• Title/Summary/Keyword: Solid state sintering

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Effects of High-Energy Ball Milling and Sintering Time on the Electric-Field-Induced Strain Properties of Lead-Free BNT-Based Ceramic Composites

  • Nga-Linh Vu;Nga-Linh Vu;Dae-Jun Heo;Thi Hinh Dinh;Chang Won Ahn;Chang Won Ahn;Hyoung-Su Han;Jae-Shin Lee
    • Journal of the Korean Institute of Electrical and Electronic Material Engineers
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    • v.36 no.5
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    • pp.505-512
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    • 2023
  • This study investigated crystal structures, microstructures, and electric-field-induced strain (EFIS) properties of Bi-based lead-free ferroelectric/relaxor composites. Bi1/2Na0.82K0.18)1/2TiO3 (BNKT) as a ferroelectric material and 0.78Bi1/2(Na0.78K0.22)1/2TiO3-0.02LaFeO3 (BNKT2LF) as a relaxor material were synthesized using a conventional solid-state reaction method, and the resulting BNKT2LF powders were subjected to high-energy ball milling (HEBM) after calcination. As a result, HEBM proved a larger average grain size of sintered samples compared to conventional ball milling (CBM). In addition, the increased sintering time led to grain growth. Furthermore, HEBM treatment and sintering time demonstrated a significant effect on EFIS of BNKT/BNKT2LF composites. At 6 kV/mm, 0.35% of the maximum strain (Smax) was observed in the HEBM sample sintered for 12 h. The unipolar strain curves of CBM samples were almost linear, indicating almost no phase transitions, while HEBM samples displayed phase transitions at 5~6 kV/mm for all sintering time levels, showing the highest Smax/Emax value of 700 pm/V. These results indicated that HEBM treatment with a long sintering time might significantly enhance the electromechanical strain properties of BNT-based ceramics.

Luminescence Characteristics of ZnGa2O4 Phosphors with the Doped Activator (활성제 첨가에 따른 ZnGa2O4 형광체의 발광특성)

  • Hong Beom-Joo;Choi Hyung-Wook
    • Journal of the Korean Institute of Electrical and Electronic Material Engineers
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    • v.19 no.5
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    • pp.432-436
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    • 2006
  • The $ZnGa_2O_4$ and Mn, Cr-doped $ZnGa_2O_4$ Phosphors were synthesized through conventional solid state reactions. The XRD patterns show that the $ZnGa_2O_4$ has a (3 1 1) main peak and a spinel phase. The emission wavelength of $ZnGa_2O_4$ showed main peak of 420 nm and maximum intensity at the sintering temperature of $1100^{\circ}C$. In the crystalline $ZnGa_2O_4$, the Mn shows green emission (510 nm, $^4T_1-^6A_1$) with a quenching concentration of 0.6 mol%, and the Cr shows red emission (705 nm, $^4T_2-^4A_2$) with a quenching concentration of 2 mol%. These results indicate that $ZnGa_2O_4$ Phosphors hold promise for potential applications in field emission display devices with high brightness operating in full color regions.

Photoluminescence Properties of Green Phosphor Y1-xBO3:Tbx3+ Synthesized by Solid-state Reaction Method (고상 반응법으로 제조한 녹색 형광체 Y1-xBO3:Tbx3+의 형광 특성)

  • Cho, Shin-Ho
    • Journal of the Korean Institute of Electrical and Electronic Material Engineers
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    • v.24 no.8
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    • pp.659-663
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    • 2011
  • [ $Y_{1-x}BO_3:Tb_x^{3+}$ ]ceramic phosphors were synthesized with changing the concentration of $Tb^{3+}$ at a sintering temperature of $1,100^{\circ}C$ and a reduction temperature of $950^{\circ}C$ by using a solid-state reaction method. The crystal structure, surface morphology, and photoluminescence properties of the phosphors were investigated as a function of $Tb^{3+}$ ion concentration by using XRD (x-ray diffractometer), scanning electron microscopy, and photoluminescence spectrophotometry, respectively. The XRD results showed that the main peak of the phosphor powders occurs at (101) plane. As for the photoluminescence properties, the excitation spectra showed the broad band centered at 306 nm and the emission intensity of the spectra peaked at 543 nm indicated a significant decrease as the concentration of $Tb^{3+}$ ion is increased.

