• Title/Summary/Keyword: XRD Analysis

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Mineralogical Analysis of Calcium Silicate Cement according to the Mixing Rate of Waste Concrete Powder (폐콘크리트 미분말 치환율에 따른 이산화탄소 반응경화 시멘트의 광물상 분석)

  • Lee, Hyang-Sun;Song, Hun
    • Journal of the Korea Institute of Building Construction
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    • v.24 no.2
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    • pp.181-191
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    • 2024
  • In the realm of cement manufacturing, concerted efforts are underway to mitigate the emission of greenhouse gases. A significant portion, approximately 60%, of these emissions during the cement clinker sintering process is attributed to the decarbonation of limestone, which serves as a fundamental ingredient in cement production. Prompted by these environmental concerns, there is an active pursuit of alternative technologies and admixtures for cement that can substitute for limestone. Concurrently, initiatives are being explored to harness technology within the cement industry for the capture of carbon dioxide from industrial emissions, facilitating its conversion into carbonate minerals via chemical processes. Parallel to these technological advances, economic growth has precipitated a surge in construction activities, culminating in a steady escalation of construction waste, notably waste concrete. This study is anchored in the innovative production of calcium silicate cement clinkers, utilizing finely powdered waste concrete, followed by a thorough analysis of their mineral phases. Through X-ray diffraction(XRD) analysis, it was observed that increasing the substitution level of waste concrete powder and the molar ratio of SiO2 to (CaO+SiO2) leads to a decrease in Belite and γ-Belite, whereas minerals associated with carbonation, such as wollastonite and rankinite, exhibited an upsurge. Furthermore, the formation of gehlenite in cement clinkers, especially at higher substitution levels of waste concrete powder and the aforementioned molar ratio, is attributed to a synthetic reaction with Al2O3 present in the waste concrete powder. Analysis of free-CaO content revealed a decrement with increasing substitution rate of waste concrete powder and the molar ratio of SiO2/(CaO+SiO2). The outcomes of this study substantiate the viability of fabricating calcium silicate cement clinkers employing waste concrete powder.

Pedological and Mineralogical Characterizations of Hwangto (Yellow Residual Soils), Naju, Jeollanam-do, Korea (전라남도 나주시 동강면 일대 황토(풍화잔류토)의 토양학적 및 광물학적 특성 연구)

  • Kim, Yumi;Bae, Jo-Ri;Kim, Cheong-Bin;Roh, Yul
    • Economic and Environmental Geology
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    • v.47 no.2
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    • pp.87-96
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    • 2014
  • The objectives of this study were to characterize the physicochemical properties and mineralogy of Hwangto (yellow residual soils) from the southwestern part of Korea and to understand the soil-forming processes of the residual soils from their parent rocks. Both the yellowish residual soils as well as the unweathered and weathered parent rocks were obtained from Jangdong-ri, Donggang-myun, Naju, Jeollanam-do, Korea. The soil samples were examined to analyze the said soil's physicochemical properties such as color, pH, and particle size distribution. A scanning electron microscopy (SEM) with energy dispersive X-ray (EDX) analysis, transmission electron microscopy (TEM) and X-ray diffraction (XRD) analysis were performed in order to understand the mineralogy, chemical composition, and morphology of the soils. Two thin sections of a parent rock were analyzed to study its mineral composition. A particle size analysis of the soils indicates that the residual soil consists of mainly silt and clay (approximately 95%) and that soil textures are silty clay or silt clay loam. The soil colors of the residual soil are dark brown (7.5YR 3/4) through yellowish red (5YR 4/6). The pH of the residual soil ranges from 4.3 to 5.1. The major minerals of the parent rocks were quartz, biotite, chlorite, and plagioclase. The mineralogy of the sand fraction of the residual soil was quartz, biotite, muscovite and sanidine. The mineralogy of the silt fraction of the residual soil was quartz, biotite, muscovite, Na-feldspar, K-feldspar, and sanidine. The clay mineralogy of the soil was goethite, kaolinite, ilite, hydroxy-interlayed vermiculite(HIV), vermiculite, mica, K-feldspar and quartz. The mineral composition of the residual soil and the parent rock indicates that feldspar and mica in the parent rock weathered into illite, vermiculite and hydroxy-interlayed vermiculite(HIV), and finally changed into kaolinite and halloysite in the yellowish residual soils.

