• Title/Summary/Keyword: Rietveld

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Mössbauer Studies of Changed Interaction on Cr Ions in Chromite (Chromite 물질의 자기상호작용에 관한 뫼스바우어 분광연구)

  • Choi, Kang-Ryong;Kim, Chul-Sung
    • Journal of the Korean Magnetics Society
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    • v.17 no.1
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    • pp.47-50
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    • 2007
  • [ $ZnCr_2O_4$ ] shows geometrically frustrated magnet. Recently, $CoCr_2O_4$ has been investigated for multiferroic property and dielectric anomalies by spin-current model. Polycrystalline $CoCr_2O_4$ and $CoCrFeO_4$ compounds was prepared by wet-chemical process. Crystallographic and magnetic properties of $CoCr_2O_4$ and $CoCrFeO_4$ were investigate by using the x-ray diffractometer(XRD), vibrating sample magnetometer(VSM), superconducting quantum interference device magnetometer(SQUID), and $M\"{o}ssbauer$ spectroscopy. The crystal structure was found to be single-phase cubic spinel with space group of Fd3m. The lattice constants of $CoCr_2O_4$ and $CoCrFeO_4$ $a_0$ were determined to be 8.340 and 8.377 ${\AA}$, respectively. The ferrimagnetic transition temperature for the both samples were observed at 97 K and 320 K. The $M\"{o}ssbauer$ absorption spectra at 4.2 K show that the well developed two sextets are superposed with small difference of hyperfine field($H_{hf1}=507\;and\;H_{hf2}=492\;kOe$). Isomer shift values($\delta$) of the two sextets are found to be 0.33 and 0.34 mm/s relative to the Fe metal, respectively, which are consistent with the high spin $Fe^{3+}$ charge state.

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.

Effect of Low-grade Limestone on Raw Mill Grinding and Cement Clinker Sintering (저품위 석회석이 원료밀의 분쇄성과 시멘트 클링커 소성성에 미치는 영향)

  • Yoo, Dong-Woo;Park, Tae-Gyun;Choi, Sang-Min;Lee, Chang-Hyun
    • Journal of the Korean Recycled Construction Resources Institute
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    • v.9 no.1
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    • pp.20-25
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    • 2021
  • The cement clinker, the main raw material of cement, is manufactured using limestone as the main material. Depending on the quality of limestone, the use of subsidiary materials changes, and has a great influence on the production of cement clinkers. In this study, the effect of CaO content of limestone, a cement clinker material, on Raw Mill grinding and sintering of cement clinker was investigated. The grinding time of the union materials changed in the content of limestone CaO was measured to identify the grinding properties. The raw material combination was cleaned within a range of 1,350-1,500℃. The sintering performance of cement clinker by Burnability index calculation was identified. The lower the grade of limestone, the lower the grinding quality of the raw material combination. The lower the CaO content of limestone, the greater the variation in F-CaO for sintering temperature. The lower the class of limestone, the higher B. I. value was calculated, indicating the lower cement clinker sintering. In addition, the mineral analysis results of cement clinker showed that if the F-CaO value was low due to the increase in sintering temperature, the Belite content decreased and the Alite content increased. In the case of Alite, the ratio of R-type decreased and that of M-type increased as the content of limestone CaO 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.

Electrochemical Characteristics of LiMn2O4 Cathodes Synthesized from Various Precursors of Manganese Oxide and Manganese Hydroxide (다양한 형태 및 구조의 망간산화물 및 망간수산화물 전구체로부터 합성한 LiMn2O4양극의 전기화학적 특성 연구)

  • Lee, Jong-Moon;Kim, Joo-Seong;Hong, Soon-Kie;Lee, Jeong-Jin;Ahn, Han-Cheol;Cho, Won-Il;Mho, Sun-Il
    • Journal of the Korean Electrochemical Society
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    • v.15 no.3
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    • pp.172-180
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    • 2012
  • The $LiMn_2O_4$ cathodes for lithium ion battery were synthesized from various precursors of manganese oxides and manganese hydroxides. As the first step, nanosized precursors such as ${\alpha}-MnO_2$ (nano-sticks), ${\beta}-MnO_2$ (nano-rods), $Mn_3O_4$ (nano-octahedra), amorphous $MnO_2$(nano-spheres), and $Mn(OH)_2$ (nano-plates) were prepared by a hydrothermal or a precipitation method. Spinel $LiMn_2O_4$ with various sizes and shapes were finally synthesized by a solid-state reaction method from the manganese precursors and LiOH. Nano-sized (500 nm) octahedron $LiMn_2O_4$ showed high capacities of 107 mAh $g^{-1}$ and 99 mAh $g^{-1}$ at 1 C- and 50 C-rate, respectively. Three dimensional octahedral crystallites exhibit superior electrochemical characteristics to the other one-dimensional and two-dimensional shaped $LiMn_2O_4$ nanoparticles. After 500 consecutive charge discharge battery cycles at 10 C-rate with the nano-octahedron $LiMn_2O_4$ cathode, the capacity retention of 95% was observed, which is far better than any other morphologies studied in this work.

The Effect of Non Magnetic ion Substitution for the FeCr2-xMxS4(M=Ga, In) by Mossbauer Spectroscopy (비자성 이온 Ga, In이 치환된 유화물 스피넬의 뫼스바우어 분광학 연구)

  • Son, Bae-Soon;Kim, Sam-Jin;Kim, Chul-Sung
    • Journal of the Korean Magnetics Society
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    • v.16 no.1
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    • pp.6-10
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    • 2006
  • The sulphur spinel $FeCr_{2-x}M_xS_4$(M=Ga, In) have been studied with Mossbauer spectroscopy, x-ray diffraction (XRD), and vibrating sample magnetometer. The XRB patterns for samples $FeCr_{2-x}M_xS_4$(M=Ga, In: x=0.1, 0.3) reveal a single phase, which the Ga and In ions are partially occupied to the tetrahedral (A) site. The Neel temperature for the Ga substituted samples increases from 180 to 188 K, with increase from x=0.1 to 0.3. While, it decreases from 173 to 160 K, for the In substituted samples of the x=0.1 and 0.3, respectively. The Mossbauer spectra were collected from 4.2 K to room temperature. We have analyzed the Mossbauer spectra using eight Lorentzian lines fitting method for the $FeCr_{2-x}In_xS_4$(x=0.1) at 4.2 K, yielding the 1311owing results; $H_{hf}=146.0kOe,\;{\Delta}E_Q=1.88mm/s,\;\theta=36^{\circ},\;\phi=0^{\circ},\;\eta=0.6$, and R=1.9. The Ga ions enter into the both sites octahedral (B) and tetrahedral (A), simultaneously the same amounts of Fe ions migrate from the A to the B site, this result is an agreement with XRD results, too. The ${\Delta}E_Q$ of the A and B site in Mossbauer spectra of the samples $FeCr_{2-x}Ga_xS_4$(x=0.3) are 0.83 and 2.94mm/s, respectively. While they are 0.56 and 2.36mm/s for the $FeCr_{2-x}In_xS_4$(x=0.3). It is noticeable that the ${\Delta}E_Q$ for the Ga doped samples are larger than that of the corresponding In doped samples, in spite of the larger ionic radius for In ions. The bond lengths of Cr-S, for the Ga and In doped samples (x=0.3) are found to be 2.41 and $2.43\;{\AA}$, respectively. We interpret that the larger covalence effect from the smaller bond length induces a large asymmetric charge distribution. Finally, it gives a large quadrupole interaction.

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.