• Title/Summary/Keyword: XRD-Rietveld analysis

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Hydrogen Storage Properties of Hydriding-Dehydriding Cycled Magnesium-Nickel-Iron Oxide Alloy

  • Song, Myoung Youp;Kwon, Sung Nam;Park, Hye Ryoung;Kim, Byoung-Goan
    • Korean Journal of Metals and Materials
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    • v.50 no.2
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    • pp.171-175
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    • 2012
  • By measuring the absorbed hydrogen quantity as a function of the number of cycles, the cycling properties of the Mg-15 wt%Ni-5 wt%$Fe_2O_3$ alloy were investigated. The absorbed hydrogen quantity decreased as the number of cycles increased. The $H_a$ value varied almost linearly with the number of cycles. The maintainability of absorbed hydrogen quantity at n=100 was 89.0% for the hydriding reaction time of 10 min. After the $150^{th}$ hydriding-dehydriding cycle, Mg, $Mg_2Ni$, $Mg(OH)_2$, MgO, and Fe were observed. The phases were analyzed by Rietveld analysis from the XRD patterns of the Mg-15 wt%Ni-5 wt%$Fe_2O_3$ alloy after 150 hydriding-dehydriding cycles. The crystallite size and strain of Mg were then estimated with the Williamson-Hall technique.

A Quantitative Study for Hydrothermal Alteration Zones using Short Wavelength Infrared Spectrometry (단파장적외선 분광분석법을 이용한 열수변질대 정량화 연구)

  • Kim, Yong-Hwi;Choi, Seon-Gyu;Ko, Kwang-Beom;Han, Kyeong-Soo;Koo, Min-Ho
    • Economic and Environmental Geology
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    • v.50 no.1
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    • pp.15-26
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    • 2017
  • Advanced argillic, argillic, and phyllic zones are the most important alteration patterns to predict the hidden ore body during exploration of hydrothermal deposits. We examined the quantitative relationship between the spectral absorption characteristics and the mineral content of the synthetic mixtures such as alunite-kaolinite and illite-kaolinite using short wavelength infrared (SWIR) spectroscopy. In the alunite-kaolinite mixtures, the spectral absorption characteristics of the alunite was highly correlated with the Hull quotient reflectance(0.99) and the kaolinite had the highest correlation with the Gaussian peak(0.92). Illite-kaolinite mixtures are essential for Gaussian deconvolution because of the overlap of absorption region. Illite and kaolinite mixtures indicate the high correlation of 0.93 and 0.98, respectively. The error ranges in the alunite-kaolinite(8%) and illite-kaolinite mixtures(5%) derived from SWIR were smaller than the ones(29% and 26%) obtained from X-ray diffraction(Rietveld) analysis. These results show that SWIR spectroscopic analysis is more reliable than XRD Rietveld analysis in terms of quantification of allowed minerals.

Layered Metal Hydroxides Containing Calcium and Their Structural Analysis

  • Kim, Tae-Hyun;Heo, Il;Paek, Seung-Min;Park, Chung-Berm;Choi, Ae-Jin;Lee, Sung-Han;Choy, Jin-Ho;Oh, Jae-Min
    • Bulletin of the Korean Chemical Society
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    • v.33 no.6
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    • pp.1845-1850
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    • 2012
  • Layered metal hydroxides (LMHs) containing calcium were synthesized by coprecipitation in solution having two different trivalent metal ions, iron and aluminum. Two mixed metal solutions ($Ca^{2+}/Al^{3+}$ and $Ca^{2+}/Fe^{3+}$ = 2/1) were added to sodium hydroxide solution and the final pH was adjusted to ~11.5 and ~13 for CaAl-and CaFe-LMHs. Powder X-ray diffraction (XRD) for the two LMH samples showed well developed ($00l$) diffractions indicating 2-dimensional crystal structure of the synthesized LMHs. Rietveld refinement of the X-ray diffraction pattern, the local structure analysis through X-ray absorption spectroscopy, and thermal analysis also confirmed that the synthesized precipitates show typical structure of LMHs. The chemical formulae, $Ca_{2.04}Al_1(OH)_6(NO_3){\cdot}5.25H_2O$ and $Ca_{2.01}Fe_1(OH)_6(NO_3){\cdot}4.75H_2O$ were determined by inductively coupled plasma-atomic emission spectroscopy (ICP-AES). Particle morphology and thermal behavior for the synthesized LMHs were examined by field emission scanning electron microscopy and thermogravimetricdifferential scanning calorimetry.

