• Korean Journal of Materials Research
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• v.11 no.3
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• pp.178-184
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• 2001

Transparent and highly oriented KLN thin films have been grown by an rf- magnetron sputtering deposition method. A homogeneous and stable KLN target was prepared by calcine and sintering process. For KLN target, stoichiometry and composition excess with K of 30% and 60%, and Li of 15% and 30% respectively, was prepared. The targets were sintered at low temperature to prevent vaporization of K and Li. KLN thin films were fabricated by rf-magnetron sputtering method using those targets. In this experiment, using the target of composition excessed with K of 60% and Li of 30%, single phase KLN thin film was produced. KLN thin film has excellent crystallinity and highly c-axis oriented on Corning 1737 substrate. Transmittance of thin film in visible range was 90%, absorption edge is 333 nm and refractive index at 632.8 nm was 1.93.

• Journal of the Korean Institute of Electrical and Electronic Material Engineers
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• v.24 no.9
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• pp.723-727
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• 2011

0.935Ba$TiO_3$-0.065($Bi_{0.5}Na_{0.5}$)$TiO_3+xmol%MnO_2$ (BBNTM-x) ceramics with $0{\leq}x{\leq}0.05$ were fabricated with muffled sintering by a modified synthesis process. Their microstructure and enhanced positive temperature coefficient of resistivity (PTCR) characteristics were systematically investigated in order to obtain lead-free high TC PTCR thermistors. All specimens showed a perovskite structure with a tetragonal symmetry and no secondary phase was observed. Grain growth was achieved when the doped MnO2 was increased above 0.02 mol%. This is due to the effect of positive Mn ion doping as an acceptor compensating a Ba vacancy occurred by the higher donor dopant concentration of $Bi^{3+}$ ion. Especially, enhanced PTCR characteristics of the extremely low ${\rho}_{RT}$ of $9\;{\Omega}{\cdot}cm$, PTCR jump of $5.1{\times}10^3$, ${\alpha}$ of 15.5%/$^{\circ}C$ and high $T_C$ of $167^{\circ}C$ were achieved for the BBNTM-0.04 ceramics.

• Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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• 2007.11a
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• pp.295-295
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• 2007

기계적 에너지를 전기적 에너지로 변화하는 에너지 변환소자인 압전 세라믹스는 액츄에이터, 변압기, 초음파모터, 초음파 소자 및 각종 센서로 응용되고 있으며, 그 응용분야는 크게 증가하고 있다. 최근 이러한 에너지 변화 소자는 앞으로 도래하는 ubiquitous, 무선 모바일 시대의 휴대용 전자제품, robotics, 항공우주, 자동차, 의료, 건축, MEMS 분야 등의 대체 에너지원으로 응용하기 위한 연구가 진행되고 있다. 특히 인간의 동작 등과 같은 일상적인 동작으로 필요한 전력을 얻을 수 있고, 세라믹 소자를 이용하기 때문에 전자노이즈가 발생되지 않을 뿐 아니라 반영구적으로 사용할 수가 있어서, 기존 이차전지, 연료전지를 대체 또는 보완 할 수 있는 방안도 검토되고 있다. PZT계 세라믹스는 높은 유전상수와 압전특성으로 전자세라믹스분야에서 가장 널리 사용되어지고 있지만 $1200^{\circ}C$이상의 높은 소결온도 때문에 $1000^{\circ}C$ 부근에서 급격히 휘발되는 PbO로 인한 환경오염과 기본조성의 변화로 인한 압전 특성의 저하가 문제시되고 있다. 또한, 적층 세라믹스의 제작 시 구조적 특성상 내부 전극이 도포된 상태에서 동시 소결이 필요한데, 융점이 낮은 Ag전극 대신 값비싼 Pd나 Pt가 다량 함유된 Ag/Pd, Ag/Pt 전극이 사용되고 있어 경제적인 문제가 발생하게 된다. 따라서 순수 Ag 전극을 사용하거나, Ag의 비율이 높은 내부 전극을 사용하기 위해서는 $950^{\circ}C$ 이하에서 소결되는 압전 세라믹스를 개발 하는 것이 필요하다. 따라서 본 연구에서는 압전특성이 우수한 $(Pb_{1-x}Cd_x)\;[(Ni_{1/3}/Nb_{2/3})_{0.25}Zr_{0.35}Ti_{0.4}]O_3$계의 조성을 설계하여, 소결온도를 낮추기 위해서 2단계 하소법을 이용하였다. 분말을 ball milling을 통해 24시간 동안 혼합하였다. 혼합된 분말은 $800^{\circ}C$에서 2시간 동안 하소하였다. 하소한 분말을 72시간 동안 ball milling 하여 최종 분말을 얻었다. 최종 분말에 PVB를 첨가하여 ${\Phi}21$ disk 형태로 성형한 후, $800{\sim}950^{\circ}C$ 소결을 하였다. 최종 분말 및 소결된 시편을 XRD분석을 통하여 상을 확인하였고, SEM을 이용하여 미세조직을 관찰하였다. 전기적 특성을 확인하기 위하여 두께 1mm로 연마한 시편에 Ag 전극을 도포하여 열처리한 후, 분극 처리하였다. 압전특성은 $d_{33}$ 미터로 측정하였고, impedance analyzer를 이용하여 주파수 및 impedance 특성을 측정하였다. 그 결과 $900^{\circ}C$에서 우수한 압전 특성 및 전기적 특성을 확보 할 수 있었다.

• Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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• 2004.07a
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• pp.138-141
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• 2004

[ $MnO_2$ ]가 첨가된 $0.9Pb(Zr_{0.5}Ti_{0.5})O_3-0.2Pb[(Zn_{0.8}Ni_{0.2})_{1/3}Nb_{2/3}]O_3$(0.8PZT-0.2PZNN) 세라믹스는 그 압전특성과 유전특성이 뛰어나지만 $1000^{\circ}C$ 이하의 낮은 소결 온도에서는 소결되지 않는다. $1000^{\circ}C$이하의 낮은 소결온도에서 소결하기 위해 CuO를 첨가한 결과, 소결온도 $920^{\circ}C$에서 소결성은 우수하였으나 그 압전 특성의 저하가 두드러졌다. 이는 XRD에서 확인한 결과에 따르면 CuO의 첨가가 우수한 MPB 조성으로 판명된 $MnO_2$ 가 첨가된 0.8PZT-0.2PZNN 세라믹스의 결정구조를 Rhombohedral 구조로 바꾸기 때문인 것으로 보였으며 이러한 문제는 PZNN의 비율을 조절하여 0.875PZT-0.125PZNN 세라믹스를 선택함으로 인해 해결할 수 있었다. 그러나 여전히 낮은 $Q_m$값을 높이기 위해서 $Al_2O_3$를 첨가하였고 그 결과 시편의 tetragonality 감소와 $Q_m$값의 증가를 확인할 수 있었으나 그 첨가량이 0.2wt% 이상일 경우에는 밀도의 감소로 인한 압전특성의 저하가 나타났다. 밀도의 향상을 위해 Zn and Ni excess 조성을 선택하였고 그 결과 0.5wt% $MnO_2$와 0.2wt% CuO 그리고 0.3wt% $Al_2O_3$를 첨가한 0.875PZT-0.125PZNN 세라믹스(Zn and Ni excess 조성)를 $920^{\circ}C$에서 소결한 경우 $k_p=0.581,\;Q_m=809,\;d_{33}=345\;pC/N\;and\;{\varepsilon}_{33}/{\varepsilon}_0=1345$의 빼어난 압전 및 유전특성과 $330^{\circ}C$의 높은 $T_c$를 보였고 그 조성의 vibration velocity는 약4.5 m/s로 나타났다.

• Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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• 2005.07a
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• pp.363-364
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• 2005

