• 한국세라믹학회지
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• 제31권6호
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• pp.581-586
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• 1994

Effect of excess and deficiency of PbO on the sintering and electrical properties of tetragonal Pb(Zr0.5Ti0.5)O3 were investigated. Fired density revealed maximum value with 4 wt% of excess PbO, and decreased with increasing amount of both excess and deficient PbO. Grain size increased with excess PbO, and decreased with deficiency of PbO. It appeared that excess PbO forms a liquid phase to enhance grain growth and completely volatilizes after sintering, whereas ZrO2 particles formed in PbO-deficient PZT inhibit grain growth. The change in the values of the equivalent circuit elements of PZT corresponded well with thar of porosity formed by excess and deficiency of PbO; kp, Co and Cm decreased while Qm, Rm and Lm increased conosiderably with porosity. This change was more pronounced in PbO-deficient type probably due to change in Zr/Ti ratio of PZT.

• 한국세라믹학회지
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• 제32권6호
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• pp.726-734
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• 1995

Pb(Zr0.53Ti0.47)O3 (PZT) ceramics having different microstructures were fabricated at low temperatures using calcined PZT powders with addition of excess PbO powder and/or ball milling. The effects of excess PbO and ball milling time on the microstructure, the sintering characteristic, and the mechanical properties of these ceramics were studied. Fine powders with average particle size of 0.38㎛ could be obtained by ball milling with 2.5 mm Ф zirconia balls for 120 hours. By the addition of 2mol% of excess PbO to these powders, it was possible to obtain well-densitified PZT ceramics at low sintering temperature of 980℃. Densification behavior of PZT was affected by the addition of excess PbO powder, while, grain growth was hardly affected by PbO addition. It was observed that Vicker's hardness decreased and fracture toughness increased with the increasing amount of PbO. At 1mol% excess PbO, it was shown that the minimum values of hardness and maximum fracture toughness were achieved. In addition, with increasing sintering time, the fracture toughness decreased and the hardness increased.

• 한국세라믹학회지
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• 제34권3호
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• pp.281-288
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• 1997

유전율이 높고 온도안정성이 우수하다고 알려져 있는 40Pb(Mg1/3Nb2/3)O3-30PbTiO3-30Pb(Mg1/2W1/2)O3계 세라믹스에 소결온도를 낮추기 위하여 저온에서 액상을 형성하는 91PbO-9WO3를 과잉첨가하여 소결성, 미세구조 및 유전성의 변화에 대하여 조사하였다. 91PbO-9WO3의 첨가량이 증가함에 따라 소결온도가 저하하였으며 6 mol%첨가시는 875$^{\circ}C$에서 소결이 가능하였다. 유전율은 기본조성에서 16,400이었고, 첨가제가 1 mol% 과잉첨가된 경우 18,500으로 최대값을 나타냈으며 이후 첨가량이 증가함에 따라 감소하였다. 첨가제의 첨가량이 2~4mol%인 시편의 온도에 따른 유전율 변화곡선에서 double peak maxima가 나타났으나, 첨가량이 5 mol% 이상인 시편에서는 입계에 텅스텐을 많이 포함하고 있는 결정상이 생성되었고 double peak maxima는 나타나지 않았다.

• 한국세라믹학회지
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• 제37권7호
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• pp.673-680
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• 2000

The effect of excess PbO(0, 1, 2, 4, and 8 mol%) on grain growth and densification of (65)Pb(Mg1/3Nb2/3)O3-(35)PbTiO3 [mol%] ceramics has been investigaetd. With increasing the amount of excess PbO and sintering time, densities of sintered samples decreased gradually. The samples containing less than 1 mol% of PbO showed normal grain growth behavior, however abnormal grain growth was observed to occur in the samples with more than 2 mol% of PbO. In the samples with more than 2 mol% of PbO, the number of abnormal grains decreased and thus the average grain size became smaller with increasing the amount of excess PbO. These results demonstrated that the abnormal grain growth started to occur when a critical amount of excess PbO was added to a (65)Pb(Mg1/3Nb2/3)O3-(35)PbTiO3 sample. Since PMN-PT grains in a liquid matrix were angular, the observed abnormal grain growth was explained to proceed through the two dimensional nucleation process.

