• Title/Summary/Keyword: spinel phase

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Analysis of microstructure for glass-ceramics made of silicate glasses containing EAF dust (제강분진이 첨가된 규산염계 결정화유리의 미세구조 분석)

  • Kim, H.S.;Kang, S.G.
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.16 no.5
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    • pp.227-234
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    • 2006
  • Microstructures of free surface and interior of glass-ceramics obtained by heat treating silicate glass specimen containing electric arc furnace dust(EAF dust) were observed. The crystallization temperature, $T_c$ of glassy specimen was measured around $850^{\circ}C$ from the result of different thermal analysis so heat treatment temperature to obtain glass-ceramic specimen was selected as $950^{\circ}C$ for 1 hr. Glass specimens containing 50 wt% dust were amorphous, while glass specimens containing 70 wt% dust showed spinel crystal peaks in XRD results. In case of glass-ceramic specimens, spinel crystalline phase was appeared with willemite, and willemite crystal peak intensity increased with increasing dust contents. The fractured surface of glass specimens containing 50 wt% dust was smooth like mirror surface, but that containing 70 wt% dust showed spinel crystals of 10 ${\mu}m$ size in glass matrix. In case of glass-ceramic specimens, ZnO crystal particles of $2{\sim}5{\mu}m$ size were produced in free surface and glassy phase, spinel and willemite crystal phases existed in interior. There were no crystals in glasses containing 50 wt% dust, while glass containing 70 wt% dust had 14 vol% crystals. Crystallinity of glass-ceramic specimens containing 50 and 70 wt% dust were 19 and 43%, respectively. When microstructures of glass and glass-ceramic specimens were observed through SEM after TCLP experiment, glass specimens showed flaking phenomenon while glass-ceramic specimens showed a slight corrosion evidence without any cracks.

The Oxidation of Kovar in Humidified $N_2$/H$_2$ Atmosphere (가습된 $N_2$/H$_2$혼합가스 분위기에서의 Kovar 산화 거동)

  • 김병수;김민호;김상우;최덕균;손용배
    • Journal of the Microelectronics and Packaging Society
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    • v.8 no.2
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    • pp.1-7
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    • 2001
  • In order to form a uniform oxidation layer of spinel phase on Kovar which helps the strong bonding in Kovar-to-glass sealing, the humidified $N_2/H_2$ was used as an oxidation atmosphere. The oxidation of Kovar was controlled by diffusion mechanism and the activation energy was 31.61 kacl/mol at 500~$800^{\circ}C$. After oxidation at $600^{\circ}C$, the external oxidation layer was below 0.5 $\mu \textrm{m}$ thick. According to TEM analysis, oxidized Kovar was spinel its lattice parameter of 7.9 $\AA$. Oxidation of under $600^{\circ}C$ and in a humidified $N_2/H_2$ atmosphere, Kovar was found to be appropriate for the Kovar-to-glass sealing.

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Phase Equilibria of the Ferrous Ferrite System of $(Mg_{0.29}-yMnyFe_{0.71})_{3-}\delta$O_4$ ($(Mg_{0.29}-yMnyFe_{0.71})_{3-}\delta$O_4$ 훼라이트계의 상평형)

  • 채정훈;유한일;강선호;강대석;유병두
    • Journal of the Korean Ceramic Society
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    • v.32 no.3
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    • pp.394-402
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    • 1995
  • Electrical conductivity and thermoelectric power of the ferrous ferrite system of (Mg0.29-yMnyFe0.71)3-$\delta$O4 have been measured as function of the thermodynamic variables, cationic composition(y), temperature(T) and oxygen partial pressure(Po2) under thermodynamic equilibrium conditions at elevated temperatures. On the basis of the electrical properties-phase stability correlation, the stability regions of the ferrite spinel and its neighboring phases have been subsequently located in the log Po2 vs. y and log Po2 vs. 1/T planes in the ranges of 0 y 0.29, 1100 T/$^{\circ}C$ 1400 and 10-14 Po2/atm 1. The stability region, Δlog Po2(y, 1/T), of the ferrite spinel single phase widens with increasing Mn-content(y) and the boundaries of each region are linear against 1/T with negative slopes.

