• Title/Summary/Keyword: XRD 분석

Search Result 2,855, Processing Time 0.044 seconds

Petrological Study on the Spherulitic Rhyolite in the Jangsan Area, Busan (부산 장산 지역의 구과상(球課狀) 유문암에 대한 암석학적 연구)

  • Park, Sumi;Yun, Sung-Hyo
    • The Journal of the Petrological Society of Korea
    • /
    • v.22 no.3
    • /
    • pp.219-233
    • /
    • 2013
  • Spherulitic rhyolite occur as part of ring dyke which showing a vertical flowage of $60^{\circ}{\sim}90^{\circ}$, of the Jangsan cauldron was studied. The spherulites range in diameter from a few millimeters to 2.8 centimeters or more, and average 5~10 millimeters. It belongs to radiated simple spherulite type. They consist of a core of moderate brown dense material encased by a thin crust, a few millimeters thick at most of white grey material. The spherulites frequently have a radiating fibrous structure, which are thought to have formed as a consequence of rapid mineral growth caused by very fast cooling of the dykes in shallow depth near the surface. EPMA examination of the concentric-zoned core of spherulites show that they are mainly composed of cryptocrystalline-fibrous intergrowth of silica minerals and alkali feldspars which have $SiO_2$ 82% or more, $Al_2O_3$ 7~10%, $Na_2O+K_2O$ less than 8%. The feldspar compositions of the spherulites lie essentially within the sanidine field. XRD examination show that spherulites are mainly composed of quartz, sanidine, albite with minor mica, kaolinite and chlorite. According to X-ray mapping, the spherulites are enriched in $SiO_2$ in the core and partly enriched $Na_2O$ or $K_2O$, $Al_2O_3$ in the shell that reflect in compositional zoning with increasing spherulitic devitrification. The feathery and non-equant crystal shapes of spherulites from rhyolite dyke of Jangsan cauldron suggest that they may have formed during the rapid cooling of dyke under the static state, or faster velocity of devitrification from glassy materials than movement velocity of the magma intrusion. The spherulitic rhyolite originated from high-silica(75.4~75.7 wt.%) rhyolite magma.