Mineralogy and Biogeochemistry of Intertidal Flat Sediment, Muan, Chonnam, Korea (전남 무안 갯벌 퇴적물에 관한 광물학적 및 생지화학적 연구)

  • Park, Byung-No;Lee, Je-Hyun;Oh, Jong-Min;Lee, Seuug-Hee;Han, Ji-Hee;Kim, Yu-Mi;Seo, Hyun-Hee;Roh, Yul
    • Journal of the Mineralogical Society of Korea
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    • v.20 no.1 s.51
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    • pp.47-60
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    • 2007
  • While sedimentological researches on Western coastal tidal flats of Korea have been much pelformed previously, mineralogical and biogeochemical studies are beginning to be studied. The objectives of this study were to investigate mineralogical characteritics of the inter-tidal flat sediments and to explore phase transformation of iron(oxyhydr)oxides and biomineralization by metal-reducing bacteria enriched from the inter-tidal flat sediments from Muan, Jeollanam-do, Korea. Inter-tidal flat sediment samples were collected in Chungkye-myun and Haeje-myun, Muan-gun, Jeollanam-do. Particle size analyses were performed using the pipette method and sedimentation method. The separates including sand, silt and clay fractions were examined by scanning electron microscopy (SEM) with energy dispersive X-ray (EDX) analysis, transmission electron microscopy (TEM), and X-ray diffiaction (XRD). After enriching the metal-.educing bacteria from the into,-tidal flat sediments, the bacteria were used to study phase transformation of the synthesized iron (oxyhydr)oxides and iron biomineralization using lactate or glucose as the electron donors and Fe(III)-containing iron oxides as the electron accepters. Mineralogical studies showed that the sediments of tidal flats in Chung]rye-myun and Haeje-myun consist of quartz, plagioclase, microcline, biotite, kaolinite and illite. Biogeochemical researches showed that the metal-reducing bacteria enriched from the inter-tidal flat sediments reduced reddish brown akaganeite and mineralized nanometer-sized black magnetite. The bacteria also reduced the reddish brown ferrihydrite into black amorphous phases and reduced the yellowish goethite into greenish with formation of nm-sized phases. These results indicate that microbial Fe(III) reduction may play one of important roles in iron and carbon biogeochemistry as well as iron biomineralization in subsurface environments.

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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A Conversion of AFm Phases by Addition of CaCO3, CaCl2 and CaSO4 · 2H2O (CaCO3, CaCl2 및 CaSO4 · 2H2O 첨가에 의한 AFm상의 변화)

  • 이종규;추용식
    • Journal of the Korean Ceramic Society
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    • v.40 no.1
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    • pp.24-30
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    • 2003
  • A formation and conversion of AFm phases decisively play role in the hydration, hardening and corrosion processes of various cement. In this study, the conversion of Alumino-Ferrite Monohydrates(AFm) phases under the addition of $CaCO_3,;CaCl_2;and;CaSO_4{cdot}2H_2O$was investigated by the XRD quantitative analysis. The thypical AFm phases are $M_S(monosulfoaluminate),;M_C(monocarboaluminate);and;M_{Cl}(monochloroaluminate and also Called Friedel's salts)$in this cementitious system, The conversion reaction were not occurred in $M_C-CaCO_3,;M_{Cl}-CaCO_3$ and $M_{Cl}-CaCl_2$system. However, in $M_S-CaCO_3$ system, ettringite and $monocarboaluminate(M_C)$ were formed. In $M_S-CaCl_2;system;M_S$ was transformed to Friedel's $salts(M_{Cl})$ and ettringite was formed. In the case of $CaSO_4{cdot}2H_2O$ addition, all AFm $phases(M_S,;M_C;and;M_{Cl})$ were transformed to ettringite. The order of stabilization of AFm phases under $CaCO_3,;CaCl_2;and;CaSO_4{cdot}2H_2O$ was as follows : $M_S< M_C