Sintering and Electrical Properties of Mn-doped ZnO-$TeO_2$ Ceramics

  • Hong, Youn-Woo;Baek, Seung-Kyoung;Hwang, Hyun-Suk;Shin, Hyo-Soon;Yeo, Dong-Hun;Kim, Jong-Hee
    • Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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    • 2008.06a
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    • pp.49-49
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    • 2008
  • ZnO-based varistors have been widely used for voltage stabilization or transient surge suppression in electric power systems and electronic circuits. Recently, It has reported that the varistor behavior with nonlinear coefficient of 6~17 in Mn-doped ZnO. In this study we have chosen the composition of ZnO-$TeO_2-Mn_3O_4$ (ZTM) system to the purpose of whether varistor behavior appeared in doped ZnO by the solid state sintering or not. We investigated the sintering and electric properties of 0.5~3.0 at% Mn doped ZnO-1.0 at% $TeO_2$ system. Electrical properties, such as current-voltage (I-V), capacitance-voltage (C-V), and impedance spectroscopy were conducted. $TeO_2$ itself melts at $732^{\circ}C$ in air but forms the $ZnTeO_3$ phase with ZnO as increasing temperature and therefore retards the densification of ZnO to $1000^{\circ}C$. The average grain size of sintered samples was at about $3{\mu}m$ and decreased with increasing Mn contents. It was found that a good varistor characteristics were developed in ZTM system sintered at $1100^{\circ}C$ (nonlinear coefficient $\alpha$ ~ 60). The results of C-V characteristics such as barrier height ($\Theta$), donor density ($N_d$), depletion layer (W), and interface state density ($N_t$) in ZTM ceramics were $4\times10^{17}cm^{-3}$, 0.7 V, 40 nm, and $1.6\times10^{12}cm^{-2}$, respectively. It will be discussed about the stability and homogeneity of grain boundaries using distribution parameter ($\alpha$) simulated with the Z(T)"-logf plots in ZTM system.

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Investigation of Spherical LiMn2O4 Cathode Materials by Spray-drying with Different Electrochemical Behaviors at High Rate (분무건조법으로 제조한 구형 스피넬계 LiMn2O4 양극소재의 합성 조건에 따른 고출력 거동에 대한 연구)

  • Song, Jun Ho;Cho, Woosuk;Kim, Young Jun
    • Journal of the Korean Electrochemical Society
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    • v.19 no.2
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    • pp.50-56
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    • 2016
  • Spherical lithium manganese oxide spinel, $Li_{1.10}Mn_{1.86}Al_{0.02}Mg_{0.02}O_4$ was prepared by wet-milling, spray-drying, and sintering process. In the spray-drying process, solid content in slurry was varied from 20 to 30 wt%. In the sintering process, the precursors have been sintered under air or $O_2$ atmosphere. While the as-prepared samples exhibit excellent electrochemical properties at room temperature, the discharge voltage profiles at 5.0C are very different one from another. The origin for the difference especially at initial state of discharge is oxygen defect. The sample prepared in air has larger capacity related to the plateau at 3.3 V (vs. $Li/Li^+$) which is caused by the oxygen defects than the one prepared in $O_2$. The difference of discharge voltage profiles especially at the final state of discharge comes from different diffusion rate of $Li^+$ ions. The sample prepared from 30 wt% solid content of slurry shows twice higher diffusion rate than the samples prepared from 20 wt% solid content, which is attributed to better compactness between primary particles for the sample prepared from 30wt % solid content than the one prepared by 20 wt%.

