• 한국표면공학회지
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• 제50권6호
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• pp.465-472
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• 2017

The ingot fabrication conditions related with the thermal shock bearing phase and microstructure have investigated for the rare earth zirconate ceramic material, lanthanum gadolinium zirconate, as a thermal barrier coating using electron beam evaporation method. The thermal shock resistance of the prepared ingot was evaluated by high energy electron beam irradiation. The rare earth zirconate ceramic powder was prepared by controlling the raw material powder composition of $La_2O_3$, $Gd_2O_3$ and $ZrO_2$ so as to have a composition of $(La_{0.3}Gd_{0.7})_2Zr_2O_7$ which was selected from the former study. Ingot samples were prepared under two conditions. The first condition is prepared by sintering the prepared powder mixture to form an ingot. The second condition is prepared by calcining the prepared powder mixture to form a composite phase and then sintering to form an ingot. X-ray diffraction(XRD) and Scanning Electron Microscope(SEM) were used to analyze phase forming behavior and microstructure of ingot samples. Nanoindentation method used to obtain elastic modulus and hardness of each ingot specimen. Also the stress distribution of ingot was simulated by using FEM method assuming the ingot surface was exposed to electron beam. As a results, in the case of an ingot having a network-shaped microstructure in which relatively coarse pores are included, it seems that the thermal shock resistance was higher than in the case of an ingot having a microstructure composed of relatively fine grains only or particles with the similar level size when the high energy electron beam irradiation.

• Journal of Ceramic Processing Research
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• 제20권6호
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• pp.609-616
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• 2019

The optimum powder to ball ratio was examined, which is one of the important conditions in reactive mechanical grinding processing. Yttria (Y2O3)-stabilized zirconia (ZrO2) (YSZ), Ni, and graphene were chosen as additives to enhance the hydriding and dehydriding rates of Mg. Samples with a composition of 92.5 wt% Mg + 2.5 wt% YSZ + 2.5 wt% Ni + 2.5 wt% graphene (designated as Mg-2.5YSZ-2.5Ni-2.5graphene) were prepared by grinding in hydrogen atmosphere. Mg-2.5YSZ-2.5Ni-2.5graphene had a high effective hydrogen-storage capacity of almost 7 wt% (6.85 wt%) at 623 K in 12 bar H2 at the second cycle (n = 2). Mg-2.5YSZ-2.5Ni-2.5graphene contained Mg2Ni phase after hydriding-dehydriding cycling. Mg-2.5YSZ-2.5Ni-2.5graphene had a larger quantity of hydrogen absorbed for 60 min, Ha (60 min), than Mg-2.5Ni-2.5graphene and Mg-2.5graphene. The addition of YSZ also increased the initial dehydriding rate and the quantity of hydrogen released for 60 min, Hd (60 min), compared with those of Mg-2.5Ni-2.5graphene. Y2O3-stabilized ZrO2, Ni, and graphene-added Mg had a higher initial hydriding rate and a larger Ha (60 min) than Fe2O3, MnO, or Ni and Fe2O3-added Mg at n = 1.

• 한국재료학회지
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• 제11권9호
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• pp.769-775
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• 2001

High quality PZT piezoelectric thin films were sputter- deposited on$ RuO_2$/$SiO_2$/Si substrates by using 2-step deposition method. As the first step, PZT seed layers were fabricated at a low temperature($475^{\circ}C$ ) to form a pure perovskite phase by reducing the volatility of Pb oxide. and then, as the second step, the PZT films were deposited at high temperatures ($530^{\circ}C$~$570^{\circ}C$) to reduce the defect density in the films. By this method, the pure perovskite phase was obtained at high deposition temperature range ($530^{\circ}C$~$570^{\circ}C$) and the superior electrical properties of PZT films were obtained on $RuO_2$substrate : 2Pr : 60$\mu$C/$\textrm{cm}^2$, $E_c: 60kV/cm, \;J_t: 10^{-6}A/cm^2\; at\; 250kV/cm$. The residual stress of PZT films fabricated by the 2-step deposition method was tensile and below 150MPa. It was attempted to control the residual stress in the PZT films by applying a negative bias to the substrate. As the amplitude of the substrate bias was increased, the residual tensile stress was slightly decreased, however, the ferroelectric properties of PZT films were degraded by ion bombardment.