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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Micromorphological and Mineral Characteristics of the Jang-won Series which have Fragipan in the soil Profile (경반층 토양인 장원통의 미세형태학적 및 광물학적 특성)

  • Moon, Yong-Hee;Zhang, Yong-Seon;Chun, Hyen-Chung;Sonn, Yeon-Kyu;Hyun, Byung-Keun;Park, Chan-Won;Song, Kwan-Cheol
    • Korean Journal of Soil Science and Fertilizer
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    • v.44 no.5
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    • pp.916-921
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    • 2011
  • This study was carry out on a Jang-Won series (fine loamy, mixed, mesic family of typic fragipan) that were established and classified as a fragipan soil in Korea. The morphological, physical, chemical and minerals characteristics of Jang-Won series were studied to determine the genesis of fragipan soils in natural environment. Each sample was analyzed for its physical, chemical and mineralogical characteristics. The particle size distribution of samples was measured using pipette method. Clay minerals were investigated on parallel-oriented specimens of the clay fraction ($<2{\mu}m$) from each horizon, separated by sieving and centrifugation, using X-ray diffraction (XRD) analysis. Micromorphological observations were made on thin sections prepared from soil blocks impregnated with Crystic Resin, cut and ground to less than $30{\mu}m$ in thickness, and finally polished with diamond paste. Most horizons have pH values in the range of fewer than 5.0 and have very low base-saturation values. Their textural classification ranges from silt loam to loam, the lower horizons being the finer. The clay fraction revealed the occurrence of illite, kaolinite, chlorite and vermiculite. The micro-morphological analysis carries out thin sections from each soil profile. The silt concentrations occur as extremely dense and homogenous bands or zones of silt-sized materials, brownish in colour in plane-polarized light and anisotropic in cross-polarized light, surrounding or adhering to skeleton grains. The genesis of fragipan in the Jangweon series assumed composition of clay fraction rather than silt concentration. Therefore, this results suggested an authentic interpretation which Jangweon series is classification as Typic Fragiochrepts.

The Effect of Chloride Additives and pH on Direct Aqueous Carbonation of Cement Paste (시멘트 풀의 직접수성탄산화에서 Chloride 첨가제와 pH의 영향)

  • Lee, Jinhyun;Hwang, Jinyeon;Lee, Hyomin;Son, Byeongseo;Oh, Jiho
    • Journal of the Mineralogical Society of Korea
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    • v.28 no.1
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    • pp.39-49
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    • 2015
  • Recently, carbon capture and storage (CCS) techniques have been globally studied. This study was conducted to use waste cement powder as an efficient raw material of mineral carbonation for $CO_2$ sequestration. Direct aqueous carbonation experiment was conducted with injecting pure $CO_2$ gas (99.9%) to a reactor containing $200m{\ell}$ reacting solution and the pulverized cement paste (W:C = 6:4) having particle size less than 0.15 mm. The effects of two additives (NaCl, $MgCl_2$) in carbonation were analyzed. The characteristics of carbonate minerals and carbonation process according to the type of additives and pH change were carefully evaluated. pH of reacting solution was gradually decreased with injecting $CO_2$ gas. $Ca^{2+}$ ion concentration in $MgCl_2$ containing solution was continuously decreased. In none $MgCl_2$ solution, however, $Ca^{2+}$ ion concentration was increased again as pH decreased. This is probably due to the dissolution of newly formed carbonate mineral in low pH solution. XRD analysis indicates that calcite is dominant carbonate mineral in none $MgCl_2$ solution whereas aragonite is dominant in $MgCl_2$ containing solution. Unstable vaterite formed in early stage of experiment was transformed to well crystallized calcite with decreasing pH in the absence of $MgCl_2$ additives. In the presence of $MgCl_2$ additives, the content of aragonite was increased with decreasing pH whereas the content of calite was decreased.

