• Title/Summary/Keyword: Calcination reaction

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Hydrothermal Synthesis and Mechanical Characterization of 3mol%Y2O3-ZrO2 by Urea Contents (우레아 첨가량 변화에 따라 수열합성법으로 제조 된 3mol%Y2O3-ZrO2 분말의 합성 및 기계적 특성 평가)

  • Lee, Hak-Joo;Go, Myung-Won;Kim, Taik-Nam
    • Korean Journal of Materials Research
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    • v.21 no.8
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    • pp.425-431
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    • 2011
  • The industrial manufacturing of YSZ products can be summarized as a three step process: a) hydrolysis of zirconyl chloride and mixing of other solutions, b) precipitation, and c) calcination. The addition of ammonia or OH- is essential in the precipitation process. However, a strong agglomeration was observed in the results of an ammonia or OH- addition. Thus, it is necessary to disperse the powders smoothly in order to improve the mechanical strength of YSZ. In this study, YSZ was synthesized using the urea stabilizer and hydrothermal method. YSZ powders were synthesized using a hydrothermal method with Teflon Vessels at $180^{\circ}C$ for 24 h. The mole ratio of urea to Zr was 0, 0.5, 1, and 2. The crystal phase, particle size, and morphologies were analyzed. Rectangular specimens ($33\;mm{\times}8\;mm{\times}1{\pm}0.5\;mm$) for three-point bend tests were used in the mechanical properties evaluation. The crystalline of YSZ powders observed a tetragonal phase in the sample with a ratio of Zr:urea = 1:2 addition and a hydrothermal reaction time of 24 h. The average primary particle size of YSZ was measured to be 9 nm to 11 nm. The agglomerated particle size was measured from 15 nm to 30 nm. The three-point bending strength of the YSZ samples was 142.47 MPa, which is the highest value obtained for the Zr:urea = 1:2 ratio addition YSZ sample.

Synthesis and Spectroscopic Characterization of Vanadium-Incorporated V-AlMCM-48 Mesoporous Material (바나듐이 들어있는 Mesoporous V-AlMCM-48 분자체의 합성 및 분광학적 특성 조사)

  • Back, Gernho;Yu, Jong-Sung;Park, Sung-Kun;Lee, Chul Wee;Won, Taejin
    • Korean Chemical Engineering Research
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    • v.44 no.4
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    • pp.369-374
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    • 2006
  • A solid-state reaction of $V_2O_5$ with AlMCM-48 followed by calcination generated very weak paramagnetic $VO^{2+}$ species in the mesoporous material. Dehydration and subsequent reduction with CO result in the formation of vanadyl $VO^{2+}$ species that can be characterized by EPR. The chemical environment of vanadium centers in $VO^{2+}-AlMCM-48$ was investigated by XRD, EDX, DR-UV-Vis, EPR,$^{29}Si$ and $^{27}Al$ and $^{51}V$ NMR. Vanadium species in MCM-48 are existed as pseudotetrahedral $VO^{2+}$ state when they were dehydrated or reduced with CO. The coordination of water on vanadyl ions transformed their structure to distorted octahedral.

Photocatalytic Degradation of a Congo red Using ZnO/rutile-$TiO_2$, ZnO, rutile-$TiO_2$ and CdS (ZnO/rutile-$TiO_2$, ZnO, rutile-$TiO_2$, CdS를 이용한 Congo red의 광 촉매 분해반응)

  • Kim, Chang Suk;Ryu, Hae-Ill
    • Analytical Science and Technology
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    • v.14 no.3
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    • pp.259-265
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    • 2001
  • Photocatalytic degradation of Congo red was performed using various semiconductors as ZnO, CdS, rutile-$TiO_2$ or mixed rutile-$TiO_2$/ZnO. The change of degradation of the dye was investigated by UV-visible spectrophotometric method. The photocatalytic action of CdS was greater than ZnO and rutile-$TiO_2$ in account of low band gap energy of CdS. The rate of photocatalytic degradation reaction increased drastically in according to increasing ratio of ZnO on mixed rutile-$TiO_2$/ZnO. These photocatalytic effect of rutile-$TiO_2$ was suppressed by more stable rutile-$TiO_2$, doping the hydrolysis product with $Zn^{2+}$ prior to calcination onto the rutile-$TiO_2$ surface.