• 한국결정성장학회지
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• 제10권3호
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• pp.245-251
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• 2000

Pb($(Ni_{1/3}Nb_{2/3})O_3-PbTiO_3-PbZrO_3$세라믹스에서 NiO첨가에 따른 유전, 압전 및 기계적 특성의 변화를 연구하였다. Columbite precursor법을 사용하여 분말을 제조 후 공기중에서 $1100^{\circ}C$~$1250^{\circ}C$의 온도로 2시간 소결하여 시편을 제조하였다. $1150^{\circ}C$이하 온도에서 소결한 시편에서는 NiO를 1 mol% 첨가시까지 유전상수와 압전상수가 증가하였으나 첨가량이 그 이상 증가함에 따라 감소하였는데 이는 NiO가 소결조제 역할을 한 것으로 보여진다. 그러나 $1200^{\circ}C$ 이상 온도에서 소결한 시편에서는 NiO 첨가량 증가에 따라 유전상수와 전기기계결합계수가 감소하였으며, 기계적품질계수는 증가하였다. 경도 및 파괴인성은 1 mol% 첨가시 최대 값을 보이다가 그 이후 감소하였다. NiO 첨가 PNN-PT-PZ 세라믹스의 전기적 및 기계적 특성은 결정립크기, 소결밀도 및 2차상의 양 등의 미세구조적 요소와 긴밀한 관계가 있음을 보여준다.

• The Korean Journal of Ceramics
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• 제4권4호
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• pp.352-355
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• 1998

Dense $ Pb(Zr, Ti)O_3(PZT)/Al_2O_3$ nanocomposites were prepared by the 28 GHz microwave heating method and conventional electric furnace sintering. Electrical and mechanical properties of the composites were investigated. The fracture strength of the PZT composites with 0.1vol% $Al_2O_3$ was significantly improved in both sintering methods. Smaller grain size and effective reinforcement of the PZT matrix by the second phase were considered to be responsible for the excellent fracture strength. Planar electromechanical coupling factor Kp of the composites sintered by 28GHz microwave heating was higher than that of the materical prepared by the conventional route. It seemed that the control of the reaction between PZT and $Al_2O_3$ by the microwave rapid sintering resulted in the high piezoelectric properties.

• 한국세라믹학회지
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• 제25권3호
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• pp.261-267
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• 1988

완도납석과 carbon black 의 혼합물을 135$0^{\circ}C$에서 질소분위기를 사용하여 탄소환원질화법으로 $\beta$-Sialon 분물에 $\beta$-SiC를 제2상으로 넣어서 $Y_2O_3$와 $ZrO_2$를 각 소결조제로 사용하여 175$0^{\circ}C$에서 2시간 동안 상압소결하였다. 10wt %의 $Y_2O_3$를 소결조제로 사용하였을 때에 파괴인성은 3.8MN/m^{3/2}$, 3점꺽임 강도는 470MN/$m^2$ 그리고 경도는 13.7MN/$m^2$로서 좋은 값을 나타내었다. 이와 같은 파괴인성과 꺽임강도의 증가는 균열편향과 균열나눠짐에 의한 것으로 생각된다.

• 한국분말야금학회:학술대회논문집
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• 한국분말야금학회 1996년도 추계학술강연 및 발표대회 강연 및 발표논문 초록집
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• pp.6-6
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• 1996

Ceramic based nanocomposite, in which nano-sized ceramics and metals were dispersed within matrix grains and/or at grain boundaries, were successfully fabricated in the ceramic/cerarnic and ceramic/metal composite systems such as $Al_2O_3$/SiC, $Al_2O_3$/$Si_3N_4$, MgO/SiC, mullite/SiC, $Si_3N_4/SiC, $Si_3N_4$/B, $Al_2O_3$/W, $Al_2O_3$/Mo, $Al_2O_3$/Ni and $ZrO_2$/Mo systems. In these systems, the ceramiclceramic composites were fabricated from homogeneously mixed powders, powders with thin coatings of the second phases and amorphous precursor composite powders by usual powder metallurgical methods. The ceramiclmetal nanocomposites were prepared by combination of H2 reduction of metal oxides in the early stage of sinterings and usual powder metallurgical processes. The transmission electron microscopic observation for the $Al_2O_3$/SiC nanocomposite indicated that the second phases less than 70nm were mainly located within matrix grains and the larger particles were dispersed at the grain boundaries. The similar observation was also identified for other cerarnic/ceramic and ceramiclmetal nanocornposites. The striking findings in these nanocomposites were that mechanical properties were significantly improved by the nano-sized dispersion from 5 to 10 vol% even at high temperatures. For example, the improvement in hcture strength by 2 to 5 times and in creep resistance by 2 to 4 orders was observed not only for the ceramidceramic nanocomposites but also for the ceramiclmetal nanocomposites with only 5~01%se cond phase. The newly developed silicon nitride/boron nitride nanocomposites, in which nano-sized hexagonal BN particulates with low Young's modulus and fracture strength were dispersed mainly within matrix grains, gave also the strong improvement in fracture strength and thermal shock fracture resistance. In presentation, the process-rnicro/nanostructure-properties relationship will be presented in detail. The special emphasis will be placed on the understanding of the roles of nano-sized dispersions on mechanical properties.

