• Title/Summary/Keyword: Solid state route

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Dielectric and Piezoelectric Properties of Alkaline Lead-free Piezoceramic-epoxy Composites (알칼리계 무연 압전 세라믹과 에폭시 복합소재의 유전 및 압전 특성)

  • Yoon, Chang-Ho;Le, Duc Thang;Heo, Dae-Jun;Ahn, Kyoung-Kwan;Lee, Jae-Shin
    • Journal of the Korean Institute of Electrical and Electronic Material Engineers
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    • v.25 no.6
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    • pp.420-425
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    • 2012
  • Lead-free piezoelectric ceramic/epoxy composites with '0-3' connectivity were prepared by cold-pressing with a temperature controlled curing method. A ceramic powder with a composition of $(Na_{0.51}K_{0.47}Li_{0.02})(Nb_{0.8}Ta_{0.2})O_3$ was synthesized by a conventional solid state reaction route. The dielectric and piezoelectric properties of ceramic/epoxy composites were characterized as a function of the volume fraction (${\phi}$) of piezoelectric ceramics, which was varied from 70 to 95 vol%. The results indicated that the piezoelectric properties of composites were significantly affected by the volume fraction of ceramics. In terms of the piezoelectric properties, specimens showed the best performance at ${\phi}$= 85 vol%, resulting in the piezoelectric constant $d_{33}$ of 39 pC/N and the figure of merit as a piezoelectric energy harvester ($d_{33}{\cdot}g_{33}$) of 1.24 $pm^2/N$.

Size Tailored Nanoparticles of ZrN Prepared by Single-Step Exothermic Chemical Route

  • Lee, Sang-Ki;Park, Kyung-Tae;Ryu, Hong-Youl;Nersisyan, Hayk H.;Lee, Kap-Ho;Lee, Jong-Hyeon
    • Korean Journal of Materials Research
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    • v.22 no.5
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    • pp.243-248
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    • 2012
  • ZrN nanoparticles were prepared by an exothermic reduction of $ZrCl_4$ with $NaN_3$ in the presence of NaCl flux in a nitrogen atmosphere. Using a solid-state combustion approach, we have demonstrated that the zirconium nitride nanoparticles synthesis process can be completed in only several minutes compared with a few hours for previous synthesis approaches. The chemistry of the combustion process is not complex and is based on a metathesis reaction between $ZrCl_4$ and $NaN_3$. Because of the low melting and boiling points of the raw materials it was possible to synthesize the ZrN phase at low combustion temperatures. It was shown that the combustion temperature and the size of the particles can be readily controlled by tuning the concentration of the NaCl flux. The results show that an increase in the NaCl concentration (from 2 to 13 M) results in a temperature decrease from 1280 to $750^{\circ}C$. ZrN nanoparticles have a high surface area (50-70 $m^2/g$), narrow pore size distribution, and nano-particle size between 10 and 30 nm. The activation energy, which can be extracted from the experimental combustion temperature data, is: E = 20 kcal/mol. The method reported here is self-sustaining, rapid, and can be scaled up for a large scale production of a transition metal nitride nanoparticle system (TiN, TaN, HfN, etc.) with suitable halide salts and alkali metal azide.

Crystal Structure and Microstructure Variation of Nonstoichiometric Bi1±xFeO3±δ and Ti-doped BiFeO3 Ceramics under Various Sintering Conditions (비화학양론적 Bi1±xFeO3±δ와 Ti가 첨가된 BiFeO3의 소결조건에 따른 결정구조와 미세구조 변화)

  • Bae, Jihee;Kim, Jun Chan;Kim, Myong-Ho;Lee, Soonil
    • Korean Journal of Materials Research
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    • v.30 no.2
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    • pp.61-67
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    • 2020
  • BiFeO3 with perovskite structure is a well-known material that has both ferroelectric and antiferromagnetic properties called multiferroics. However, leaky electrical properties and difficulty of controlling stoichiometry due to Bi volatility and difficulty of obtaining high relative density due to high dependency on the ceramic process are issues for BiFeO3 applications. In this work we investigated the sintering behavior of samples with different stoichiometries and sintering conditions. To understand the optimum sintering conditions, nonstoichiometric Bi1±xFeO3±δ ceramics and Ti-doped Bi1.03Fe1-4x/3TixO3 ceramics were synthesized by a conventional solid-state route. Dense single phase BiFeO3 ceramics were successfully fabricated using a two-step sintering and quenching process. The effects of Bi volatility on microstructure were determined by Bi-excess and Ti doping. Bi-excess increased grain size, and Ti doping increased sintering temperature and decreased grain size. It should be noted that Ti-doping suppressed Bi volatility and stabilized the BiFeO3 phase.

