• 한국세라믹학회지
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• 제48권5호
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• pp.471-478
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• 2011

Investigations of crystal structure and phase transition of $Pb(Zr_{0.52}Ti_{0.48})O_3$ ceramics doped with A-site substitution impurity (La, Nd) or B-site substitution impurity (Sb, Nb) at 2 mol% concentration were carried out. X-ray diffraction patterns of impurities doped $Pb(Zr_{0.52}Ti_{0.48})O_3$ ceramics have been measured at pressures up to ~5 GPa with diamond anvil cell and synchrotron radiation. The patterns were obtained at room temperature using methanol-ethanol mixture as pressure-transmitting media. In order to refine the crystal structure, Rietveld analysis has been performed. The structures of impurities doped $Pb(Zr_{0.52}Ti_{0.48})O_3$ ceramics are tetragonal in space group P4mm at ambient pressure and are transformed into a cubic phase in space group Pm$\bar{3}$m as the pressure increases. In this study, when A-site substitution donor $La^{3+}$ or $Nd^{3+}$ ion was added to $Pb(Zr_{0.52}Ti_{0.48})O_3$ ceramics, the phase transition phenomena showed up at the pressure of 2.5~4.6 GPa, but when B-site substitution donor $Nb^{5+}$ or $Sb^{5+}$ ion was added to it, the phase transition appeared at relatively lower pressure of 1.7~2.6 GPa.

• 한국세라믹학회지
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• 제39권11호
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• pp.1055-1062
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• 2002

정방정 지르코니아의 상안정성 및 저온열화기구를 고찰하기 위해 Y2O3 안정화 지르코니아에 3가 양이온 산화물을 첨가한 후 그 소결체의 기계적 물성, 라만 스펙트럼 및 격자상수 변화 등을 관찰하였다. 2Y-TZP에 $Zr^{4+}$ 보다 이온크기가 큰 3가 양이온($Sc^{3+},\;Yb^{3+},\;Y^{3+},\;Sm^{3+},\;Nd^{3+},\;La^{3+}$)들을 2 mol%까지 첨가하여 $1500{\circ}C$에서 1시간 소결후, X-ray 상분석 결과 $La^{3+}$의 경우에는 0.5 mol% 이상 첨가시 pyrochlore 상$(La_2Zr_2O_7)$의 형성으로 정방정상의 상안정성이 저하되었다. 첨가량이 증가할수록 $Zr6{4+}$과 이온크기가 거의 비슷한 $Sc^{3+}$를 첨가한 경우에는 정방정상만 관찰되었으나 $Yb^{3+},\;Y^{3+},\;Sm^{3+},\;Nd^{3+}$를 첨가한 경우에는 입방정상이 형성되었다. 양이온 크기가 커질수록 c/a비는 증가하였으나 $220{\circ}C$에서 500시간까지 열처리후 상분석 결과 단사정량은 감소하였다.

• 한국세라믹학회지
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• 제54권4호
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• pp.278-284
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• 2017

In this work, Ta-substituted $Li_7La_3Zr_{2-x}O_{12}$ (LLZTO) powder and pellets with garnet cubic structure were fabricated and characterized by modified and optimized sol-gel synthesis. Ta-substituted LLZO powder with the smallest grain size and pure cubic structure with little pyrochlore phase was obtained by synthesis method in which Li and La sources in propanol solvent were mixed together with Zr and Ta sources in 2-methoxy ethanol. The LLZTO pellets made with the prepared powder showed cubic garnet structure for all conditions when the amount of Li addition was varied from 6.2 to 7.4 mol. All the X-ray peaks of the pyrochlore phase disappeared when the Li addition was increased above 7.0 mol. When the final sintering temperature was varied, the LLZTO pellet had a pyrochlore-mixed cubic phase above $1000^{\circ}C$. However, the surface morphology became much denser when the final sintering temperature was increased. The sol-gel-driven LLZTO pellet with a sintering temperature of $1100^{\circ}C$ showed a lithium ionic conductivity of 0.21 mS/cm when Au was adopted as electrode material for the blocking capacitor. The results of this study suggest that modified sol-gel synthesis is the optimum method to obtain cubic phase of LLZTO powder for highly dense and conductive solid electrolyte ceramics.

• 센서학회지
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• 제11권1호
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• pp.48-53
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• 2002

강유전 물질인 $Pb_{0.99}[(Zr_{0.6}Sn_{0.4})_{1-x}Ti_x]_{0.98}Nb_{0.02}O_3$(PNZST) 박막을 10 mole%의 과잉 PbO가 첨가된 타겟을 이용하여 $La_{0.5}Sr_{0.5}CoO_3$(LSCO)/Pt/Ti/$SiO_2$/Si 기판상에 RF 마그네트론 스퍼터링 방법으로 증착하였다. Ti의 조성비를 변화시키면서 증착된 박막에 대하여 그 결정성과 전기적 특성을 조사하였다. 80 W의 RF 전력, $500^{\circ}C$의 기판온도에서 증착한 후, $650^{\circ}C$, 공기중에서 10초 동안 급속 열처리된 박막이 가장 우수한 페로브스카이트상으로 결정화되었다. 또한. Ti의 조성비가 10 mole%를 가지는 PNZST이 가장 우수한 결정성과 강유전 특성을 나타내었다. 이러한 박막으로 제작된 PNZST 커패시터는 약 $20\;{\mu}C/cm^2$정도의 잔류분극과 약 50 kV/cm 정도의 항전계를 나타내었으며, $2.2{\times}10^9$의 스위칭 후에도 잔류분극의 감소는 10% 미만이었다.

