• 한국세라믹학회지
• /
• 제45권2호
• /
• pp.126-131
• /
• 2008

In this study, we prepared zirconia gel by the sol-gel method and investigated its photoluminescence properties by varying pyrolysis temperature. The addition of acetic acid into a Zr-alkoxide solution resulted in forming the bidentate ligands with Zr ions and producing a stable gel. At the pyrolysis temperature of $350^{\circ}C$, the zirconia nanocrystals with tetragonal structure gradually appeared in the gel. The PL intensity of the zirconia gel increased with increasing the pyrolysis temperature up to $350^{\circ}C$, but decreased above the temperature. Concurrently, its PL peak wavelength continuously shifted from ${\sim}440\;nm$ to ${\sim}550\;nm$ with the temperature. The PL characteristics of the zirconia gels were closely associated with decomposition of residual organic groups, the formation of the zirconia nanocrystals, and the tetragonal to monoclinic phase transformation.

• 한국세라믹학회지
• /
• 제34권2호
• /
• pp.171-174
• /
• 1997

산소포논(phonon)이 Yttiria안정화 정방정 지르코니아 소결체(Yttria Stabilized Tetragonal Zirconia Po-lycrystals, Y-TZP)의 저온열화에 큰 영향을 미치는 사실을 실험적으로 밝혔다. Y-TZP의 저온열화 (정방정$\longrightarrow$단사정 상전이) 현상은 Y-TZP의 16O을 18O으로 치환함으로써 급격히 저하되었다. 이는 16O이 보다 무거운 18O으로 치환됨에 따라 임계변위 이상에서 산소원자가 존재할 확률이 감소하는 데 기인하는 것으로 설명하였다.

• 한국세라믹학회지
• /
• 제26권4호
• /
• pp.568-574
• /
• 1989

Effect of PbO addition on sintering and piezoelectric properties at 0.45Pb(Ni1/3Nb2/3)O3-0.40PbTiO3-0.15PbZrO3 composition which is tetragonal phase was investigated. In this composition, Porosity and dielectric constant were increased with excess PbO addition, but Kp and d31 was not changed. These variation of physical properties could be interpreted as composition change of solid grains from tetragonal to MPB region due to amount of PbO-rich liquid changing.

• 한국분말야금학회:학술대회논문집
• /
• 한국분말야금학회 2006년도 Extended Abstracts of 2006 POWDER METALLURGY World Congress Part 1
• /
• pp.124-125
• /
• 2006

Multilayer ceramic capacitor (MLCC) miniaturization has increased the demand for superfine $BaTiO_3$ powder due to its thin dielectric layer. Hydrothermally synthesized $BaTiO_3$ powder a pseudo-cubic phase resulting in poor dielectric properties due to size effect and hydroxyl ion inclusion in the $BaTiO_3$ lattice. We attempted a superfine (lower than 100 nm) highly tetragonal $BaTiO_3$ powder via a solvothermal method without precipitating agent. The lattice parameters and the relative amounts of tetragonal and cubic phases were determined using Rietveld refinement.

• 한국결정학회지
• /
• 제3권2호
• /
• pp.120-128
• /
• 1992

BaTiO3 단결정을 용액의 서냉속도를 달리하면서 TSSG법으로 육성하였으며, 성장된 단결정의 결정외형, 결정 결함, 분역구조 등을 관찰하였다. 0.5℃/hr이 하의 속도로 서 냉함으로써 비교적 등차원적인 큰 단 결정을 육성할 수 있었으며, 성장된 BaTiO3 단결정 은 |111|면이 가장 잘 발달된 외형을 나타내었다. 용 액 냉각속도가 너무 빠르거나 용액내의 수직 온도구 배가 너무 크면 용액이 불안정해지므로, 침상의 Ba6 TiL7040 결정상이 석출된다. 성장된 결정내에 평행 한 쐐기모양의 lamella 분역 집단이 이와 수직하게 진행하는 lamella 분역 집단과 불규칙한 경계를 이루 고 있으며, 이들은 x-ray topography에서 현저한 회 절 명암 차이를 나타낸다. 단결정을 127℃ 이상으로 가열하면 입 방정으로 상전이 된다. 상전이 전단이 이 동할 때 정방정 영역에서는 연속적 분역 재배열이 이루어 지고 입방정 영역에서는 규칙적인 음력변형이 나타나며, BaTiO의 PTF정벽면은 |110|에 대해 약 9°기울어진 면으로 이루어진다.