Dielectric Properties of Cation-deficient Perovskite Ceramics and Oscillator Application (Cation-deficient 페로브스카이트 세라믹스의 유전 특성과 발진기 응용)

  • Kim, Jae-Sik;Choi, Eui-Sun;Ryu, Ki-Won;Lee, Young-Hie
    • Proceedings of the KIEE Conference
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    • 2006.10a
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    • pp.18-19
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    • 2006
  • In this study, dielectric properties of the ${Mg_5}{B_4}{O_{15}}$ (B=Ta, Nb) cation-deficient perovskite ceramics and its oscillator application are investigated. The cation-deficient perovskite ceramics are prepared through the solid-state route. According to the XRD pattern, ${Mg_4}{Ta_2}{O_9}$ and $Mg{Ta_2}{O_6}$ phase existed 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 ${Mg_5}{Nb_4}{O_{15}}$ is appeared. 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, $-10.91ppm/^{\circ}C$ and 14, 37,350 GHz, $-52.3\;ppm/^{\circ}C$, respectively. Simulated DR with ${Mg_5}{Ta_4}{O_{15}}$ ceramics had the operating frequency of 10.99 GHz and S(2,1) of -29.795 dB. Size of manufactured oscillator was $56{\times}48{\times}34\;mm^3 and operated at 11.93 GHz. Power output and second harmonic of oscillator were +13.61 dBm and -23.81 dBc at 23.85 GHz, respectively.

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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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Effect of BaF2 as a Flux in Solid State Synthesis of Y3Al5O12:Ce3+ (고상법을 이용한 Y3Al5O12:Ce3+의 제조에서 BaF2가 미치는 영향)

  • Won, Hyung-Seok;Hayk, Nersisyan;Won, Chang-Whan;Won, Hyung-Il
    • Korean Journal of Materials Research
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    • v.21 no.11
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    • pp.604-610
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    • 2011
  • The effect of $BaF_2$ flux in $Y_3Al_5O_{12}:Ce^{3+}$(YAG:Ce) formation was investigated. Phase transformation of $Y_3Al_5O_{12}$(YAG) was characterized by using XRD, SEM, and TEM-EDS, and it was revealed that the sequential formation of the $Y_4Al_2O_9$(YAM), $YAlO_3$(YAP) and $Y_3Al_5O_{12}$(YAG) in the temperature range of 1000-1500$^{\circ}C$. Single phase of YAG was revealed from 1300$^{\circ}C$. In order to find out the effect of $BaF_2$ flux, three modeling experiments between starting materials (1.5$Al_2O_3$-2.5$Y_2O_3$, $Y_2O_3$-$BaF_2$, and $Al_2O_3$-$BaF_2$) were done. These modeling experiments showed that the nucleation process occurs via the dissolution-precipitation mechanism, whereas the grain growth process is controlled via the liquid-phase diffusion route. YAG:Ce phosphor particles prepared using a proposed technique exhibit a spherical shape, high crystallinity, and an emission intensity. According to the experimental results conducted in this investigation, 5% of $BaF_2$ was the best concentration for physical, chemical and optical properties of $Y_3Al_5O_{12}:Ce^{3+}$(YAG:Ce) that is approximately 10-15% greater than that of commercial phosphor powder.

Dielectric and Electrical Characteristics of Lead-Free Complex Electronic Material: Ba0.8Ca0.2(Ti0.8Zr0.1Ce0.1)O3

  • Sahu, Manisha;Hajra, Sugato;Choudhary, Ram Naresh Prasad
    • Korean Journal of Materials Research
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    • v.29 no.8
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    • pp.469-476
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    • 2019
  • A lead-free bulk ceramic having a chemical formula $Ba_{0.8}Ca_{0.2}(Ti_{0.8}Zr_{0.1}Ce_{0.1})O_3$ (further termed as BCTZCO) is synthesized using mixed oxide route. The structural, dielectric, impedance, and conductivity properties, as well as the modulus of the synthesized sample are discussed in the present work. Analysis of X-ray diffraction data obtained at room temperature reveals the existence of some impurity phases. The natural surface morphology shows close packing of grains with few voids. Attempts have been made to study the (a) effect of microstructures containing grains, grain boundaries, and electrodes on impedance and capacitive characteristics, (b) relationship between properties and crystal structure, and (c) nature of the relaxation mechanism of the prepared samples. The relationship between the structure and physical properties is established. The frequency and temperature dependence of the dielectric properties reveal that this complex system has a high dielectric constant and low tangent loss. An analysis of impedance and related parameters illuminates the contributions of grains. The activation energy is determined for only the high temperature region in the temperature dependent AC conductivity graph. Deviation from the Debye behavior is seen in the Nyquist plot at different temperatures. The relaxation mechanism and the electrical transport properties in the sample are investigated with the help of various spectroscopic (i.e., dielectric, modulus, and impedance) techniques. This lead free sample will serve as a base for device engineering.