The Effect of SiO2 on the Microstructure and Electrical Properties of BaTiO3 PTC Thermistor (BaTiO3 PTC 써미스터의 미세구조 및 전기적 특성에 대한 SiO2 영향)

  • Chun, Myoung-Pyo
    • Journal of the Korean Institute of Electrical and Electronic Material Engineers
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    • v.26 no.1
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    • pp.22-26
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    • 2013
  • PTCR ceramics of $(Ba_{0.998}Sm_{0.002})TiO_3+0.001MnCO_3+xSiO_2$ (x=1, 2, 3, 4, 5, 6 mol%) were fabricated by solid state method. Disk samples of diameter 5 mm and thickness about 1mm were sintered at $1,290^{\circ}C$ for 2 h in reduced atmosphere of $5%H_2-95%N_2$ followed by re-oxidation at $600^{\circ}C$ for 30 min. in $20%O_2-80%N_2$.and their microstructures and electrical properties were investigated with SEM and Multimeter. The color of sintered samples was strongly dependent on $SiO_2$ content showing that the color of samples with $SiO_2$ of 1~2 mol% was gray but that of samples with $SiO_2$ of 4~6 mol% was changed from gray to blue, which seems to be related with the reduction of samples due to the oxygen vacancies created during the sintering in reduced atmosphere. $SiO_2$ content had a great influence on the microstructure and the electrical properties. With increasing $SiO_2$ content, the grain size of samples increased and the resistivity as well as the resistivity jump ($R_{285}/R_{min}$) decreased, which is considered to be attributed to the resistivity change at grain interior and grain boundary due to the fast mass transfer through $SiO_2$ liquide phase during the sintering. Samples with 2 mol% $SiO_2$ has the resistivity of $202{\Omega}cm$ and the resistivity jump of 3.28. It is expected that $SiO_2$ doped $BaTiO_3$ based PTC ceramics can be used for multilayered PTC thermistor due to the resistance to the sintering in reduced atmosphere.

Structural and Microwave Dielectric Properties of $Mg_{5}B_{4}O_{15}$ (B=Ta, Nb) Ceramics with Sintering Temperature (소결온도에 따른 $Mg_{5}B_{4}O_{15}$ (B=Ta, Nb) 세라믹스의 구조 및 마이크로파 유전 특성)

  • Kim, Jae-Sik;Choi, Eui-Sun;Lee, Moon-Kee;Ryu, Ki-Won;Lee, Young-Hie
    • Proceedings of the KIEE Conference
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    • 2006.07c
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    • pp.1420-1421
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    • 2006
  • In this study, structural and micowave dielectric properties of the $Mg_{5}B_{4}O_{15}$ (B=Ta, Nb) cation-deficient perovskite ceeramics. The specimens are prepared through the solid-state route. According to the XRD pattern, $Mg_{4}Ta_{2}O_9$ and $MgTa_{2}O_6$ phase exist in calcined and sintered $Mg_{5}Ta_{4}O_{15}$ powder. Also $Mg_{5}Ta_{4}O_{15}$ phase added with increasing sintering temperature. In the case of calcined and sintered $Mg_{5}Nb_{4}O_{15}$ powder, single phase of $Mg_{5}Nb_{4}O_{15}$ were appeared. The bulk density and quality factor of the $Mg_{5}B_{4}O_{15}$ (B=Ta, Nb) ceramics were increased with sinteming temperature in $1400^{\circ}C{\sim}1450^{\circ}C$, but these were decreased in another sintering temperature. Dielectric constant of the $Mg_{5}Ta_{4}O_{15}$ ceramics was increased continuously with increasing of sintering temperature. And the dielectric constant of the $Mg_{5}Nb_{4}O_{15}$ ceramics was increased in $1400^{\circ}C{\sim}1450^{\circ}C$ but decreased in $1475^{\circ}C$. In the case of the $Mg_{5}Ta_{4}O_{15}$ and $Mg_{5}Nb_{4}O_{15}$ ceramics sintered at $1450^{\circ}C$ for 5h, the dielectric constant, quality factor, and temperature coefficient of the resonant frequency (TCRF) were 8.2, 259,473 GHz, -10.91 $ppm/^{\circ}C$ and 14, 37,350 GHz, -52.3 $ppm/^{\circ}C$, respectively.