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Characteristics of Ni1/3Co1/3Mn1/3(OH)2 Powders Prepared by Co-Precipitation in Air and Nitrogen Atmospheres (공기와 질소 분위기에서 공침법으로 합성된 Ni1/3Co1/3Mn1/3(OH)2 분말의 특성 비교)

  • Choi, Woonghee;Park, Se-Ryen;Kang, Chan Hyoung
    • Journal of Powder Materials
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    • v.23 no.2
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    • pp.136-142
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    • 2016
  • As precursors of cathode materials for lithium ion batteries, $Ni_{1/3}Co_{1/3}Mn_{1/3}(OH)_2$ powders are prepared in a continuously stirred tank reactor via a co-precipitation reaction between aqueous metal sulfates and NaOH in the presence of $NH_4OH$ in air or nitrogen ambient. Calcination of the precursors with $Li_2CO_3$ for 8 h at $1,000^{\circ}C$ in air produces dense spherical cathode materials. The precursors and final powders are characterized by X-ray diffraction (XRD), scanning electron microscopy, particle size analysis, tap density measurement, and thermal gravimetric analysis. The precursor powders obtained in air or nitrogen ambient show XRD patterns identified as $Ni_{1/3}Co_{1/3}Mn_{1/3}(OH)_2$. Regardless of the atmosphere, the final powders exhibit the XRD patterns of $LiNi_{1/3}Co_{1/3}Mn_{1/3}O_2$ (NCM). The precursor powders obtained in air have larger particle size and lower tap density than those obtained in nitrogen ambient. NCM powders show similar tendencies in terms of particle size and tap density. Electrochemical characterization is performed after fabricating a coin cell using NCM as the cathode and Li metal as the anode. The NCM powders from the precursors obtained in air and those from the precursors obtained in nitrogen have similar initial charge/discharge capacities and cycle life. In conclusion, the powders co-precipitated in air can be utilized as precursor materials, replacing those synthesized in the presence of nitrogen injection, which is the usual industrial practice.

Effects of Precursor Co-Precipitation Temperature on the Properties of LiNi1/3Co1/3Mn1/3O2 Powders (전구체 공침 온도가 LiNi1/3Co1/3Mn1/3O2 분말의 특성에 미치는 영향)

  • Choi, Woonghee;Kang, Chan Hyoung
    • Journal of Powder Materials
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    • v.23 no.4
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    • pp.287-296
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    • 2016
  • $Ni_{1/3}Co_{1/3}Mn_{1/3}(OH)_2$ powders have been synthesized in a continuously stirred tank reactor via a co-precipitation reaction between aqueous metal sulfates and NaOH using $NH_4OH$ as a chelating agent. The co-precipitation temperature is varied in the range of $30-80^{\circ}C$. Calcination of the prepared precursors with $Li_2CO_3$ for 8 h at $1000^{\circ}C$ in air results in Li $Ni_{1/3}Co_{1/3}Mn_{1/3}O_2$ powders. Two kinds of obtained powders have been characterized by X-ray diffraction (XRD), scanning electron microscopy, particle size analyzer, and tap density measurements. The co-precipitation temperature does not differentiate the XRD patterns of precursors as well as their final powders. Precursor powders are spherical and dense, consisting of numerous acicular or flaky primary particles. The precursors obtained at 70 and $80^{\circ}C$ possess bigger primary particles having more irregular shapes than those at lower temperatures. This is related to the lower tap density measured for the former. The final powders show a similar tendency in terms of primary particle shape and tap density. Electrochemical characterization shows that the initial charge/discharge capacities and cycle life of final powders from the precursors obtained at 70 and $80^{\circ}C$ are inferior to those at $50^{\circ}C$. It is concluded that the optimum co-precipitation temperature is around $50^{\circ}C$.