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Properties and Synthesis of Porous Cordierite from Fly Ash (플라이 애쉬를 이용한 다공성 코디어라이트의 합성 및 특성)

  • Kim, Sung-Jin;Bang, Hee-Gon;Park, Sang-Yeup
    • Journal of the Korean Ceramic Society
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    • v.43 no.6 s.289
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    • pp.344-350
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    • 2006
  • Porous cordierite was synthesized by the mechano-chemical processing using fly ash. The phase evolution of cordierite was investigated as a function of processing variables such as milling time and sintering temperature. In this study, the phase transition path of cordierite from fly ash was followed by sapprine/spinel ${\to}$ mullite/spinel ${\to}{\alpha}$-cordierite. Porous cordierite fabricated after 32 h of milling time and sintering at $1150^{\circ}C$ showed relatively low thermal expansion coefficient ($2.5{\times}10^{-6}/^{\circ}C\;(25{\sim}1000^{\circ}C$)) and high porosity (75%).

Phase Transitions of $LiMn_2O_4$ on $CO_2$ Decomposition (($CO_2$ 분해시 $LiMn_2O_4$의 상변화)

  • Kwoen, Tae-Hwan;Yang, Chun-Mo;Park, Young-Goo;Cho, Young-Koo;Rim, Byung-O
    • Journal of the Korean Applied Science and Technology
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    • v.20 no.1
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    • pp.33-43
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    • 2003
  • $LiMn_2O_4$ catalyst for $CO_2$ decomposition was synthesized by oxidation method for 30 min at 600$^{\circ}C$ in an electric furnace under air condition using manganese(II) nitrate $(Mn(NO_3)_2{\cdot}6H_2O)$, Lithium nitrate ($LiNO_3$) and Urea $(CO(NH_2)_2)$. The synthesized catalyst was reduced by $H_2$ at various temperatures for 3 hr. The reduction degree of the reduced catalysts were measured using the TGA. And then $CO_2$ decomposition rate was measured using the reduced catalysts. Phase-transitions of the catalysts were observed after $CO_2$ decomposition reaction at an optimal decomposition temperature. As the result of X-ray powder diffraction analysis, the synthesized catalyst was confirmed that the catalyst has the spinel structure, and also confirmed that when it was reduced by $H_2$, the phase of $LiMn_2O_4$ catalyst was transformed into $Li_2MnO_3$ and $Li_{1-2{\delta}}Mn_{2-{\delta}}O_{4-3{\delta}-{\delta}'}$ of tetragonal spinel phase. After $CO_2$ decomposition reaction, it was confirmed that the peak of $LiMn_2O_4$ of spinel phase. The optimal reduction temperature of the catalyst with $H_2$ was confirmed to be 450$^{\circ}C$(maximum weight-increasing ratio 9.47%) in the case of $LiMn_2O_4$ through the TGA analysis. Decomposition rate(%) using the $LiMn_2O_4$ catalyst showed the 67%. The crystal structure of the synthesized $LiMn_2O_4$ observed with a scanning electron microscope(SEM) shows cubic form. After reduction, $LiMn_2O_4$ catalyst became condensed each other to form interface. It was confirmed that after $CO_2$ decomposition, crystal structure of $LiMn_2O_4$ catalyst showed that its particle grew up more than that of reduction. Phase-transition by reduction and $CO_2$ decomposition ; $Li_2MnO_3$ and $Li_{1-2{\delta}}Mn_{2-{\delta}}O_{4-3{\delta}-{\delta}'}$ of tetragonal spinel phase at the first time of $CO_2$ decomposition appear like the same as the above contents. Phase-transition at $2{\sim}5$ time ; $Li_2MnO_3$ and $Li_{1-2{\delta}}Mn_{2-{\delta}}O_{4-3{\delta}-{\delta}'}$ of tetragonal spinel phase by reduction and $LiMn_2O_4$ of spinel phase after $CO_2$ decomposition appear like the same as the first time case. The result of the TGA analysis by catalyst reduction ; The first time, weight of reduced catalyst increased by 9.47%, for 2${\sim}$5 times, weight of reduced catalyst increased by average 2.3% But, in any time, there is little difference in the decomposition ratio of $CO_2$. That is to say, at the first time, it showed 67% in $CO_2$ decomposition rate and after 5 times reaction of $CO_2$ decomposition, it showed 67% nearly the same as the first time.