• 한국세라믹학회지
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• 제30권11호
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• pp.925-932
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• 1993

The perovskite phase in PZN-PMN-PT (Pb(Zn, Mg)1/3Nb2/3O3-PbTiO3) pseudoternary ceramics was stabilized by the addition of excess constituent divalent oxides (PbO, MgO and ZnO). The excess addition of 5mol% MgO or 7.5mol% PbO fully stabilized the perovskite phase. The enhanced diffuse phase transition (DPT) and the decrease in the electrical resistivity observed in the presence of excess ZnO or MgO were interpreted in terms of the additional formation of negatively charged, short-range ordered 1:1 domains with a concomitant generation of charge carriers, holes.

• 한국세라믹학회지
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• 제29권5호
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• pp.335-340
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• 1992

Undoped PbTiO3 ceramics was successfully prepared by using sol-gel process, which had not been fabricated due to its microcracks created by anisotropic stress during phase transition from cubic to tetragonal phase. Fabrication of undoped PbTiO3 ceramics via sol-gel processing was very much affected by the PbO content of the samples as well as PbO vapor from sintering atmosphere. Excess PbO was found to promote rapid grain growth in PbTiO3 ceramics. After sintering at 1100$^{\circ}C$ average grain size of PbTiO3 ceramics with excess PbO was about 8 times greater than that of stoichiometric composition, which may be due to PbO liquid phase from excess PbO.

• 한국전기전자재료학회:학술대회논문집
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• 한국전기전자재료학회 2002년도 하계학술대회 논문집 Vol.3 No.2
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• pp.570-573
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• 2002

Pb(Zr0.52Ti0.48)O3 (PZT) thin films were deposited on the Pt/Ti bottom electrode by rf magnetron sputtering method from target containing 5%, 25% and 50% Pb excess for applying ferroelectric random access memory (FRAM). PZT films were deposited at $300^{\circ}C$ and then they were crystallized by rapid thermal annealing (RTA) at $700^{\circ}C$. After RTA treatment, our results showed that all PZT films indicated perovskite polycrystalline structure with preferred orientation (110) and no pyrochlore phase was observed by X-ray diffraction (XRD) and by Scanning electron microscopy (SEM). A well-fabricated PZT film of excess Pb 25% capacitor showed a leakage current density in the order of $2.63{\times}10^{-7}A/cm^2$ at 100kV/cm, a remanent polarization of $3.385{\mu}C/cm^2$ and a coercive field of 41.32 kV/cm. The results showed that Pb excess of target affects to electrical properties of PZT thin film.

• 한국전기전자재료학회논문지
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• 제16권3호
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• pp.186-189
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• 2003

The role of excess Pb about the crystallization behavior and electrical properties in b(Zr$\sub$0.52/Ti$\sub$0.48/)O3(PZT) thin films has not been precisely defined. In this work, the effect of excess Pb content on the ferroelectric properties of these films was investigated. To analyze the effect, PZT films containing various amounts of excess Pb were Prepared. PZT thin films were deposited on the Pt/Ti bottom electrode by rf magnetron sputtering method and then they were crystallized by rapid thermal annealing (RTA). The experiment showed that all PZT films indicated perovskite polycrystalline structure with preferred orientation (111) and no pyrochlore phase was observed. As higher excess Pb was included, the films showed that value of leakage current shift from 2.03${\times}$10$\^$-6/ to 6.63 ${\times}$ 10$\^$-8/A/cm$^2$ at 100kV/cm, and value of remanent polarization shift from 8.587 ${\mu}$C /cm$^2$ to 4.256 ${\mu}$C/ cm$^2$. Electrical properties of PZT thin film affected by Pb excess content of target were explained to be caused of defect among space charges and defect grain boundaries.

• 한국세라믹학회지
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• 제35권9호
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• pp.905-910
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• 1998

• 한국세라믹학회지
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• 제30권8호
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• pp.629-634
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• 1993

Dielectric and electrostrictive properties of 0.99Pb(Mg1/3Nb2/3)O3-0.01Pb(Mn2/3W1/3)O3 system using KCl-NaCl salts have been investigated as a function of the amount of excess MgO. For the specimens calcined at $700^{\circ}C$ for 1h and then sintered at 115$0^{\circ}C$ for 4h, the perovskite phase and the relative density were about 98% and 95%, respectively. With the addition of excess MgO up to 10mol%, the dielectric constant and the electrostrictive strain increased due to the increase of density and grain size, and these properties were degraded by the further addition of excess MgO. For the 10mol% excess MgO added specimen, the maximum electrostrictive strain, Xmax, and the electrostrictive coefficient, Q11, were 4.5$\times$10-4, 3.5$\times$10-2m4/C2, respectively. These results were correlated with the property of PMW and microstructure.