A Study on the Simultaneous Oxidation of $CH_4$ and CO over $Pd/TiO_2$ Catalyst ($Pd/TiO_2$ 촉매를 이용한 $CH_4$, CO의 동시산화 연구)

  • Lee, Hyun Hee;Jang, Du Hun;Hong, Sung Chang
    • Applied Chemistry for Engineering
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    • v.23 no.3
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    • pp.253-258
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    • 2012
  • The effects of active sites and valence states were investigated over $Pd/TiO_2$ catalyst on simultaneous oxidation of $CH_4$ and CO. The Pd species (PdO) crystallite size increased with increasing Pd loadings, which results in enhancement of the activity of $CH_4$ oxidation. Different results from the activity of $CH_4$ and CO oxidation were shown to be dependent on the Pd valence state on the surface of the catalyst prepared through a thermal treatment. XRD and $H_2-TPR$ analysis confirmed that $Pd^{2+}$species was predominated in the calcination catalyst, while $Pd^0$species was predominated in the reduction catalyst. Additionally, it could be found that the valence state of Pd was a more important factor on the catalytic activity than that of factors as the surface area and pore volume. The reaction mechanism of $CH_4$ and CO followed by the valence state of Pd could be identified using FT-IR analysis.

Study on the Selective CO Oxidation Using $La_xCe_{1-x}Co_yCu_{1-y}O_{3-{\alpha}}$ Perovskite Catalysts ($La_xCe_{1-x}Co_yCu_{1-y}O_{3-{\alpha}}$ Perovskite촉매의 선택적 CO 산화반응에 관한 연구)

  • Kang, Dae-Kyu;Lee, Young-Il;Sohn, Jung-Min
    • Transactions of the Korean hydrogen and new energy society
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    • v.18 no.1
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    • pp.32-39
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    • 2007
  • CO oxidation and selective CO oxidation of $La_xCe_{1-x}Co_yCu_{1-y}O_{3-{\alpha}}$ perovskite(x=1, 0.9, 0.7. 0.5; y=1, 0.9, 0.7, 0.5) were investigated. For CO oxidation, catalytic activities were studied according to different preparation conditions such as pH and calcination temperature. The influence of the change of the $O_2$ concentration for selective CO oxidation was studied, too. The substitution of Ce for La improved the catalytic activity for CO oxidation and selective CO oxidation and best activity was observed for $La_{0.7}Ce_{0.3}CoO_3$ prepared at pH 11 and calcined at $600^{\circ}C$. The temperature of 90% CO conversion for CO oxidation using $La_{0.7}Ce_{0.3}CoO_3$ was $230^{\circ}C$. In contrast to the enhancement effect by Ce substitution, the partial substitution of Cu for Co in $LaCo_yCu_{1-y}O_{3-{\alpha}}$ decreased catalytic activities for CO oxidation reaction compared to that using $LaCoO_3$. For selective CO oxidation, the best CO conversion was 66% at $230^{\circ}C$ for $La_{0.7}Ce_{0.3}CoO_3$. The CO conversion of $La_{0.7}Ce_{0.3}CoO_3$ was greatly increased from 66% to 91% as increasing $O_2$ concentration from 1% to 2%.

Synthesis and Characterization of Fe-Co/mesoHZSM-5 : Effect of Desilication Agent and Iron-cobalt Composition