Study of the Electrochemical Properties of Li4Ti5O12 Doped with Ba and Sr Anodes for Lithium-Ion Secondary Batteries

  • Choi, Byung-Hyun;Lee, Dae-Jin;Ji, Mi-Jung;Kwon, Young-Jin;Park, Sung-Tae
    • Journal of the Korean Ceramic Society
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    • v.47 no.6
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    • pp.638-642
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    • 2010
  • The spinel material $Li_4Ti_5O_{12}$ has attracted considerable attention as an anode electrode material for many battery applications owing to its light weight and high energy density. However, the real capacity of $Li_4Ti_5O_{12}$ powder as determined by the solid-state method is lower than the ideal capacity. In this study, we investigated the effect of the dopants in M-doped spinel $Ba_xLi_{4-2x}Ti_5O_{12}$(x=0.005, 0.05, 0.1) powders prepared by the solid-state reaction method and used as the anode material in lithiumion batteries. The results confirmed the effect of the Ba and Sr dopants on the powder properties of the spinel $Li_4Ti_5O_{12}$, which exhibited a pure spinel structure without any secondary phase in its XRD pattern. Moreover, the electrochemical properties of the spinel M-LTO materials were investigated using a half cell. The electrochemical data show that cells with anodes made of undoped $Li_4Ti_5O_{12}$ and Ba- and Sr-doped $Li_4Ti_5O_{12}$ have discharge capacities of 97, 130, and 112 mAh/g, respectively, at the first cycle. Moreover, the Ba- and Sr-doped spinel $Li_4Ti_5O_{12}$ demonstrated good properties in the mid-voltage range at 1.55 V, showing stable cyclic voltammogram properties which surpassed those of the same material without Ba or Sr at 1 C after 100 cycles.

A study on the Spinel phase cathode materials with high capacity for lithium secondary batteries (리튬 2차 전지용 고용량 스피넬계 양극물질 연구)

  • Hong, Ki-Joo;Sun, Yang-Kook
    • Proceedings of the KIEE Conference
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    • 2001.11b
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    • pp.106-108
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    • 2001
  • As 3V cathode material, a new doping spinel material, LiMn1.6Se0.4O4 powder with a phase-pure polycrystalline was synthesized by a sol-gel method. In spite of Jahn-teller distortion in 3V region($2.4{\sim}3.5V$), the LiMn1.6Se0.4O4 electrode shows no capacity loss. The material in the 3V region initially delivers a discharge capacity of 100mAh/g which increase with cycling to reach 105mAh/g after 90cycles. And 5V cathode material LiNi0.5-xMxMn1.5O4(M=Cr, V, Fe) compounds have been synthesized by sol-gel method. a series of electroactive spinel compounds, LiNi0.5-xMxMn1.5O4(M=Cr, V, Fe) has been studied by crystallographic and electrochemical methods. The material presents only one plateau at around 4.5 V vs. Li/Li+ with a large discharge capacity of 152mAh/g and fairly good cyclability.

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Behavior of $Sb_2O_3$ in the Calcination Process of ZnO Varistor (ZnO 바리스터의 하소과정에서 $Sb_2O_3$의 거동)

  • Choi, Jin Seog;Mah, Jae Pyung;Paek, Su-Hyon
    • Journal of the Korean Institute of Telematics and Electronics
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    • v.24 no.3
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    • pp.433-438
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    • 1987
  • The current-voltage characteristics of the ZnO varisor with and without Sb2O3 which were fabricated with the various calcination and sintering temperature were discussed by comparing the results of SEM-microstructures and X-ray diffraction analysis. The samples were calcined at the temperature up to 800\ulcorner for 2 hours and they were sintered at 1200-1300\ulcorner for 1 hour. Then, we applied the power up to dc 200 volt to the samples and measured the output current up to 100mA. The samples without Sb2O3 had lower nonlinear resistances at the all calcination and sintering temperatures due to the large grains because of not forming Spinel phase. The other samples contained Sb2O3 could form Pyrochlore and Spinel phases at the all calcination temperatures by X-ray diffraction phase analysis. We found that the Spinel phases which were formed at the calcination process inhibit growth of ZnO grain and give rise to the change of nonlinear resistances by SEM-microstructures. And we found that the base of ZnO grain growth control is strongly dependent on the behavior of Sb2O3 in calcination process.

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