0.4, 0.1, and 0.6 moles for Ag, Cd, and Cu, respectively.

Influence of Preparation Conditions on the Formation of Copper (II) Architectures with Pyrazine-2,3,5-tricarboxylic Acid

  • Wang, Feng-Qin;Lin, Shu;Guo, Ming-Lin;Xu, Jun-Jian;Wang, Xiao-Qing;Zhao, Yong-Nan
    • Bulletin of the Korean Chemical Society
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    • v.32 no.7
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    • pp.2351-2357
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    • 2011
  • Three new metal-organic copper(II) complexes, $[Cu(H_2PZTC)_2]_n{\cdot}2nH_2O$ (1), $[Cu(HPZTC){\cdot}2H_2O]_n{\cdot}2nH_2O$ (2), and $Cu_2[(PZHD)(OH)(H_2O)_2]_n$ (3) ($H_3PZTC$ = pyrazine-2,3,5-tricarboxylic acid, $PZHD^{3-}$ = 2-hydroxypyrazine-3,5-dicarboxylate), have been synthesized from $Cu(II)/H_3PZTC$ system under different synthetic conditions, and characterized by single-crystal X-ray diffraction, elemental analysis, IR spectroscopy and thermogravimetric analysis. In complexes 1 and 2, $H_3PZTC$ ligands loose one and two protons, which were transformed into $H_2PZTC^-$ anion and $HPZTC^{2-}$ dianion under different preparation condition, respectively. Furthermore, two ligands coordinate with Cu(II) cations in different modes, leading to the formation of the different chain structures. In complex 3, $H_3PZTC$ ligand was converted into a new ligand-PZHD by in situ decarboxylation and hydroxylation under a higher pH value than that for complexes 1 and 2. PZHD ligands link the Cu(II) cations to form a 2D layer structure. These results demonstrate that the preparation conditions, including pH value and reaction temperature etc, play an important role in the construction of complexes based on $H_3PZTC$ ligand.

Preparation and Thermal Performance of Fullerene-Based Lead Salt

  • Guan, Hui-Juan;Peng, Ru-Fang;Jin, Bo;Liang, Hua;Zhao, Feng-Qi;Bu, Xing-Bing;Han, Wen-Jing;Chu, Shi-Jin
    • Bulletin of the Korean Chemical Society
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    • v.35 no.8
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    • pp.2257-2262
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    • 2014
  • $C_{60}$ is widely investigated because of its unique structure. But its applications in solid propellant seem to be relatively neglected. $C_{60}$ has more outstanding features than carbon black which is widely used as a catalyst ingredient of solid propellant. To combine the advantages of fullerene and lead salts, another good composite in propellant catalysts, we synthesized a kind of fullerene phenylalanine lead salt (FPL) and explored its thermal performances by differential thermal analysis (DTA) and thermogravimetry analysis (TGA). The results show it undergoes four exothermic processes started from 408 K. Combined TGA and X-ray diffractometer (XRD), the decomposition mechanism of FPL was derived by TG-IR and comparing IR spectra of FPL and its residues after burned to $327^{\circ}C$, $376^{\circ}C$ and $424^{\circ}C$, respectively. Effect of FPL on the decomposition characteristic of hexogen (RDX), a type of explosive in propellant, has been investigated using DTA at different heating rate, which shows the decomposition temperatures of the explosive are all reduced by more than 20 K. The corresponding activation energy ($E_a$) is decreased by $30kJ{\cdot}mol^{-1}$. So FPL has potential application as a combustion catalyst in solid propellant.

Landmark-based Morphometric and Meristic Analysis of Serranidae

  • Lim, Sang Gu;Jeong, Min Hwan;Kim, Bong Seok;Lee, Tae Ho;Gil, Hyun Woo;Park, In-Seok
    • Development and Reproduction
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    • v.20 no.2
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    • pp.51-63
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    • 2016
  • The landmark-based morphometric and meristic analysis of the kelp grouper (Epinephelus bruneus), red spotted grouper (E. akaara) and seven-banded grouper (E. septemfasciatus) were performed to compare the differentiation of overall body shape and structure. The measurements of the morphometric dimensions were observed in 25 parts (truss dimension: 16 parts; head part dimension: 9 parts) of 38 morphometric dimensions and also meristic differences observed in 3 parts (dorsal fin, anal fin and caudal fin) of 6 meristic counts (P < 0.05). Observed morphometric characteristics primarily involved in truss and head part dimension, kelp grouper have larger values in caudal part of truss dimension, kelp grouper, red spotted grouper and seven-banded grouper have similar values in pectoral part of truss dimension, in addition to, results of head part dimension showed that red spotted grouper have smaller values in overall dimensions (P < 0.05). As meristic characteristics, kelp grouper have more number of anal fin rays than other fish, red spotted grouper have more number of dorsal soft rays than other fish, and seven spotted grouper have more number of anal soft rays, and caudal fin rays than other fish (P < 0.05). Photographed under the x-ray, kelp grouper have the most curved vertebral column and largest swim bladder than other fishes (P < 0.05). Our results of this study confirmed that 3 subfamily fishes adequately can distinguish with external body shape, and we hope that the results of our study could be used to identify in Serranidae family as taxonomical parameters.

Addition effects of nanoscale NiO on microstructure and superconducting properties of MgB2

  • Ranot, Mahipal;Jang, S.H.;Oh, Y.S.;Shinde, K.P.;Kang, S.H.;Chung, K.C.
    • Progress in Superconductivity and Cryogenics
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    • v.18 no.1
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    • pp.37-40
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    • 2016
  • We have investigated the addition effect of NiO magnetic nanoparticles on crystal structure, microstructure as well as superconducting properties of $MgB_2$. NiO-added $MgB_2$ samples were prepared by the solid-state reaction method. The superconducting transition temperature ($T_c$) of 37.91 K was obtained for pure $MgB_2$, and $T_c$ was found to decrease systematically on increasing the addition level of NiO. X-ray diffraction (XRD) analysis revealed that no substitution of Ni for Mg in the lattice of $MgB_2$ was occurred. The microstructural analysis shows that the pure $MgB_2$ sample consists of plate shape $MgB_2$ grains, and the grains get refined to smaller size with the addition of NiO nanoparticles. At 5 K, high values of critical current density ($J_c$) were obtained for small amount NiO-added $MgB_2$ samples as compared to pure sample. The enhancement in $J_c$ could be attributed to the refinement of $MgB_2$ grains which leads to high density of grain boundaries in NiO-added $MgB_2$ samples.