• 한국전기전자재료학회:학술대회논문집
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• 한국전기전자재료학회 1994년도 춘계학술대회 논문집
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• pp.25-33
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• 1994

Temperature dependences of the remanent polarization $P_{\gamma}$/(T), effective birefringence ㅿｎ(T). dielectric constant K(T) and quadratic electro-optic coefficient R(T) of the two-stage sintered xBa(La$_{1/2}$Nb$_{1/2}$)O$_3$Pb$(Zr_{y}Ti_{1-y})O-{3}$(x=0.085, 0.09, 0.40$\leq$y$\leq$0.70)ceramics were investigated. Increasing the PbZrO$_3$ contents, the crystal structure of a specimen was varied from tetragonal and rhombohedral to cubic, and the phase transition was showed a diffuse phase transition(DPT) characteristics. Especially. in the compositions which located on the PE-FE phase boundary were showed a discrepancy between curie temperature and temperature range which a macroscopic polarization and a effective birefringence were disappeared.

• 한국진공학회:학술대회논문집
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• 한국진공학회 2013년도 제44회 동계 정기학술대회 초록집
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• pp.94-94
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• 2013

The Cr-Zr-N films have much improved mechanical properties and very smooth surface roughness. However, in spite of their outstanding properties, the Cr-Zr-N coatings revealed their mechanical properties deteriorated severely with increasing Zr content at $500^{\circ}C$ ecause of very rapid oxidation. Recently oxynitride films have been widely studied due to their excellent unique mechanical properties and oxidation resistance. In this work, CrZr-O-N films with various O contents were synthesized by unbalanced magnetron sputtering with Cr-Zr segment targets (Cr:Zr volume ratios is 1：1) and all films were prepared in a nitrogen rich mixture of N2 and O2. Characteristics such as crystalline structure, hardness and chemical composition as a function of the O content were investigated by X-ray diffraction (XRD), field emission scanning electron microscope (FE-SEM), microhardness testing system and energy dispersive spectroscopy (EDS). Results showed that the thin films had dense and compact microstructure as O content in the films increases. The microstructure of the thin films consisted of mainly crystalline Cr (Zr)N phase and Cr2O3 phase. The maximum hardness and elastic modulus of the films was measured to be approximately 33.2 GPa and 280.6 GPa from the films with low content of O elements. Detailed experimental results will be presented.

• E2M - 전기 전자와 첨단 소재
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• 제11권11호
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• pp.9-17
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• 1998

The dependence of the ionic conductivity on the B-site ion substitution in (Li0.5La0.5)Ti1-xMxO3 (M=Sn, Zr, Mn, Ge) system has been studied. Same valence state and various electronic configuration and ionic radius of Sn4+, Zr4+, Mn4+ and Ge4+(4d10(0.69$\AA$), 4p6(0.72$\AA$), 3d10(0.54$\AA$) and 3d3(0.54$\AA$), respectively) induced the various crystallographic variaton with substitutions. So it was possibleto investigate the crystallographic factor which influence the ionic conduction by observing the dependence of the conductivity on the crystallographic factor which influence the ionic conduction by observing the dependence of the conductivity on the crystallographic variations. We found that the conductivity increased with decreasing the radii of B-site ions or vice versa and octahedron distortion disturb the ion conduction. The reason for this reciprocal proportion of conductivity on the radius of B-site ions has been examined on the base of the interatomic bond strength change due to the cation substitutions. The results were good in agreement with the experimental results. Therefore it could be concluded that the interatomic bond strength change due to the cation substitutions may be the one of major factors influencing the lithium ion conductivity in perovskite(Li0.5La0.5) TiO3system.

• 한국세라믹학회지
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• 제31권2호
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• pp.155-160
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• 1994

PZT ceramics substituted by La3+ and Nd3+ were fabricated according to the formula: [Pb1-x(La or Nd)x][Zr0.58Ti0.42]1-x/4$\square$x/4O3(x=0.00, 0.02, 0.05, 0.08, 0.15, 0.20). The crystal structure and microstructure were investigated by XRD and SEM. It was observed that the phase transitions among rhombohedral, tetragonal, and cubic symmetry occured as the substitutional quantity increased. Dielectric constant, dissipation factor and piezoelectric coefficient (d33), of each sample were measured. The dielectric properties were changed as the substitutional quanity of rare earth ion increased. These changes could be explained by crystal structure and compositional fluctuaction. Its d33 was higher at tetragonal region near to phase boundry between rhombohedral and tetragonal, which was explained by reorientation of domain wall.

• 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.

• 한국세라믹학회지
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• 제23권4호
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• pp.62-68
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• 1986

$(Pb_{1-x} La_x)(Zr_{0.65} Ti_{0.35})_{1-x/4}O_3$ (PLZT X/65/35) powders were prepared by molten salt synthesis using NaCl-K Cl and conventional calcining of oxides. The effects of molten salt on formation and charactrization of PLZT powder and on dielectric piezolectric and optical properties of PLZT ceramics were studied, The completed PLZT powder formation in the presence of fused salt was attained at 50-10$0^{\circ}C$ lower temperature than that in solid state reaction and the particle size of the powder made by molten salt synthesis was markedly increased with increasing calcining temperature. The substitution of Na and/or K ions in NaCl-KCl for Pb ion in process of molten salt synthesis was increased with increasing La concentration Z. These substituted Na and/or K ions were identified as the origins of decreasing coupl-ing factor and optical transmittance of PLZT ceramics.