Physical and Chemical Properties of Cement Mortar with Gamma-C2S

  • Lee, Sung-Hyun;Kim, Kyungnam;Mabudo, Mabudo;Song, Myong-Shin
    • Journal of the Korean Ceramic Society
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    • v.53 no.2
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    • pp.194-199
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    • 2016
  • Presently, for the cement industry, studies that seek to reduce $CO_2$, because of the development of the plastic industry and demand for reduction of energy use, have been actively conducted among them, studies attempting to use Gamma-$C_2S({\gamma}-C_2S)$ to fix $CO_2$ have been actively conducted. The ${\gamma}-C_2S$ compound has an important function in reacting to $CO_2$ and stiffening through carbonatization in the air. The ${\gamma}-C_2S$ compound, reacting to $CO_2$ in the air, generates $CaCO_2$ within the pore structure of cement materials and densifies the pore structure this leads to an improvement of the durability and to the characteristic of resistance against neutralization. Therefore, in this experiment, in order to synthesize ${\gamma}-C_2S$, limestone sludge and waste foundry sands are used these materials are plasticized for 30 or 60 minutes at $1450^{\circ}C$, and are prevented from being cooled in the temperature range of $30{\sim}1000^{\circ}C$ when they are about to be cooled. XRD analysis and XRF analysis are used to determine the effects of this process on ${\gamma}-C_2S$ synthesization, the temperature at which a thing is plasticized, and the conditions for cooling that obtain in the plasticized clinker also, in order to confirm the $CO_2$ capture function, analysis of the major hydration products is conducted through an analysis of carbonatization depth and compressive strength, and through MIP analysis and XRD Rietveld analysis. As a result of these analyses, it is found that when ${\gamma}-C_2S$ was synthesized, the clinker that was plasticized at $1450^{\circ}C$ for one hour demonstrated the highest yield rate the sample with which the ${\gamma}-C_2S$ was mixed generated $CaCO_3$ when it reacted with $CO_2$ therefore, carbonatization depth and porosity were reduced, and the compressive strength was increased.

Applied-Mineralogical Characterization and Assessment of Some Domestic Bentonites (I): Mineral Composition and Characteristics, Cation Exchange Properties, and Their Relationships (국내산 벤토나이트에 대한 응용광물학적 특성 평가 (I): 광물 조성 및 특징과 양이온 교환특성과의 연계성)

  • 노진환
    • Journal of the Mineralogical Society of Korea
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    • v.15 no.4
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    • pp.329-344
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    • 2002
  • Mineralogical and chemical characterization of some domestic bentonites, such as quantitative XRD analysis, chemical leaching experiments, pH and CEC determinations, were done without any separation procedures to understand their relationships among mineral composition, characteristics, and cation exchange properties. XRD quantification results based on Rietveld method reveal that the bentonites contain totally more than 25 wt% of impurities, such as zeolites, opal-CT, and feldspars, in addition to montmorillonite ranging 30~75 wt%. Cation exchange properties of the zeolitic bentonites are deeply affected by the content of zeolites identified as clinoptilolite-heulandite series. Clinoptilolite is common in the silicic bentonites with lighter color. and occurs closely in association with opal-CT. Ca is mostly the dominant exchangeable cation, but some zeolitic bentonites have K as a major exchangeable cation, The values of cation exchange capacity (CEC) determined by Methylene Blue method are comparatively low and have roughly a linear relationship with the montmorillonite content of the bentonite, though the correlated data tend to be rather dispersed. Compared to this, the CEC determined by Ammonium Acetate method, i.e.‘Total CEC’, has much higher values (50~115 meq/100 g). The differences between those CEC values are much greater in zeolitic bentonites, which obviously indicates the CEC increase affected by zeolite. Other impurities such as opal-CT and feldspars seem to affect insignificantly on the CEC of bentonites. When dispersed in distilled water, the pH of bentonites roughly tends to increase up to 9.3 with increasing the alkali abundance, especially Na, in exchangeable cation composition. However, some bentonites exhibit lower pH (5~6) so as to regard as ‘acid clay’. This may be due to the presence of $H^{+}$ in part as an exchangeable cation in the layer site of montmorillonite. All the works of this study ultimately suggest that an assesment of domestic bentonites in grade and quality should be accomplished through the quantitative XRD analysis and the ‘Total CEC’measurement.