Mössbauer Study of Tb2Bi1GaxFe5-xO12(x=0, 1) (Tb2Bi1GaxFe5-xO12(x=0, 1)의 뫼스바우어 분광연구)

  • Park, Il-Jin;Kim, Chul-Sung
    • Journal of the Korean Magnetics Society
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    • v.18 no.2
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    • pp.67-70
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    • 2008
  • $Tb_2Bi_1Ga_xFe_{5-x}O_{12}$(x=0, 1) fabricated by sol-gel and vacuum sealed annealing process. $Tb_2Bi_1Ga_xFe_{5-x}O_{12}$(x=0, 1) have been studied by x-ray diffraction(XRD), vibrating sample magnetometer, and $M\ddot{o}ssbauer$ spectroscopy. The crystal structures were found to be a cubic garnet structure with space group Ia3d. The determined lattice constants $a_0$ of x = 0, and 1 are $12.497\AA$, and $12.465\AA$, respectively. The distribution of gallium and iron in $Tb_2Bi_1Ga_xFe_{5-x}O_{12}$ is studied by Rietveld refinement. Based on Rietveld refinement results, the terbium and bismuth ions occupy the 24c site, iron ions occupy the 24d, l6a site, and nonmagmetic gallium ions occupy the 16a site. In order to verify the magnetic site occupancy of iron and gallium, we have taken $M\ddot{o}ssbauer$ spectra for $Tb_2Bi_1Ga_xFe_{5-x}O_{12}$(x=0, 1) at room temperature. From the results of $M\ddot{o}ssbauer$ spectra analysis, the absorption area ratios of Fe ions for $Tb_2Bi_1Fe_5O_{12}$ on 24d and 16a sites are 60.8 % and 39.2 %, respectively, and the absorption area ratios of Fe ions for $Tb_2Bi_1Fe_5O_{12}$ on 24d and 16a sites are 74.7 % and 25.3 %, respectively. It is noticeable that all of the nonmagnetic Ga atoms occupy the 16a site by vacuum annealing process.

Mineralogical Characteristics of the Noro and Miag Series Soils Developed on the Cinder Cones in Jeju Island (제주도(濟州道) 산록(山麓)의 분석구(噴石丘)에서 발달(發達)된 노로통과 미악통 토양(土壤)의 광물학적(鑛物學的) 특성(特性))

  • Zhang, Yong-Seon;Kim, Yoo-Hak;Song, Kwan-Cheol;Kim, Sun-Kwan
    • Korean Journal of Soil Science and Fertilizer
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    • v.35 no.3
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    • pp.145-152
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    • 2002
  • The composition of primary minerals in the rocks and secondary minerals of clay fractions of the soil developed on the cinder cones in the foot of Halla Mt., Jeju Island was investigated. The effects of parent materials on the physico-chemical properties and mineralogical characteristics were evaluated by XRD, DTA with the chemical composition of $H^+$ saturated clays. The main rock-forming minerals of a residual cinder cones were plagioclase with subsidiary minerals of hematite, gibbsite and quartz in the red cinder cone and of augite, quartz, feldspars and olivine in black cinder cone. It is demonstrated that ignition loss and sesquioxides content were higher in the red cinder soil than black cinder, which was resulted in the intermittent eruption of volcanic activity. For the chemical analysis of whole soils, $SiO_2/Al_2O_3$ ratio was increased from 2 to 3, but Ignition loss is decreased and $K_2O$ content are very low with increasing the soil depth in regard to the composition and kinds of clay minerals. No clay formation from micas mineral were in volcanic ashes. Dominant clay minerals of the cinder cone soils as a black and red cinder cone soil were allophane with some quartz and feldspars, while vermiculite, illite, kaolin were coexisted as a subsidiary minerals. But the red cinder cones soils had more hematite and gibbsite of the clay fractions than the black soils with magnetite. The exothermic pick of DTA at about $660^{\circ}C$ for cinder cone soils might be corresponded the oxidation magnetite to hematite reation. With regarding to the compositions of mineral detected by X-ray diffractogram and the properties of minerals by D.T.A thermogram, the dominant clay mineral was allophane of the cinder cone soils with some ferrous compounds, red colour of the cinder cone soils which are originated in hematite.