Surface morphology and deuterium retention in W and W-HfC alloy exposed to high flux D plasma irradiation

  • Yongkui Wang;Xiaochen Huang;Jiafeng Zhou;Jun Fang;Yan Gao;Jinlong Ge;Shu Miao;Zhuoming Xie
    • Nuclear Engineering and Technology
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    • v.55 no.2
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    • pp.575-579
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    • 2023
  • In this work, pure W and W-0.5wt%HfC alloy (WHC05) were fabricated by sintering and hot-rolling following the same processing route. After exposing to a high flux deuterium plasma irradiation with the D+ flux to three fluences of 6.00 × 1024, 2.70 × 1025 and 7.02 × 1025 D/m2, the evolution of surface morphology, deuterium retention and hardening behaviors in pure W and WHC05 has been studied. The SEM results show the formation of D blisters on the irradiated area, and with the increase of D implantation, the size of these blisters increases from 200 ~ 500 nm (2.70 × 1025 D/m2) to 1 ~ 2 ㎛ (7.02 × 1025 D/m2) in WHC05 and from 1 ~ 2 ㎛ (2.70 × 1025 D/m2) to > 3 ㎛ (7.02 × 1025 D/m2) in pure W, respectively. A higher D retention and obvious hardening are observed in pure W than that of the WHC05 alloy, indicating an improve radiation resistance in WHC05 compared to pure W.

Synthesis of Organized $TiO_2$ Electrodes Using Graft Copolymer and Their Applications to Dye-Sensitized Solar Cells (가지형 공중합체를 이용한 나노구조 $TiO_2$ 제조 및 염료감응 태양전지 응용)

  • Ahn, Sung Hoon;Koh, Joo Hwan;Park, Jung Tae;Kim, Jong Hak
    • 한국신재생에너지학회:학술대회논문집
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    • 2010.06a
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    • pp.64.1-64.1
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    • 2010
  • The morphology of mesoporous $TiO_2$ films plays an important role in the operation of a DSSC. For example, the energy conversion efficiency of DSSCs with well-organized mesoporous $TiO_2$ films is much higher than those with traditional films possessing a random morphology. In previous research, well-organized mesoporous $TiO_2$ films have mainly been synthesized using an amphiphilic block copolymer, e.g., a poly(ethylene oxide) (PEO)-based template. A graft copolymer is more attractive than a block copolymer due to its low cost and the ease with which it can be synthesized. In this work, we provide the first report on the successful synthesis of well-organized mesoporous $TiO_2$ films templated by an organized graft copolymer as a structure directing agent. Well-organized mesoporous $TiO_2$ films with excellent channel connectivities were developed via the sol gel processusing an organized PVC-g-POEM graft copolymer synthesized by one-pot ATRP. The careful adjustment of copolymer composition and solvent affinity using a THF/$H_2O$/HCl mixture was used to systematically vary the material structure. The influence of the material structure on solar cell performance was then investigated. A solid-state DSSC employing both the graft copolymer templated organized 700 nm-thick $TiO_2$ films and graft copolymer electrolytes exhibited a solar conversion efficiency of 2.2% at 100 $mW/cm^2$. This value was approximately two-fold higher than that attained from a DSSC employing a random mesoporous $TiO_2$ film. The solar cell performance was maximized at 4.6% when the film thickness was increased to $2.5{\mu}m$. We believe that this graft copolymer-directed approach introduces a new and simple route toward the synthesis of well-organized metal oxide films as an alternative to a conventional block copolymer-based template.

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Synthesis and Electrochemical Properties of Zn and Al added LiNi0.85Co0.15O2 Cathode Materials (Zn와 Al을 첨가한 LiNi0.85Co0.15O2 양극활물질의 제조 및 전기화학적 특성평가)

  • Kim, Su-Jin;Seo, Jin-Seong;Na, Byung-Ki
    • Korean Chemical Engineering Research
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    • v.59 no.1
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    • pp.42-48
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    • 2021
  • Zn and Al added LiNi0.85Co0.15O2 cathode materials were synthesized to improve electrochemical properties and thermal stability using a solid-state route. Crystal structure, particle size and surface shape of the synthesized cathode materials was measured using XRD (X-ray diffraction) and SEM (scanning electron microscopy). CV (cyclic voltammetry), first charge-discharge profiles, rate capability, and cycle life were measured using battery cycler (Maccor, series 4000). Strong binding energy of Al-O bond enhanced structure stability of cathode material. Electrochemical properties were improved by preventing cation mixing between Li+ and Ni2+. Large ion radius of Zn+ increased lattice parameter of NC cathode material, which meant unit-cell volume was expanded. NCZA25 showed 80% of capacity retention at 0.5 C-rate during 100 cycles, which was 12% higher than that of NC cathode. The discharge capacity of NCZA25 showed 104 mAh/g at 5 C-rate. NCZA25 achieved 36 mAh/g more capacity than that of NC cathod. NCZA25 cathode material showed excellent rate capability and cycling performance.