Study on Burnability and Reactivity of High Al2O3 Content OPC Clinker for the Use of Industrial Waste (산업부산물 활용을 위한 고Al2O3 함량 OPC 클링커의 소성성 및 반응성에 관한 연구)

  • Kang, Bong-Hee;Choi, Jaewon;Ki, Tae-Kyoung;Kwon, Sang-Jin;Kim, Gyu-Yong
    • Journal of the Korean Recycled Construction Resources Institute
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    • v.8 no.3
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    • pp.294-301
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    • 2020
  • This study evaluated the burnability and hydration reaction of clinker burned with high Al2O3 content OPC to apply large amounts of industrial by-products in the cement manufacturing process. Specifically, after preparing a clinker with a high C3A content by burning the OPC raw material with a high content of Al2O3 in a laboratory electric furnace, the burnability of the clinker was evaluated through XRD Rietveld analysis and polarization microscopy, and clinker hydration reactivity was reviewed through the Isothermal conduction calorimetry analysis and the cement compressive strength. As a result, the kiln burning temperature for the production of high Al2O3 content clinker lower, and the compressive strength was equal to or higher than OPC. Therefore it was confirmed the possibility to manufacturing energy-saving high Al2O3 content clinker using a large amount of industrial by-products.

Structures and Electrochemical Properties of LiNi0.5-xCo2x}Mn0.5-xO2 as Cathode Materials for Lithium-ion Batteries

  • Choi, Hyun-Chul;Kim, Ho-Jin;Jeong, Yeon-Uk;Jeong, Soo-Hwan;Cheong, In-Woo;Jung, Uoo-Chang
    • Bulletin of the Korean Chemical Society
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    • v.30 no.11
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    • pp.2603-2607
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    • 2009
  • $LiNi_{0.5-x}Co_{2x}Mn_{0.5-x}O_{2}$ (x = 0, 0.1, 1/6, 1.2, 0.3) were synthesized by the solid-state reaction method. The crystal structure was analyzed by X-ray powder diffraction and Rietveld refinement. $LiNi_{0.5-x}Co_{2x}Mn_{0.5-x}O_{2}$ samples give single phases of hexagonal layered structures with a space group of R-3m for x = 0.1, 1/6, 0.2, and 0.3. The lattice constants of a and c-axis were decreased with the increase in Co contents in samples. The thickness of MO2 slab was decreased and inter-slab distance was increased with the increase in Co contents in $LiNi_{0.5-x}Co_{2x}Mn_{0.5-x}O_{2}$. According to XPS analysis, the valence states of Mn, Co, and Ni in the sample are mainly +4, +3, and +3, respectively. The discharge capacity of 202 mAh/g at 0.1C-rate in the potential range of 4.7 - 3.0 V was obtained in $LiNi_{0.3}Co_{0.4}Mn_{0.3}O_2$ sample, and $LiNi_{0.4}Co_{0.2}Mn_{0.4}O_2$ gives excellent cycle performance in the same potential range.

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.