• 한국재료학회:학술대회논문집
• /
• 한국재료학회 2011년도 춘계학술발표대회
• /
• pp.241.1-241.1
• /
• 2011

Numerous possible applications for $ZrO_2$ nanotubes exist such as for catalyst support structures, for sensing or for applications as a solid state electrolyte. Especially, because of a large specific surface area, high efficiency for solid oxide fuel cell (SOFC) application at low temperature can be expected for nanotublar structures in even small size. A zirconium precursor, Tetrakis (ethylmethylamino) zirconium, TEMAZr and $H_2O$ oxidant were used to deposit$ZrO_2$ thin films on an anodized aluminum oxide (AAO) templates having sub-100nm cylindrical pores by atomic layer deposition (ALD) in the temperature range of 150~250$^{\circ}C$. The crystalline structures of as-prepared and post-annealed $ZrO_2$ nanotubes were characterized by x-ray diffraction and high-resolution transmission electron microscopy. The as-prepared samples at $150^{\circ}C$ and $200^{\circ}C$ were showed amorphous, whereas a mixed phase of tetragonal, monoclinic and amorphous polymorph was observed at $250^{\circ}C$. In the bulk, zirconia remains monoclinic phase up to $1,175^{\circ}C$, however, $ZrO_2$ nanotubes were showed tetragonal phase upon post thermal treatments merely at $400^{\circ}C$. This trend may be indicative of high-curvature surfaces of nanotubes and thereby the presence of intrinsic compressive strain. The amount of amorphous structures in the mixed phase as well as as-grown $ZrO_2$ nanotubes were also gradually decreased by subsequent heat treatment.

• 한국세라믹학회지
• /
• 제47권4호
• /
• pp.343-352
• /
• 2010

A zirconia gel/polymer hybrid nanofiber was produced in a nonwoven fabric mode by electrospinning a sol derived from hydrolysis of zirconium butoxide with a polyvinyl butyral. Results indicated that the hydroxyl groups on the vinyl alcohol units in the backbone of the polymer were involved in the hydrolysis as well as grafting the hydrolyzed zirconium butoxide. In addition, use of acetic acid as a catalyst resulted in further hydrolysis and condensation in the sol, which led to the growth of -Zr-O-Zr- networks among the polymer chains. These networks gradually transformed into a crystalline zirconia structure upon heating. The as-spun fiber was smooth but partially wrinkled on the surface. The average fiber diameter was $690{\pm}110\;nm$. The fiber exhibited a strong but broad blue photoluminescence with its maximum intensity at a wavelength of ~410 nm at room temperature. When the fiber was heat-treated at $400^{\circ}C$, the fiber diameter shrunk to $250{\pm}60\;nm$. Nanocrystals which belonged to a tetragonal zirconia phase and were ~5 nm in size appeared. A strong white photoluminescence was observed in this fiber. This suggests that oxygen or carbon defects associated with the formation of the nanocrystals play a role in generating the photoluminescence. Further heating to $800^{\circ}C$ resulted in a monoclinic phase beginning to form In the heat-treated fibers, coloring occurred but varied depending on the heating temperature. Crystallization, coloring, and phase transition to the monoclinic structure influenced the photoluminescence. At $600^{\circ}C$, the fiber appeared to be fully crystallized to a tetragonal zirconia phase.

