• Title/Summary/Keyword: x-ray diffractometry

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Effects of Sugars on the Retrogradation of Rice Flour Gels (당 첨가가 쌀가루겔의 노화에 미치는 영향)

  • Choi, Cha-Ran;Shin, Mal-Shick
    • Korean Journal of Food Science and Technology
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    • v.28 no.5
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    • pp.904-909
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    • 1996
  • To investigate effects of sugars on the retrogradation of rice flour gels, sucrose and isomaltooligosaccharide (1, 2, and 5%, w/w on the flour basis were added to 50% Dongjinbyeo rice flour gels and stored at different temperature $(20^{\circ}C,\;4^{\circ}C)$ far 1, 3 and 6 days. Changes on the degree of retrogradation (DR) of these rice flour gels were measured by α-amylase-iodine method, DSC and X-ray diffractometry. DRs of rice flour gels increased over storage and showed a rapid increase up to 3 days and then decreased thereafter. DRs of rice flour gels with sucrose or oligosaccharide also increased rapidly until 3 day storage but these values were lower than those of rice flour gels without sugar. DRs of rice flour gels with oligosaccharide were lower than those of gels with sucrose. Changes in enthalpy of rice flour gels measured by DSC showed the same tendency with those in DRs of rice flour gels by ${\alpha}-amylase-iodine$ method, but varied with sugar levels.

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Characterization of Arsenic Immobilization in the Myungbong Mine Tailing (명봉광산의 광미 내 비소의 고정화 특성 연구)

  • Lee, Woo-Chun;Jeong, Jong-Ok;Kim, Ju-Yong;Kim, Soon-Oh
    • Economic and Environmental Geology
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    • v.43 no.2
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    • pp.137-148
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    • 2010
  • The Myoungbong mine located in Boseong-gun, Jellanamdo consists of Au-Ag bearing quartz veins which filled the fissures of Bulguksa granitic rocks of Cretaceous. The tailings obtained from the Myungbong mine were used to investigate the effects of various processes, such as oxidation of primary sulfides and formation(alteration) of secondary and/or tertiary minerals, on arsenic immobilization in tailings. This study was conducted via both mineralogical and chemical methods. Mineralogical methods used included gravity and magnetic separation, ultrasonic cleaning, and instrumental analyses(X-ray diffractometry, energy-dispersive spectroscopy, and electron probe microanalyzer) and aqua regia extraction technique for soils was applied to determine the elemental concentrations in the tailings. Iron (oxy)hydroxides formed as a result of oxidation of tailings were identified as three specific forms. The first form filled in rims and fissures of primary pyrites. The second one precipitated and coated the surfaces of gangue minerals and the final form was altered into yukonites. Initially, large amounts of acid-generating minerals, such as pyrite and arsenopyrite, might make the rapid progress of oxidation reactions, and lots of secondary minerals including iron (oxy)hydroxides and scorodite were formed. The rate of pH decrease in tailings diminished, in addition, as the exposure time of tailings to oxidation environments was prolonged and the acid-generating minerals were depleted. Rather, it is speculated that the pH of tailings increased, as the contribution of pH neutralization reactions by calcite contained in surrounding parental rocks became larger. The stability of secondary minerals, such as scorodite, were deteriorated due to the increase in pH, and finally arsenic might be leached out. Subsequently, calcimn and arsenic ions dissociated from calcites and scorodites were locally concentrated, and yukonite could be grown tertiarily. It is confirmed that this tertiary yukonite which is one of arsenate minerals and contains arsenic in high level plays a crucial role in immobilizing arsenic in tailings. In addition to immobilization of arsenic in yukonites, the results indicate that a huge amount of iron (oxy)hydroxides formed by weathering of pyrite which is one of typical primary minerals in tailings can strongly control arsenic behavior as well. Consequently, this study elucidates that through a sequence of various processes, arsenic which was leached out as a result of weathering of primary minerals, such as arsenopyrite, and/or redissolved from secondary minerals, such as scorodite, might be immobilized by various sorption reactions including adsorption, coprecipiation, and absorption.