Crystal structure refinement and microwave dielectric characteristic of $(1-x)CaTiO_3-x(La_{1/3}Nd_{1/3})TiO_3$ ($(1-x)CaTiO_3-x(La_{1/3}Nd_{1/3})TiO_3$계의 결정구조 해석 및 마이크로파 유전 특성)

  • 조남웅;성경필;문종하;최주현
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.8 no.3
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    • pp.478-486
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    • 1998
  • $CaTiO_3-x(La_{1/3}Nd_{1/3}TiO_3\;(0\le \textrm x\le0.8)$ system was prepared by reaction of $CaCO_3,\;LaO_3,\;Nd_2CO_3$ and ,TEX>$TiO_2$ mixture at 1673 K, which can be applied for microwave dielectric ceramic materials. The lattice parameters of(1-x))$CaTiO_3-x(La_{1/3}Nd_{1/3}TiO_3\;(0\le \textrm x\le0.8)$ system increased with the increase of x. Its structure was investigated by Rietveld profile-analysis of XRD in detail. Cations $ La^{3+}$ and Nd^{3+}$ were located at the $Ca^{2+}$ site in the range of $0\le \textrm x\le0.8$. crystal structure in $;(0\le \textrm x\le0.6)$ maintained space group Pnma with CaTiO_3 structure. The tiled and distorted $TiO_6$ was gradually released with the increase of x in $0\le \textrm x\le0.6$ .The structure was changed to a new space group of $Pmn2_1$ at the x value of 0.8. The relative dielectric constant $(\epsilon_r)$ of $(1-x)CaTiO_3-x(La_{1/3} Nd_{1/3})TiO_3$ ($(0\le \textrm x\le0.8)$) system was exponentially decreased by with the increased of x. The temperature coefficient of resonant frequency $(\tau_f)$ decreased with the increase of x in $0\le \textrm x\le0.6$ and then increased again at x=0.8 due to the change of crystal structure. The value of Q$\cdot f_o$ was 13800 (GHz) at x=0.2 and was very low under 2000 (GHz) in 0.4$\leq$x$\leq$0.8.

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Characterization of Synthesized Carbonate and Sulfate Green Rusts: Formation Mechanisms and Physicochemical Properties (합성된 탄산염 및 황산염 그린 러스트의 형성 메커니즘과 이화학적 특성 규명)

  • Lee, Seon Yong;Choi, Su-Yeon;Chang, Bongsu;Lee, Young Jae
    • Korean Journal of Mineralogy and Petrology
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    • v.35 no.2
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    • pp.111-123
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    • 2022
  • Carbonate green rust (CGR) and sulfate green rust (SGR) commonly occur in nature. In this study, CGR and SGR were synthesized through co-precipitation, and their formation mechanisms and physicochemical properties were investigated. X-ray diffraction (XRD) and Rietveld refinement showed both CGR and SGR with layered double hydroxide structure were successfully synthesized without any secondary phases under each synthetic condition. Refined structural parameters (unit cell) for two green rusts were a (=b) = 3.17 Å and c = 22.52 Å for CGR and a (=b) = 5.50 Å and c = 10.97 Å for SGR with the crystallite size 57.8 nm in diameter from (003) reflection and 40.1 nm from (001) reflections, respectively. Scanning electron microscopy/energy dispersive X-ray spectroscopy (SEM/EDS) results showed that both CGR and SGR had typical hexagonal plate-like crystal morphologies but their chemical composition is different in the content of C and S. In addition, Fourier transform infrared (FT-IR) spectroscopy analysis revealed that carbonate (CO32-) and sulfate (SO42-) molecules were occupied as interlayer anions of CGR and SGR, respectively. These SEM/EDS and FT-IR results were in good agreement with XRD results. Changes in the solution chemistry (i.e., pH, Eh and residual iron concentrations (Fe(II):Fe(III)) of the mixed solution) were observed as a function of the injection time of hydroxyl ion (OH-) into the iron solution. Three different stages were observed in the formation of both CGR and SGR; precursor, intermediator, and green rust in the formation of both CGR and SGR. This study provides co-precipitation methods for CGR and SGR in a way of the stable synthesis. In addition, our findings for the formation mechanisms of the two green rusts and their physicochemical properties will provide crucial information with researches and industrials in utilizing green rust.