LTCC(low temperature co-fired ceramics)용 glass/ceramic 복합체를 제조하기 위해 3종류 의 glass를 선정하고 filler로 $Al_2O_3$ 와 $TiO_2$를 사용하여 glass frit에 따른 소결 및 유전 특성에 대하여 조사하였다. Glass frit은 lead-borosilicate(PBS), zinc-borosilicate(ZBS), bismuth-borosilicate(BBS) glass 조성을 사용하였고 1100~$1400^{\circ}C$에서 melting시킨 후 quenching하여 frit화하였다. $Al_2O_3$와 $TiO_2$ filler에 10~50 vol%로 glass frit을 각각 혼합한 후 600~$950^{\circ}C$에서 2시간 동안 소결한 결과 50 vol% glass frit 일 때 $900^{\circ}C$ 이하에서 소성이 가능하였다. 유전특성은 $900^{\circ}C$에서 $Al_2O_3$-50vol%PBS($\varepsilon_{r}$=8.8, $Q{\times}f_o$=4,900, $\tau_f$=-24), $Al_2O_3$-50vol% ZBS($\varepsilon_{r}$=5.7, $Q{\times}f_o$=17,800, $\tau_f$=-21), $Al_2O_3$-50vol%BBS($\varepsilon_{r}$=11.1, $Q{\times}f_o$= 2,080, $\tau_f$=-48), $TiO_2$-50vol%PBS($\varepsilon_{r}$=18.6, $Q{\times}f_o$=3,800, $\tau_f$=+135), $TiO_2$-50vol%ZBS($\varepsilon_{r}$=36.4, $Q{\times}f_o$= 7,500, $\tau_f$=+159), $TiO_2$-50vol%BBS($\varepsilon_{r}$=56.4, $Q{\times}f_o$=520, $\tau_f$=+119)을 나타내었다. 따라서 LTCC용 기판재료 및 마이크로파 유전체로 응용이 가능한 것으로 확인되었다.

• Applied Chemistry for Engineering
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• v.32 no.6
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• pp.632-639
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• 2021

In this research, fluorine doping was performed to enhance the photocatalytic activities of WO₃ which were measured using methylene blue dye. WO_3-xF_x photocatalyts were prepared by a vaper phase fluorination during a sintering for preparing WO₃ photocatalysts from a WCl₆ precursor. The bandgap energy of WO₃ photocatalysts decreased from 2.95 eV to 2.54 eV, and the oxygen vacancies site increased by about 55% after fluorine doping. In addition, the initial degradation efficiency of methylene blue showed that the fluorine doped sample showed a 6-fold increase in photocatalytic activities from 10% to 60% compared to that of the untreated sample. It is believed that fluorine is doped to reduce the band gap of photocatalysts, enabling the catalytic activity with low energy, and that oxygen vacancies-generated surface defects increase the visible light absorption region of WO₃ photocatalysts, thereby increasing photocatalytic activity. In this study, it was confirmed that fluorine-doped WO_3-xF_x photocatalysts with an excellent photocatalytic activity can be manufactured easily using a one-step vaper phase fluorination that does not require a post-treatment process.

• Nuclear Engineering and Technology
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• v.52 no.12
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• pp.2860-2866
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• 2020

Oxide dispersion-strengthened materials W-1wt%Pr₂O₃ and W-1wt%La₂O₃ were synthesized by wet chemical method and spark plasma sintering. The field emission scanning electron microscopy (FE-SEM) analysis, XRD and Vickers microhardness measurements were conducted to characterize the samples. The irradiations were carried out with a 5 keV helium ion beam to fluences up to 5.0 × 10²¹ ions/m² under 600 ℃ using the low-energy ion irradiation system. Transmission electron microscopy (TEM) study was performed to investigate the microstructural evolution in W-1wt%Pr₂O₃ and W-1wt%La₂O₃. At 1.0 × 10²⁰ He⁺/m², the average loops size of the W-1wt%Pr₂O₃ was 4.3 nm, much lower than W-1wt% La₂O₃ of 8.5 nm. However, helium bubbles were not observed throughout in both doped W materials. The effects of pre-irradiation with 1.0 × 10²¹ He⁺/m² on trapping of injected deuterium in doped W was studied by thermal desorption spectrometry (TDS) technique using quadrupole mass spectrometer. Compared with the samples without He⁺ pre-irradiation, deuterium (D) retention of doped W materials increased after He⁺ irradiation, whose retention was unsaturated at the damage level of 1.0 × 10²²D₂⁺/m². The present results implied that irradiation effect of He⁺ ions must be taken into account to evaluate the deuterium retention in fusion material applications.