Characterization on the Behavior of Heavy Metals and Arsenic in the Weathered Tailings of Songcheon Mine (송천광산의 풍화광미 내 중금속 및 비소 거동 특성)

  • Lee, Woo-Chun;Kim, Young-Ho;Cho, Hyen-Goo;Kim, Soon-Oh
    • Journal of the Mineralogical Society of Korea
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    • v.23 no.2
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    • pp.125-139
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    • 2010
  • Behavior of heavy metals and arsenic in the tailings of Songcheon Au-Ag mine was characterized via both mineralogical and geochemical methods. Mineral composition of the tailings was investigated by X-ray diffractometry, energy-dispersive spectroscopy, and electron probe micro-analyzer (EPMA) and total concentrations of heavy metals and arsenic and their chemical forms were analyzed by total digestion of aqua regia and sequential extraction method, respectively. The results of mineralogical study indicate that the tailings included mineral particles of resinous shape mainly consisting of galena, sphalerite, pyrite, quartz, and scorodite, and specifically socordite was identified in the form of matrix. EPMA quantitative analyses were performed to evaluate the weatherability of each mineral, and the results suggest that it decreased in the sequence of arsenopyrite > galena > sphalerite > pyrite. The weathering pattern of galena was observed to show distinctive zonal structure consisting of secondary minerals such as anglesite and beudantite. In addition, almost all of arsenopyrite has been altered to scorodite existing asmatrix and galena, sphalerite, and pyrite which have lower weatherability than arsenopyrite were identified within the matrix of scorodite. During the process of alteration of arsenopyrite into scorodite, it is likely that a portion of arsenic was lixiviated and caused a great deal of detrimental effects to surrounding environment. The results of EPMA quantitative analyses verify that the stability of scorodite was relatively high and this stable scorodite has restrained the weathering of other primary minerals within tailings as a result of its coating of mineral surfaces. For this reason, Songcheon tailings show the characteristics of the first weathering stage, although they have been exposed to the surface environment for a long time. Based on the overall results of mineralogical and geochemical studies undertaken in this research, if the tailings are kept to be exposed to the surface environment and the weathering process is continuous, not only hazardous heavy metals, such as lead and arsenic seem to be significantly leached out because their larger portions are being partitioned in weakly-bound (highly-mobile) fractions, but the potential of arsenic leaching is likely to be high as the stability of scorodite is gradually decreased. Consequently, it is speculated that the environmental hazard of Songcheon mine is significantly high.

A Scientific Study of Roof Tiles in Joseon Dynasty from Dongdaemoon Stadium (동대문운동장유적 출토 조선시대 기와의 특성 연구)

  • Chung, Kwang-Yong
    • Korean Journal of Heritage: History & Science
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    • v.45 no.3
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    • pp.160-173
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    • 2012
  • Roofing tile research conducted in Korea so far is mostly related to studies on roofing tile patterns excavation report on the roof tile klin site in the aspects of archeology architecture and history of art. There have been continuous studies on kiln ground and manufacture techniques of roofing tiles. However it is difficult to find roofing tiles research based on scientific experiments. The research on this paper performs physical and chemical experimental study to understand order, manufacturing techniques and other characteristics of Chosun Dynasty roofing tiles excavated in Dongdaemun stadium. As for physical experimental study water absorption, specific gravity, whole-rock Magnetic susceptibility rate and Differential Thermal Analysis are conducted. As for chemical experimental study, neutron activation analysis(NAA), microstructure observation, X-ray diffractometry(XRD) analysis are conducted. Result of neutron activation analysis and statistical analysis on piece of roof tile 22 samples clearly show that the roofing tile samples are from different time line and places. It also shows different composition when compare average value of rare earth resources per findspots. It means roofing tiles were manufactured from clay mineral from several places. Close inspection using XRD and polarization microscope reveals that main components of roofing tiles are quartz and felspar. Mica and Illite are found partially. XRD analysis shows mullite mineral composition which occurs when roofing tile is calcined around $1000^{\circ}C$. Differential thermal analysis shows gradual exothermic peak near $900^{\circ}C$. Based on these results, it is assumed that roofing tile is made at $900{\sim}1000^{\circ}C$. result of XRD analysis shows mullite were made near $1000^{\circ}C$. in Differential Thermal Analysis shows gradual exothermic peak near $900^{\circ}C$. this results shows that roof tiles were made near 900~1000 near $1000^{\circ}C$ mean value of whole-rock Magnetic susceptibility rate. When performed comparative analysis using whole-rock Magnetic susceptibility rate average value, findspots provided no certain classification to arrange. Nonetheless low whole-rock Magnetic susceptibility rate 0.2~0.78(${\times}103$ SI unit) is found when roofing tile patterns are Pasangmun, Taesangmun, Eosangmun, Kyukjamun, Heongsunmun. Overall absorptivity is 14~21%. It is similar to 14~18% of roofing tile from Chosun Dynasty. There is only 1.4~2.5g/cm3 of roof tile sample specific gravity. The analysis finds no difference in specific gravity by findspots.