• 한국재료학회지
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• 제34권2호
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• pp.116-124
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• 2024

In this study, we investigated the microstructure and piezoelectric properties of 0.96(K_0.456Na_0.536)Nb_0.95Sb_0.05-0.04Bi_0.5(Na_0.82K_0.18)_0.5ZrO₃ (KNNS-BNKZ) ceramics based on one-step and two-step sintering processes. One-step sintering led to significant abnormal grain (AG) growth at temperatures above 1,085 ℃. With increasing sintering temperature, piezoelectric and dielectric properties were enhanced, resulting in a high d₃₃ = 506 pC/N for one-step specimen sintered at 1,100 ℃ (one-step 1,100 ℃ specimen). However, for one-step 1,115 ℃ specimen, a slight decrease in d₃₃ was observed, emphasizing the importance of a high tetragonal (T) phase fraction for superior piezoelectric properties. Achieving a relative density above 84 % for samples sintered by the one-step sintering process was challenging. Conversely, two-step sintering significantly improved the relative density of KNNS-BNKZ ceramics up to 96 %, attributed to the control of AG nucleation in the first step and grain growth rate control in the second step. The quantity of AG nucleation was affected by the duration of the first step, determining the final microstructure. Despite having a lower T phase fraction than that of the one-step 1,100 ℃ specimen, the two-step specimen exhibited higher piezoelectric coefficients (d₃₃ = 574 pC/N and k_p = 0.5) than those of the one-step 1,100 ℃ specimen due to its higher relative density. Performance evaluation of magnetoelectric composite devices composed of one-step and two-step specimens showed that despite having a higher g₃₃, the magnetoelectric composite with the one-step 1,100 ℃ specimen exhibited the lowest magnetoelectric voltage coefficient, due to its lowest k_p. This study highlights the essential role of phase fraction and relative density in enhancing the performance of piezoelectric materials and devices, showcasing the effectiveness of the two-step sintering process for controlling the microstructure of ceramic materials containing volatile elements.

• Bulletin of the Korean Chemical Society
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• 제18권1호
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• pp.56-61
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• 1997

Lead zirconate titanate (PZT) thin fills were deposited onto the Pt/Ti/SiO2/Si substrate by the pulsed laser deposition with the second harmonic wavelength (532 nm) of Nd:YAG laser. In order to determine the optimum conditions for the film deposition, the phase of the films were investigated as functions of ambient oxygen pressure, substrate temperature, and laser fluence. Also the chemical composition analysis was conducted for the PZT films deposited under various ambient oxygen pressure. When the distance between substrate and bulk PZT target is set to 20 mm, the optimum conditions have been determined to be 3 torr of oxygen pressure, 1.5 J/cm2 of laser fluence, and 823-848(±10) K range of substrate temperature. At these conditions, perovskite phase PZT films were obtained on platinized silicon. The chemical composition of the films is very similar to that of PZT bulk target. The physical structure of the deposited films analyzed by scanning electron microscopy shows a columnar morphology perpendicular to the substrate surface. Capacitance-Voltage hysteresis loop measurements show also a typical characteristics of ferroelectric thin film. The dielectric constant is found to be 528 for the 0.48 μm thickness of PZT thin film.

• 한국세라믹학회지
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• 제32권1호
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• pp.120-130
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• 1995

To analyze the mechanical property and the residual stress in functionally gradient materials(FGMs), disctype TZP/Ni-and TZP/SUS304-FGM were hot pressed using powder metallurgy compared with directly bonded materials which were fabricated by the same method. The continuous interface and the microstructure of FGMs were characterized by EPMA, WDS, optical microscope and SEM. By fractography, the fracture behavior of FGMs was mainly influenced by the defects which originated from the fabrication process. And the defectlike cracks in the FGMs induced by the residual stress have been shown to cause failure. This fact has well corresponded to the analysis of the residual stress distribution by Finite Element Method (FEM). The residual stress generated on the interface (between each layer, and matrix and second phase, respectively) were dominantly influenced on the sintering temperature and the material constants. As a consequence, the interfacial stability and the relaxation of residual stress could be obtained through compositional gradient.