  • Jimmy, Jimmy;Roesyadi, Achmad;Suprapto, Suprapto;Kurniawansyah, Firman
    • Korean Chemical Engineering Research
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    • v.58 no.1
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    • pp.163-169
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    • 2020
  • Synthesis of Fe-Co/meso-HZSM5 catalyst, intended to be applied in Fischer-Tropsch (FT) reaction was investigated. The study emphasized the effect of desilication agents, NaOH and KOH, on the catalyst materials properties. Impregnation composition of active metal (Fe and Co) was also examined. HZSM-5, converted from ammonium ZSM-5 through calcination, was treated with NaOH and KOH for desilication, followed by impregnation with 10% metal loading. Fe composition in the initial mixture was varied at 10-50% from total composition. After impregnation, reduction was applied by flowing hydrogen gas at 400 ℃ for 10 hours. The use of KOH solution induced greater mesoporous volumes; however, it had a detrimental effect on zeolite crystal structure. NaOH solutions, on the other hand, increased mesopore area as high as 100%, indicated from surface area increase from 266.28 m2/g of HZSM-5, to 526.03 m2/g of NaOH-desilicated HZSM-5. In addition, the application of NaOH solution increased pore volume from 0.14 cc/g to 0.486 cc/g. Further, more Fe-Co alloys and less oxide of iron (Fe2O3) as well cobalt (Co3O4) had been commonly observed in the produced catalysts. The largest Fe-Co alloys could be found in 50Fe-50Co/HZSM-5

Evaluation of Magnesia Cement Using MgCO3 and Serpentine (MgCO3와 사문석을 사용한 마그네시아 시멘트의 특성평가)

  • Lee, Jong-Kyu;Soh, Jung-Sub;Chu, Yong-Sik;Song, Hun;Park, Ji-Sun
    • Korean Journal of Materials Research
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    • v.22 no.11
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    • pp.598-603
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    • 2012
  • MgO based cement for the low-temperature calcination of magnesite required less energy and emitted less $CO_2$ than the manufacturing of Portland cements. Furthermore, adding reactive MgO to Portland-pozzolan cement can improve their performance and also increase their capacity to absorb atmospheric $CO_2$. In this study, the basic research for magnesia cement using $MgCO_3$ and magnesium silicate ore (serpentine) as starting materials was carried out. In order to increase the hydration activity, $MgCO_3$ and serpentinite were fired at a temperature higher than $600^{\circ}C$. In the case of $MgCO_3$ as starting material, hydration activity was highest at $700^{\circ}C$ firing temperature; this $MgCO_3$ was completely transformed to MgO after firing. After the hydration reaction with water, MgO was totally transformed to $Mg(OH)_2$ as hydration product. In the case of using only $MgCO_3$, compressive strength was 35 $kgf/cm^2$ after 28 days. The addition of silica fume and $Mg(OH)_2$ led to an enhancements of the compressive strength to 55 $kgf/cm^2$ and 50 $kgf/cm^2$, respectively. Serpentine led to an up to 20% increase in the compressive strength; however, addition of this material beyond 20% led to a decrease of the compressive strength. When we added $MgCl_2$, the compressive strength tends to increase.

La0.8Ca0.2CrO3 Interconnect Materials for Solid Oxide Fuel Cells: Combustion Synthesis and Reduced-Temperature Sintering

  • Park, Beom-Kyeong;Lee, Jong-Won;Lee, Seung-Bok;Lim, Tak-Hyoung;Park, Seok-Joo;Song, Rak-Hyun;Shin, Dong-Ryul
    • Journal of Electrochemical Science and Technology
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    • v.2 no.1
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    • pp.39-44
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    • 2011
  • Sub-micrometer $La_{0.8}Ca_{0.2}CrO_3$ powders for ceramic interconnects of solid oxide fuel cells were synthesized by the aqueous combustion process. The materials were prepared from the precursor solutions with different glycine (fuel)-to-nitrate (oxidant) ratios (${\phi}$). Single-phase $La_{0.8}Ca_{0.2}CrO_3$ powders with a perovskite structure were obtained after combustion when ${\phi}$ was equal to or larger than 0.480. Especially, the stoichiometric precursor with ${\phi}$ = 0.555 yielded the spherical $La_{0.8}Ca_{0.2}CrO_3$ particles with 150-250 nm diameters after calcination at $1000^{\circ}C$. When compared with the powders synthesized by the solid-state reaction, the combustion-derived, fine powders exhibited improved sinterability, leading to near-full densification at $1400^{\circ}C$ in oxidizing atmospheres. Moreover, a small quantity of glass additives was used to reduce the sintering temperature, and considerable densification was indeed achieved at temperatures as low as $1100^{\circ}C$.