모재/중간층/박막의 H/E ratio 구배에 따른 Cr계 경질 박막의 기계적 특성에 관한 연구

  • Kim, Hoe-Geun;Song, Myeon-Gyu;Lee, Sang-Yul
    • Proceedings of the Korean Institute of Surface Engineering Conference
    • /
    • 2018.06a
    • /
    • pp.135-135
    • /
    • 2018
  • 천이금속 질화물 코팅은 우수한 기계적 특성들로 인해 공구 코팅으로 많이 사용 되어왔다. 그 중에서도 특히 Cr계 경질 코팅은 높은 경도와 낮은 표면조도, 우수한 마찰특성 등 뛰어난 기계적 특성을 나타내므로 공구 코팅으로의 적용 가능성이 크다. 그러나 최근 공구산업의 발전으로 인해 공구가 더욱 가혹한 환경에서 사용됨에 따라, 공구의 수명을 향상시키고 보호하기 위해 코팅의 높은 밀착력이 요구되고 있으며, 모재와 코팅 사이에 중간층을 합성함으로써 공구의 밀착력을 향상시키는 연구가 활발히 진행되고 있다. 이전 연구에서 모재/중간층/코팅간의 경도와 탄성계수 비율(H/E ratio)의 구배가 코팅의 밀착력에 큰 영향을 미치는 것으로 확인되었다. 그러므로, WC 모재와 Cr계 코팅의 중간값의 H/E ratio를 갖는 중간층의 합성을 통해 코팅의 밀착력을 향상시킬 수 있을 것으로 판단된다. 본 연구에서는, 코팅의 밀착력을 향상시키기 위해 다양한 중간층을 증착한 CrZrN, CrAlN 코팅을 비대칭 마그네트론 스퍼터링 장비를 이용하여 합성하였다. 모재로는 디스크 형상의 WC-6wt.%Co 시편을 사용하였고 Cr, Zr, Si, Al single 타겟을 이용하여 Cr, CrN, CrZrN, CrZrSiN 등의 중간층이 증착된 코팅을 합성했다. 코팅의 합금상, 경도 및 탄성계수, 미세조직 및 조성, 표면 조도을 확인하기 위해 X-ray diffractometer (XRD), Fischer scope, field-emission scanning electron microscopy (FE-SEM), energy dispersive X-ray spectroscopy (EDS), atomic force microscopy를 사용하였고, 코팅의 밀착 특성을 분석하기 위해 scratch tester와 optical microscopy (OM)를 이용하였다. 코팅의 내열성을 확인하기 위해 코팅을 furnace에 넣어 공기중에서 500, 600, 700, 800, 900, $1,000^{\circ}C$로 30분 동안 annealing 한 후에 nano-indentation을 사용하여 경도를 측정하였다. CrZrN 및 CrAlN 코팅을 나노 인덴테이션으로 분석한 결과, 모든 코팅의 경도(33.4-35.8 GPa)와 탄성계수(384.1-391.4 GPa)는 중간층의 종류에 상관없이 비슷한 값을 보인 것으로 확인됐다. 그러나, 코팅의 마찰계수는 중간층의 종류에 따라 다른 값을 보였다. CrZrN 코팅의 경우 CrN 합금상 중간층을 갖을 때 가장 낮은 값을 보였으며, CrAlN 코팅의 경우 CrN/CrZrSiN 중간층을 증착하였을때 마찰계수는 0.34로 CrZrN 중간층을 증착하였을 때(0.41)에 비해 낮은 값을 보였다. 또한, 코팅의 마모율 및 마모폭도 비슷한 경향을 보인 것으로 보아, CrN/CrZrSiN 중간층을 합성한 CrAlN 코팅의 내마모성이 상대적으로 우수한 것으로 판단된다. 코팅의 밀착력의 경우도 마찰계수와 비슷한 경향을 보였다. 이것은 중간층의 H/E ratio가 코팅의 내마모성에 미치는 영향에 의한 결과로 사료된다. H/E ratio는 파단시의 최대 탄성 변형율로써, 모재/중간층/코팅의 H/E ratio 구배에 따라 코팅 내의 응력의 완화 정도가 변하게 된다. WC 모재 (H/E=0.040)와 CrAlN 코팅(H/E=0.089) 사이에서 CrN, CrZrSiN 중간층의 H/E ratio는 각각 0.076, 0.083으로 모재/중간층/코팅의 H/E ratio 구배가 점차 증가함을 확인 할 수 있었고, 일정 응력이 지속적으로 가해지면서 진행되는 마모시험중에 CrN과 CrZrSiN 중간층이 WC와 CrAlN 코팅 사이에서 코팅 내부의 응력구배를 완화시키는 역할을 함으로써 CrAlN 코팅의 내마모성이 향상된 것으로 판단된다. 모든 코팅을 열처리 후 경도 분석 결과, CrN/CrZrSiN 중간층을 증착한 CrAlN 코팅은 $1,000^{\circ}C$까지 약 28GPa의 높은 경도를 유지한 것으로 확인 되었고, 이는 CrZrSiN 중간층 내에 존재하는 SiNx 비정질상의 우수한 내산화성에 의한 결과로 판단된다.

  • PDF

Relationship between Physicochemical Properties, Heavy Metal Contents and Magnetic Susceptibility of Soils (토양의 물리화학적 특성, 중금속 함량, 대자율 간의 상호관계 연구)

  • Chon, Chul-Min;Park, Jeong-Sik;Kim, Jae-Gon;Lee, Youn-Soo
    • Journal of the Mineralogical Society of Korea
    • /
    • v.23 no.4
    • /
    • pp.281-295
    • /
    • 2010
  • This paper deals with magnetic susceptibility, mineralogy, soil properties (pH, EC, CEC, loss on ignition), iron and manganese oxides, the content and partitioning of heavy metals (As, Cd, Cr, Cu, Ni, Pb, Zn), and their mutual relationship in the soil samples of an unpolluted, abandoned mine area, and industrial complex area. The various minerals derived from weathered bedrock were identified by X-ray diffraction in the unpolluted soil samples, except for the magnetic minerals. XRD analysis also revealed the existence of hematite and magnetite related to mine tailings and waste rocks in the abandoned mine area samples. The industrial complex area samples had carbonate minerals, such as calcite and dolomite, that might be due to anthropogenic deposition. The sum of the reducible, oxidizable, and residual fractions was over 80% for the abandoned mine area samples and over 50% for the industrial complex area samples using the sequential extraction method. The industrial complex area samples had a relatively high carbonate fraction that was associated with carbonate minerals. The content of aqua regia-extractable Fe, Mn, As, and Zn had a high positive correlation with the content of the dithionite-citrate-bicarbonate (DCB)-extractable method related to Fe/Mn oxide phases. The 54% and 58% of aqua regia-extractable Fe and As content, respectively, acted together with the concentrations of the DCB-extractable phases. Magnetic susceptibility values of total samples ranged from 0.005 to $2.131{\times}10^{-6}m^3kg^{-1}$. The samples including iron oxide minerals, such as hematite and magnetite, had a high magnetic susceptibility. The magnetic susceptibility showed a significant correlation with the heavy metals, Cd (r=0.544, p<0.05), Cr (r=0.714, p<0.01), Ni (r=0.645, p<0.05), Pb (r=0.703, p<0.01), and Zn (r=0.496, p<0.01), as well as Fe (r=0.608, p<0.01) and Mn (r=0.615, p<0.01). The aqua regia-extractable Fe and Mn content had a significant positive correlation with Cd, Cr, Cu, Ni, and Zn. However, the DCB-extractable Fe and Mn content had a significant positive correlation with As and Ni, indicating that the heavy metals were associated with Fe and Mn oxide minerals.