A Study of Coloration of Topaz(I): Mineralogical and Chemical Study on the Topaz Selected from Some Localities of the World (토파즈의 人工着色 處理를 위한 硏究(I) : 世界 主要 産地別 토파즈의 鑛物學的 및 化學的 特性)

  • Han, Yi-Kyeong;Park, Maeng-Eon;Jang, Yong-Nam
    • Journal of the Mineralogical Society of Korea
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    • v.5 no.2
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    • pp.109-121
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    • 1992
  • For the purpose of mineralogical and chemical study on the topazes from various localities of world(Brzail, China, India, Nigeria and Sri Lanka), electron microprobe analysis(EPMA), neutron activation analysis(NAA), X-ray diffractometry, Raman spectroscopy, etch test, scanning electron microscopy, refractive index, specific gravity, fluid inclusion were performed. The chemical composition in topaz was discussed along with its physical and structural properties. Variations in the unit-cell dimension and physical properties of topaz were found to have a close relations in the unit-cell dimension and physical properties of topaz were found to have a close relationship with extent of substitution of $OH^-\;for\;F^-$. According to neutron activation analyses, the trace elements had no effects on the physical properties of topaz. Raman spectra showed that the peaks of topaz were different in intensity from one locality to another. Etching defects in topaz includes negative crystal defect o point-bottom pit(India, Nigeria) and net work defect of curl-bottom pit(Brazil, China). Fluid inclusions in topaz may be classiffied into liquid $CO_2$-bearing inclusion, gaseous inclusion, halite, sylvite-bearing inclusion and liquid inclusion. The results of this study can be useful to devising artificial coloring methods for topaz with different mineralogical compositions.

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Compositional Variation of Arsenopyrites in Arsenic and Polymetallic Ores from the Ulsan Mine, Republic of Korea, and their Application to a Geothermometer (울산광산산(蔚山鑛山産) 유비철석(硫砒鐵石)의 조성변화(組成變化) 및 지질온도계(地質溫度計)에 대(對)한 적용(適用))

  • Choi, Seon-Gyu;Chung, Jae-Ill;Imai, Naoya
    • Economic and Environmental Geology
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    • v.19 no.3
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    • pp.199-218
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    • 1986
  • Arsenopyrite in arsenic and polymetallic ores from calcic Fe-W skarn deposit of the Ulsan mine, Republic of Korea, has been investigated by means of electron microprobe analysis and X-ray diffractometry. As a result, it is revealed that the Ulsan arsenopyrite may be classified into the following three species with different generation on the basis of its mode of occurrence, chronological order during polymetallic mineralization and chemical composition; arsenopyrites I, II and III. 1) Arsenopyrite I-(Ni, Co)-bearing species belonging to the oldest generation, which has crystallized together with (Ni, Co)-arsenides and -sulpharsenides in the early stage of polymetallic mineralization. In rare cases, it contains a negligible amount of antimony. It occurs usually as discrete grains with irregular outline, showing rarely subhedral form, and is diffused in skarn zone. The maximum contents of nickel and cobalt are 10.04 Ni and 2.45 Co (in weight percent). Occasionally, it shows compositional zoning with narrow rim of lower (Ni+Co) content. 2) Arsenopyrite II-arsenian species, in which (Ni+Co) content is almost negligible, may occur widely in arsenic ores, and its crystallization has followed that of arsenopyrite I. It usually shows subhedral to euhedral form and is closely associated with $l{\ddot{o}}llingite$, bismuth, bismuthinite, chalcopyrite, sphalerite, bismuthian tennantite, etc. It is worthy of note that arsenopyrite II occasionally contains particles consisting of both bismuth and bismuthinite. 3) Arsenopyrite III-(Ni, Co)-free, S-excess and As-deficient species is close to the stoichiometric composition, FeAsS. It occurs in late hydrothermal veins, which cut clearly the Fe-W ore pipe and the surrounding skarn zone. It shows euhedral to subhedral form, being extremely coarse-grained, and is closely associated with pyrite, "primary" monoclinic pyrrhotite, galena, sphalerite, etc. Among three species of the Ulsan arsenopyrite, arsenopyrite I does not serve as a geothermometer, because (Ni+Co) content always exceeds 1 weight percent. In spite of the absence of Fe-S minerals as sulphur-buffer assemblage, the presence of $Bi(l)-Bi_2S_3$ sulphur-buffer enables arsenopyrite II to apply successfully to the estimation of either temperature and sulphur fugacity, the results are, $T=460{\sim}470^{\circ}C$, and log $f(S_2)=-7.4{\sim}7.0$. With reference to arsenopyrite III, only arsenopyrite coexisting with pyrite and "primary" monoclinic pyrrhotite may serve to restrict the range of both temperature and sulphur fugacity, $T=320{\sim}440^{\circ}C$, log $f(S_2)=-9.0{\sim}7.0$. These temperature data are consistent with those obtained by fluid inclusion geothermometry on late grandite garnet somewhat earlier than arsenopyrite II. At the beginning of this paper, the geological environments of the ore formation at Ulsan are considered from regional and local geologic settings, and physicochemical conditions are suspected, in particular the formation pressure (lithostatic pressure) is assumed to be 0.5kb (50MPa). The present study on arsenopyrite geothermometry, however, does not bring about any contradictions against the above premises. Thus, the following genetical view on the Ulsan ore deposit previously advocated by two of the present authors (Choi and Imai) becomes more evident; the ore deposit was formed at shallow depth and relatively high-temperature with steep geothermal gradient-xenothermal conditions.