• Korean Chemical Engineering Research
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• v.60 no.4
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• pp.620-629
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• 2022

By varying various experimental conditions such as heating rate, molar hourly space velocity (MHSV), and nitridation reaction temperature, vanadium oxynitride was prepared through temperature programmed reduction/nitridation reaction (TPRN) of vanadium pentoxide and ammonia, and characterization were performed. In order to investigate the physico-chemical properties of the prepared catalyst, N₂ adsorption-desorption analysis, X-ray diffraction analysis (XRD), hydrogen temperature programmed reduction (H₂-TPR), temperature programmed oxidation (TPO), ammonia temperature programmed desorption (NH₃-TPD), transmission electron microscopy (TEM) was performed. Transformation of V₂O₅ with 5 m² g^-1 low specific surface area by reduction at 340 ℃ to V₂O₃ showed a high specific surface area value of 115 m² g^-1 by micropore formation. As the nitridation temperature increased beyond that, the specific surface area continued to decrease due to sintering. The nitridation reaction variable that had the greatest influence on the specific surface area was the reaction temperature, and the x + y value of VN_xO_y of a single phase approached from 1.5 to 1.0 as the nitridation reaction temperature increased. At a high reaction temperature of 680 ℃, the cubic lattice constant a was VN. close to the value. At 680 ℃, the highest nitridation temperature among the experimental conditions, the ammonia conversion rate was 93%, and no deactivation was observed.

• Nuclear Engineering and Technology
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• v.56 no.6
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• pp.2174-2181
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• 2024

In this work, Sr_0.5Zr₂(PO₄)₃-SmPO₄ dual-phase ceramics were prepared via in-situ synthesis process, which is a potential novel nuclear waste form for immobilizing the fission product ⁹⁰Sr and the trivalent actinide radionuclides in high-level waste (HLW). And the preparation technology, microstructure and chemical durability of Sr_0.5Zr₂(PO₄)₃-SmPO₄ dual-phase ceramics were systematically investigated. It was confirmed that the optimum microwave-sintering temperature (1050 ℃) and heat preservation time (1.5 h) is estimated by Archimedes method. Besides, the as-prepared samples that were consisted of strontium zirconium phosphate (SrZP) and monazite showed the remarkable densification, in which the two crystalline phases were intermixed well with each other. Meanwhile, the formation and evolution of microstructure was also consistent with the variational rule of Sr_0.5Zr₂(PO₄)₃/SmPO₄, indicating that there was not mutual reaction during the in-situ synthesis process. The PCT and MCC-1 experimental results demonstrated that the elemental normalized leaching rates of tested samples are all at a low level (LR_Sr ~10^-4 g·m^-2·d^-1, LR_Zr ~10^-8-10^-6 g·m^-2·d^-1, LR_Sm ~10^-7-10^-5 g·m^-2·d^-1 and LR_P ~10^-4 g·m^-2·d^-1). It is indicated that Sr_0.5Zr₂(PO₄)₃-SmPO₄ dual-phase ceramics possesses excellent chemical durability for HLW disposal.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.29 no.6
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• pp.317-328
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• 2019

In this work, we investigated clay and raw materials from China (black clay, red clay, white clay) and Korea (Cheonan clay, Obu clay) used for the manufacture of porcelain products. According to chemical analysis results, feldspar components containing CaO, K₂O, Na₂O and quartz are found in clay materials besides primary clay such as kaollinte, for the clay materials from Korea, which is found more in clay materials from Korea than from China. For the Fe₂O₃ content, governing whiteness of porcelain products, more iron oxide (> 5 %) is found in Korean clays (Cheonan clay, obu clay, red clay) compared to those form China (black, white clay). Through X-ray diffraction analysis, kaolinite and Halloysite are found to be main phases for all the raw materials and second phases such as quartz and pyrophyllite are found. Using these clay materials, raw materials for porcelain products were produced, and the physicochemical properties were investigated for sintered samples. Absorption rate is in order of Baekja-A < Baekja-B < Yeonbuncheong < Jinbuncheong < Cheongja, and the sample, sintered at 1250℃ in reductive atmosphere, exhibits the lowest absorption rate. Comparing the color of the sintered samples, the samples sintered in oxidative atmosphere (L^* value: 86~95 %) show higher whiteness value than those sintered in reductive atmosphere (L^* value: 81~93 %). For the Cheongja and Buncheong, the samples sintered in reductive atmosphre shows higher whiteness, L^* values, and low a^*/b^* value, which is due to reduction of iron oxide (Fe₂O₃).