Physicochemical Characteristic of the Silkworm Sericin Cocoon (세리신잠견의 이화학적 특성)

  • 김수연;손해룡;배도규;김정호
    • Journal of Sericultural and Entomological Science
    • /
    • v.45 no.1
    • /
    • pp.10-17
    • /
    • 2003
  • This study was carried out to analyze physicochemical characteristics of sericin cocoon from silkworm, Bombyx mori. The degumming loss increased with increasing treatment time up to 2 hr, and temperature up to 130$^{\circ}C$. At 130$^{\circ}C$, degumming loss of Nd-s jam and Nd$\^$H/ jam were 100% while that of Baegok jam was 24%. Nd-s jam and Baegok jam ha high glycine content of 29.1∼46.3 mol% where as Nd$\^$H/ jam had high serine content of 32.6 mol%. Thermal denaturation temperatures were found at 218$^{\circ}C$ for Nd-s jam, 216$^{\circ}C$ for Nd$\^$H/ jam, and 218$^{\circ}C$ for Baegok jam. Before degumming, crystallinities obtained by FT-IR analysis were 44.3, 43.7, and 59.9% for Nd-s jam, Nd$\^$H/ jam, and Baegok jam respectively. After degumming, crystallinity increased to 61.8% for Baegok jam. Before degumming, crystallinitics obtained from XRD were 35.9, 33.5, and 47.2%, for Nd-s jam, Nd$\^$H/ jam, and Baegok jam. After degumming, crystallinity increased to 49.8% for Baegok jam. The molecular weight of Nd$\^$H/ jam were 9,417 in 1 hr, 3,744 in 2 hr, 4,944 in hr, and 3,910 in 6 hr.

Geochemical Equilibria and Kinetics of the Formation of Brown-Colored Suspended/Precipitated Matter in Groundwater: Suggestion to Proper Pumping and Turbidity Treatment Methods (지하수내 갈색 부유/침전 물질의 생성 반응에 관한 평형 및 반응속도론적 연구: 적정 양수 기법 및 탁도 제거 방안에 대한 제안)

  • 채기탁;윤성택;염승준;김남진;민중혁
    • Journal of the Korean Society of Groundwater Environment
    • /
    • v.7 no.3
    • /
    • pp.103-115
    • /
    • 2000
  • The formation of brown-colored precipitates is one of the serious problems frequently encountered in the development and supply of groundwater in Korea, because by it the water exceeds the drinking water standard in terms of color. taste. turbidity and dissolved iron concentration and of often results in scaling problem within the water supplying system. In groundwaters from the Pajoo area, brown precipitates are typically formed in a few hours after pumping-out. In this paper we examine the process of the brown precipitates' formation using the equilibrium thermodynamic and kinetic approaches, in order to understand the origin and geochemical pathway of the generation of turbidity in groundwater. The results of this study are used to suggest not only the proper pumping technique to minimize the formation of precipitates but also the optimal design of water treatment methods to improve the water quality. The bed-rock groundwater in the Pajoo area belongs to the Ca-$HCO_3$type that was evolved through water/rock (gneiss) interaction. Based on SEM-EDS and XRD analyses, the precipitates are identified as an amorphous, Fe-bearing oxides or hydroxides. By the use of multi-step filtration with pore sizes of 6, 4, 1, 0.45 and 0.2 $\mu\textrm{m}$, the precipitates mostly fall in the colloidal size (1 to 0.45 $\mu\textrm{m}$) but are concentrated (about 81%) in the range of 1 to 6 $\mu\textrm{m}$in teams of mass (weight) distribution. Large amounts of dissolved iron were possibly originated from dissolution of clinochlore in cataclasite which contains high amounts of Fe (up to 3 wt.%). The calculation of saturation index (using a computer code PHREEQC), as well as the examination of pH-Eh stability relations, also indicate that the final precipitates are Fe-oxy-hydroxide that is formed by the change of water chemistry (mainly, oxidation) due to the exposure to oxygen during the pumping-out of Fe(II)-bearing, reduced groundwater. After pumping-out, the groundwater shows the progressive decreases of pH, DO and alkalinity with elapsed time. However, turbidity increases and then decreases with time. The decrease of dissolved Fe concentration as a function of elapsed time after pumping-out is expressed as a regression equation Fe(II)=10.l exp(-0.0009t). The oxidation reaction due to the influx of free oxygen during the pumping and storage of groundwater results in the formation of brown precipitates, which is dependent on time, $Po_2$and pH. In order to obtain drinkable water quality, therefore, the precipitates should be removed by filtering after the stepwise storage and aeration in tanks with sufficient volume for sufficient time. Particle size distribution data also suggest that step-wise filtration would be cost-effective. To minimize the scaling within wells, the continued (if possible) pumping within the optimum pumping rate is recommended because this technique will be most effective for minimizing the mixing between deep Fe(II)-rich water and shallow $O_2$-rich water. The simultaneous pumping of shallow $O_2$-rich water in different wells is also recommended.