• 한국재료학회지
• /
• 제23권10호
• /
• pp.543-549
• /
• 2013

The purpose of this paper was to investigate the effect of a high-energy milling (HEM) process on the particle morphology and the correlation between a thermal treatment and tetragonal/monoclinic nanostructured zirconia powders obtained by a precipitation process. To eliminate chloride residue ions from hydrous zirconia, a modified washing method was used. It was found that the used washing method was effective in removing the chloride from the precipitated gel. In order to investigate the effect of a pre-milling process on the particle morphology of the precipitate, dried $Zr(OH)_4$ was milled using a HEM machine with distilled water. The particle size of the $Zr(OH)_4$ powder exposed to HEM reduced to 100~150 nm, whereas that of fresh $Zr(OH)_4$ powder without a pre-milling process had a large and irregular size of 100 nm~1.5 ${\mu}m$. Additionally, modified heat treatment process was proposed to achieve nano-sized zirconia having a pure monoclinic phase. It was evident that two-step calcining process was effective in perfectly eliminating the tetragonal phase, having a small average particle of ~100 nm with good uniformity compared to the sample calcined by a single-step process, showing a large average particle size of ~300 nm with an irregular particle shape and a broad particle size distribution. The modified method is considered to be a promising process for nano-sized zirconia having a fully monoclinic phase.

• 한국전기전자재료학회논문지
• /
• 제24권8호
• /
• pp.622-626
• /
• 2011

Lead-free piezoelectric ceramics with the composition of $(Na_{0.54}K_{0.46})_{0.96}Li_{0.04}(Nb_{1-0.10-x}Ta_{0.10}Sb_x)O_{3}$ (x= 0~8 mol%) were fabricated by nomal sintering at $1,090^{\circ}C$ for 5 h. the phase structure, microstructure and electrical properties were investigated with a emphasis on the influence of the Sb content. All samples exhibit a single perovskite phase over the whole compositional range. For the ceramics with x= 4 [mol%], two phase transitions are observed at $75^{\circ}C$ and $366^{\circ}C$, corresponding to the phase transitions of orthorhombic to tetragonal (To-t) and tetragonal to cubic (Tc), respectively. high electrical properties of $d_{33}$= 210.83 pC/N, kp= 40%, ${\varepsilon}_r$= 1,091.35, $\rho$= 4.54 g/$cm^2$ were obtained from the specimen with x= 4 [mol%], which suggests that the composition ceramics is a promising lead-free piezoelectric material.

• Journal of Ceramic Processing Research
• /
• 제13권spc2호
• /
• pp.341-345
• /
• 2012

[Li0.055(K0.5Na0.5)0.945](Nb1-xTax)O3 (0.05 ≤ x ≤ 0.25) ceramics were prepared by the partial sol-gel (PSG) method to improve the microstructure homogeneity of Ta5+ ion and were compared to those prepared by the conventional mixed oxide (CMO) method. For the PSG method, Ta(OC2H5)5 was directly reacted with calcined [Li0.055(K0.5Na0.5)0.945]NbO3 powders and the specimens sintered at 1100 ℃ for 5 hrs showed a single phase with a perovskite structure. Compared to the specimens prepared by conventional mixed oxide powders, the relative ratio of tetragonal phase to orthorhombic phase of the sintered specimens prepared by Ta(OC2H5)5 was larger than that of the sintered specimens prepared by Ta2O5. The electromechanical coupling factor (kp), piezoelectric constant (d33) and dielectric constant (εr) of the sintered specimens were increased with Ta5+ content. These results could be attributed to the decrease of the orthorhombic-tetragonal polymorphic phase transition temperature (To-t), which could be evaluated by oxygen octahedral distortion. Strain of the sintered specimens prepared by the PSG method was higher than that of specimens prepared by the CMO method due to the increase of relative density. The effects of crystal structure on the strain characteristics of the specimens were also discussed.