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A Study on the Synthesis and Consolidation of Ti3Al by Electro-Discharge (전기방전에 의한 Ti3Al의 합성 및 소결 특성 연구)

  • Jang, Hyungsun;Cho, Yujung;Kang, Taeju;Kim, Kibeom;Lee, Wonhee
    • Korean Journal of Metals and Materials
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    • v.47 no.8
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    • pp.488-493
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    • 2009
  • Direct syntheses of bulk $Ti_3Al$ via electro-discharge-sintering (EDS) of a stoichiometric elemental powder mixture were investigated. A capacitor bank of $450{\mu}F$ was charged with three input energies, 0.5, 1.0, and 1.5 kJ. The charged capacitor bank was then instantaneously discharged through 0.3 g of a Ti-25.0 at.%Al powder mixture for consolidation. Complete phase transformation occurred in less than $200{\mu}sec$ by the discharge and a bulk $Ti_3Al$ compact was obtained. Compared with consolidated samples fabricated by conventional methods such as high vacuum sintering and casting, the electro-discharge-sintered $Ti_3Al$ compact shows a very fine microstructure with a hardness value of 425 Hv. Electro-discharge-sintering under a $N_2$ atmosphere successfully modified the surface Ti oxide of the $Ti_3Al$ compact into Ti nitride, which concurred with the synthesis and consolidation of $Ti_3Al$. Complete conversion yielding a single phase $Ti_3Al$ is primarily dominated by the fast solid state diffusion reaction.

A Study on the Microstructures and Ionic Conductivity of Li1.3Al0.3Ti1.7(PO4)3 with Different Synthesis Routes (합성 방법에 따른 Li1.3Al0.3Ti1.7(PO4)3 소결체의 미세 구조 및 이온전도 특성 연구)

  • Seul Ki Choi;Jeawon Choi;MinHo Yang
    • Journal of Powder Materials
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    • v.30 no.2
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    • pp.107-115
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    • 2023
  • Li1.3Al0.3Ti1.7(PO4)3(LATP) is considered a promising material for all-solid-state lithium batteries owing to its high moisture stability, wide potential window (~6 V), and relatively high ion conductivity (10-3-10-4 S/cm). Solid electrolytes based on LATP are manufactured via sintering, using LATP powder as the starting material. The properties of the starting materials depend on the synthesis conditions, which affect the microstructure and ionic conductivity of the solid electrolytes. In this study, we synthesize the LATP powder using sol-gel and co-precipitation methods and characterize the physical properties of powder, such as size, shape, and crystallinity. In addition, we have prepared a disc-shaped LATP solid electrolyte using LATP powder as the starting material. In addition, X-ray diffraction, scanning electron microscopy, and electrochemical impedance spectroscopic measurements are conducted to analyze the grain size, microstructures, and ion conduction properties. These results indicate that the synthesis conditions of the powder are a crucial factor in creating microstructures and affecting the conduction properties of lithium ions in solid electrolytes.

Effect of the Si-C Powder Prepared by Mechanical Alloying on the Densification of Silicon Carbide Powder

  • Yoon, Bola;Lee, Sea-Hoon;Lee, Heesoo;Hwang, Geumchan;Kim, Byungsook
    • Journal of the Korean Ceramic Society
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    • v.53 no.1
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    • pp.99-104
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    • 2016
  • High purity Si-C (99.999%) powder prepared by mechanical alloying was added to a commercial SiC powder as a sintering additive. Reaction bonded silicon carbide balls and jars with high purity (99.98%) were used for the mechanical alloying. As a result, the purity of the sintered Si-C was higher than 99.99%. When sintered at $2200^{\circ}C$ under 50 MPa pressure for 1 h, SiC containing 10 wt% of high purity Si-C showed a relative density of 95.3%, similar to the relative density of commercial SiC (95%). However, the relative density of SiC decreased to 90.6% without the additive when the applied pressure decreased to 40 MPa. In contrast, the relative density was nearly unaffected by the decrease of the pressure when using the Si-C additive. Therefore, the addition of Si-C powder promoted the densification of SiC above $2000^{\circ}C$ under 40 MPa pressure.