  • PDF

Heat Shield Property of Nanostructural-regulated Fe2O3/TiO2 Composites Filled with Polyacrylate Paint (나노구조 변화에 의한 Fe2O3/TiO2 복합재료를 충전한 Poly Acrylate 도료의 열차단 특성)

  • Kim, Dae Won;Ma, Young Kil;Kim, Jong Seok
    • Applied Chemistry for Engineering
    • /
    • v.31 no.1
    • /
    • pp.43-48
    • /
    • 2020
  • Fe2O3 nanoparticles with the mixed structure of cubic and nanorod were synthesized by precipitation, hydrothermal, sol-gel method, etching process and heat treatment. Fe2O3/TiO2 core-shell (CS) of type Fe2O3@TiO2 composite was fabricated on a 20 nm nanolayer of TiO2 coated on the surface of Fe2O3 nanoparticles. Fe2O3/TiO2 yolk-shell (YS) composite was prepared by chemical etching and heat treatment of Fe2O3/TiO2 CS nanoparticles. Physical properties of Fe2O3, Fe2O3@TiO2 CS and Fe2O3@TiO2 YS nanoparticles were characterized by FE-SEM, HR-TEM and X-ray diffraction. The solar reflectance, commission internationale de l'Elcairage (CIE) color coordinate and heat shield temperatures of Fe2O3, CS and YS type Fe2O3@TiO2 pigments filled with poly acrylate (PA) paints were investigated by UV-Vis-NIR spectrometer and homemade heat shield temperature measuring device. The Fe2O3@TiO2 YS red pigment filled PA composite exhibited excellent near infrared light reflecting performance and also reduced the heat shield temperature of 13 ℃ than that of Fe2O3 filled counterparts.

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
    • /
    • v.28 no.1
    • /
    • pp.39-49
    • /
    • 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.

A study on the synthesis of lanthanum oxide (La2O3) from NaLa(SO4)2·H2O by metathesis reaction (NaLa(SO4)2·H2O 결정상으로부터 이온치환반응에 의한 산화란탄 (La2O3) 분말 합성에 관한 연구)

  • Kim, Dae-Weon;Ahn, Nak-Kyoon;Shim, Hyun-Woo;Lee, Chan-Gi;Choi, Hee-Lack;Hong, Hyun Seon
    • Journal of the Korean Crystal Growth and Crystal Technology
    • /
    • v.28 no.5
    • /
    • pp.211-216
    • /
    • 2018
  • The recovery of rare earth elements (REE) including La, Nd and Ce from spent batteries is important issues to reuse scarce resources. Herein, we present a simple recovery process to obtain lanthanum oxide ($La_2O_3$) from spent Ni-MH batteries, and demonstrate the conversion mechanism from $NaLa(SO_4)_2{\cdot}H_2O$ to $La_2O_3$. This strategy requires the initial preparation of $NaLa(SO_4)_2{\cdot}H_2O$ and subsequent metathesis reaction with $Na_2CO_3$ at $70^{\circ}C$. This metathesis reaction resulted in the crystalline lanthanum carbonate hydrate ($La_2(CO_3)_3{\cdot}xH_2O$) powder with plate-like morphology. On the basis of TGA result, the $La_2(CO_3)_3{\cdot}xH_2O$ powder was calcined in air at three different temperatures, that is, $300^{\circ}C$, $500^{\circ}C$, and $1000^{\circ}C$. As the calcination temperature increased, the morphology of powder was changed; prism-like ($NaLa(SO_4)_2{\cdot}H_2O$) ${\rightarrow}$ platelike ($La_2(CO_3)_3{\cdot}xH_2O$) ${\rightarrow}$ aggregated irregular shape ($La_2O_3$). Futhermore, XRD results indicated that the crystalline $La_2O_3$ could be synthesized after the metathesis reaction with $Na_2CO_3$, followed by heat-treatment at $1000^{\circ}C$, along with a change of crystallographic structures; $NaLa(SO_4)_2{\cdot}H_2O$ ${\rightarrow}$ $La_2(CO_3)_3{\cdot}xH_2O$ ${\rightarrow}$ $La_2O_3$.