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A bilayer diffusion barrier of atomic layer deposited (ALD)-Ru/ALD-TaCN for direct plating of Cu

  • Kim, Soo-Hyun;Yim, Sung-Soo;Lee, Do-Joong;Kim, Ki-Su;Kim, Hyun-Mi;Kim, Ki-Bum;Sohn, Hyun-Chul
    • Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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    • 2008.06a
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    • pp.239-240
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    • 2008
  • As semiconductor devices are scaled down for better performance and more functionality, the Cu-based interconnects suffer from the increase of the resistivity of the Cu wires. The resistivity increase, which is attributed to the electron scattering from grain boundaries and interfaces, needs to be addressed in order to further scale down semiconductor devices [1]. The increase in the resistivity of the interconnect can be alleviated by increasing the grain size of electroplating (EP)-Cu or by modifying the Cu surface [1]. Another possible solution is to maximize the portion of the EP-Cu volume in the vias or damascene structures with the conformal diffusion barrier and seed layer by optimizing their deposition processes during Cu interconnect fabrication, which are currently ionized physical vapor deposition (IPVD)-based Ta/TaN bilayer and IPVD-Cu, respectively. The use of in-situ etching, during IPVD of the barrier or the seed layer, has been effective in enlarging the trench volume where the Cu is filled, resulting in improved reliability and performance of the Cu-based interconnect. However, the application of IPVD technology is expected to be limited eventually because of poor sidewall step coverage and the narrow top part of the damascene structures. Recently, Ru has been suggested as a diffusion barrier that is compatible with the direct plating of Cu [2-3]. A single-layer diffusion barrier for the direct plating of Cu is desirable to optimize the resistance of the Cu interconnects because it eliminates the Cu-seed layer. However, previous studies have shown that the Ru by itself is not a suitable diffusion barrier for Cu metallization [4-6]. Thus, the diffusion barrier performance of the Ru film should be improved in order for it to be successfully incorporated as a seed layer/barrier layer for the direct plating of Cu. The improvement of its barrier performance, by modifying the Ru microstructure from columnar to amorphous (by incorporating the N into Ru during PVD), has been previously reported [7]. Another approach for improving the barrier performance of the Ru film is to use Ru as a just seed layer and combine it with superior materials to function as a diffusion barrier against the Cu. A RulTaN bilayer prepared by PVD has recently been suggested as a seed layer/diffusion barrier for Cu. This bilayer was stable between the Cu and Si after annealing at $700^{\circ}C$ for I min [8]. Although these reports dealt with the possible applications of Ru for Cu metallization, cases where the Ru film was prepared by atomic layer deposition (ALD) have not been identified. These are important because of ALD's excellent conformality. In this study, a bilayer diffusion barrier of Ru/TaCN prepared by ALD was investigated. As the addition of the third element into the transition metal nitride disrupts the crystal lattice and leads to the formation of a stable ternary amorphous material, as indicated by Nicolet [9], ALD-TaCN is expected to improve the diffusion barrier performance of the ALD-Ru against Cu. Ru was deposited by a sequential supply of bis(ethylcyclopentadienyl)ruthenium [Ru$(EtCp)_2$] and $NH_3$plasma and TaCN by a sequential supply of $(NEt_2)_3Ta=Nbu^t$ (tert-butylimido-trisdiethylamido-tantalum, TBTDET) and $H_2$ plasma. Sheet resistance measurements, X-ray diffractometry (XRD), and Auger electron spectroscopy (AES) analysis showed that the bilayer diffusion barriers of ALD-Ru (12 nm)/ALD-TaCN (2 nm) and ALD-Ru (4nm)/ALD-TaCN (2 nm) prevented the Cu diffusion up to annealing temperatures of 600 and $550^{\circ}C$ for 30 min, respectively. This is found to be due to the excellent diffusion barrier performance of the ALD-TaCN film against the Cu, due to it having an amorphous structure. A 5-nm-thick ALD-TaCN film was even stable up to annealing at $650^{\circ}C$ between Cu and Si. Transmission electron microscopy (TEM) investigation combined with energy dispersive spectroscopy (EDS) analysis revealed that the ALD-Ru/ALD-TaCN diffusion barrier failed by the Cu diffusion through the bilayer into the Si substrate. This is due to the ALD-TaCN interlayer preventing the interfacial reaction between the Ru and Si.

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