Structural and optical properties of TiO2 thin films prepared by Sol-Gel dip coating method (졸-겔 침지코팅법으로 제조된 TiO2 박막의 구조적.광학적 특설)

  • 김동진;이학준;한성홍;김의정
    • Korean Journal of Optics and Photonics
    • /
    • v.13 no.3
    • /
    • pp.197-203
    • /
    • 2002
  • The TiO$_2$ coating solutions were synthesized with different concentrations (T1-0.7N, T2-2.0N) of hydrochloric acid used as catalyst. and TiO$_2$ thin films were prepared by sol-gel dip coating. Their structural and optical properties were examined as a function of calcination temperature. XRD results showed that T1 thin films calcined at 400~80$0^{\circ}C$ had the anatase phase, while those calcined at 100$0^{\circ}C$ had the rutile phase. T2 thin films calcined at 40$0^{\circ}C$ and $600^{\circ}C$ had the anatase phase, with the rutile phase for calcination at 80$0^{\circ}C$. Crystallinity of T2 thin films was superior to that of T1 thin films. The crystallite size of TiO$_2$ thin films increased with increasing calcination temperature, and the crystallite size of anatase phase in T2 thin films was larger than that in T1 thin films, but the crystallite size of rutile phase in T2 thin films was smaller. The surface morphology of the films showed that the films were formed more densely in the rutile phase than in the anatase phase, this phenomenon appeared conspicuously in T2 thin films. The transmittance of the samples with thin films on quartz glass calcined at 100$0^{\circ}C$ was significantly reduced at wavelength range about 300-700 nm due to the increased absorption originating from the change of crystallite phase and composition of the films and the scattering effect originating from increasing crystallite size. The refractive index of TiO$_2$ thin films increased, and hence the film thickness as well as the porosity of TiO$_2$ thin films decreased with increasing calcination temperature. Furthermore, the refractive index of T2 thin films was higher than T1 thin films, and porosity of T2 films was lower.

Improved Electrochemical Performance and Minimized Residual Li on LiNi0.6Co0.2Mn0.2O2 Active Material Using KCl (KCl을 사용한 LiNi0.6Co0.2Mn0.2O2계 양극활물질의 잔류리튬 저감 및 전기화학특성 개선)

  • Yoo, Gi-Won;Shin, Mi-Ra;Shin, Tae-Myung;Hong, Tae-Whan;Kim, Hong-kyeong
    • Journal of the Korean Electrochemical Society
    • /
    • v.20 no.1
    • /
    • pp.7-12
    • /
    • 2017
  • Using a precursor of $LiNi_{0.6}Co_{0.2}Mn_{0.2}O_2$ as a starting material, a surface-modified cathode material was obtained by coating with KCl, where the added KCl reduces residual Li compounds such as $Li_2CO_3$ and LiOH, on the surface. The resulting electrochemical properties were investigated. The amounts of $Li_2CO_3$ and LiOH decreased from 8,464 ppm to 1,639 ppm and from 8,088 ppm to 6,287 ppm, respectively, with 1 wt% KCl added $LiNi_{0.6}Co_{0.2}Mn_{0.2}O_2$ that had been calcined at $800^{\circ}C$. X-ray diffraction results revealed that 1 wt% of KCl added $LiNi_{0.6}Co_{0.2}Mn_{0.2}O_2$ did not affect the parent structure but enhanced the development of hexagonal crystallites. Additionally, the charge transfer resistance ($R_{ct}$) decreased dramatically from $225{\Omega}$ to $99{\Omega}$, and the discharge capacity increased to 182.73mAh/g. Using atomic force microscopy, we observed that the surface area decreased by half because of the exothermic heat released by the Li residues. The reduced surface area protects the cathode material from reacting with the electrolyte and hinders the development of a solid electrolyte interphase (SEI) film on the surface of the oxide particles. Finally, we found that the introduction of KCl into $LiNi_{0.6}Co_{0.2}Mn_{0.2}O_2$ is a very effective method of enhancing the electrochemical properties of this active material by reducing the residual Li. To the best of our knowledge, this report is the first to demonstrate this phenomenon.