• Title/Summary/Keyword: sol-gel processing

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Investigation on the property and preparation of ferroelectric Pb(Zr,Ti)$O_3$ by Sol-Gel method (Sol-Gel법에 의한 강유전체 Pb(Zr, Ti)$O_3$의 제조 및 특성에 관한 연구)

  • 임정한;김영식;장복기
    • Electrical & Electronic Materials
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    • v.7 no.6
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    • pp.496-503
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    • 1994
  • In recent years Sol-Gel processing provides an interesting alternative method for the fabrication of ferroelectric thin layers and powder. PZT powder was prepared from an alkoxide-based solution by a Sol-Gel method. Gelation of synthesized complex solutions, microstructure, thermal analysis and crystallization behaviors of the calcined powder were studied in accordance with a water content and a catalyst. Especially gelation and crystallization behavior were analysed with the change of pH. The gelation time decreased as the pH of the mixed solution increased. For PZT powder with 650.deg. C heat treatment, 100% perovskite phase was formed by using either acidic or basic catalyst. By using either acidic or basic catalyst, we were able to get very fine powders of uniform shape with an average particle size of 0.8-1.mu.m.

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Densification and Crystallization Characteristics of LAS Gels Prepared by the Hydrolysis-Condensation Reaction and the Mixed Colloidal Processing Route (가수분해-축합반응 및 콜로이드 혼합법으로 유도된 LAS gel의 치밀화와 결정화 특성)

  • 김광수;장현명;정창주
    • Journal of the Korean Ceramic Society
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    • v.28 no.11
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    • pp.865-872
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    • 1991
  • LAS (lithium aluminosilicate) sol was synthesized using the hydrolysis-condensation reaction of TEOS, chelated Al(OBus)3 and LiNO3 with H2O in alcohol (ethanol+2-propanol) medium. Lowering Li content by a factor of 1/2 significantly enhanced densification and retarded the crystallization of LAS gel by ~30$0^{\circ}C$. Dense LAS specimen with essentially pore-free microstructure was obtained by sintering the sol-gel derived gel at 80$0^{\circ}C$ for 4 h and annealing at 120$0^{\circ}C$ for 2 h. Similary, a mixed colloidal processing was attempted as a convenient, alternative route for the fabrication of dense LAS sintered body. The $\beta$-spodumene seeding (~0.8 ${\mu}{\textrm}{m}$) in the sol-gel derived LAS modified the sequence of phase transformations and lowered the temperature of crystallization by ~12$0^{\circ}C$. Combining the epitaxial seeding with the sol-gel process, we could lower the crystallization temperature to the sintering temperature range (~80$0^{\circ}C$) and, demonstrate a possibility of making the viscous sintering/crystallization as a continuous as a continuous unit process.

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Preparation of PZT Fibers Using Triethanolamine Complexed Sol (Triethanolamine 착체졸을 이용한 PZT 섬유의 제조)

  • 박용일;이해욱;최용수;이종혁;김승현;김창은
    • Journal of the Korean Ceramic Society
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    • v.33 no.7
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    • pp.755-760
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    • 1996
  • Sol-gel processing was used to prepare PZT fibers. Titanium isopropoxide Zirconium n-butoxide and lead acetate trihydrate were used as starting materials and TEA(triethanolamine) was added to form stabilized Pb-Ti-Zr complex alkoxide, Effects of catalysts and various solvents on the state of precursor sol gelation reaction fiber spinnability pyrolysis and crystallization were also investiated.

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Electrical properties of $Pb(Zr_xTi_{1-x})O_3$ferroelectric thin films prepared by sol-gel processing (Sol-gel법에 의한 $Pb(Zr_xTi_{1-x})O_3$ 강유전 박막의 전기특성)

  • 백동수;박창엽
    • Electrical & Electronic Materials
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    • v.9 no.2
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    • pp.132-137
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    • 1996
  • Pb(Zr$_{x}$Ti$_{1-x}$ )O$_{3}$ solutions prepared by sol-gel processing with different Zr/Ti ratio were coated on Pt/SiO$_{2}$/Si substrates using spin coating method. Coated films were annealed by rapid thermal annealing at 650.deg. C for 20sec to fabricate Pb(Zr, Ti)O$_{3}$ ferroelectric thin films. Electrical properties of the films such as dielectric constant and loss, ferroelectric hysteresis, fatigue, switching time, and leakage current were measured. Hysteresis of the films with different Zr/Ti ratio yield Pr ranging 10-21.mu.C/cm$^{2}$, E$_{c}$ ranging 37.5-137.5kV/cm. Hysteresis curve was changed from square-type to slim type according to increasing Zr contents. Switching time was faster than 180ns, and leakage current was about 20.mu.A/cm$^{2}$. The film underwent above 10$^{8}$ cycles of reversed polarization showed fatigue with increased coercive field and decreased remnant polarization.tion.

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Preparation of Y2O2:Eu Red Phosphor by Sol-Gel and Calcination Process (솔-젤 및 소성공정에 의한 이트륨-유로퓸계 적색형광체 제조)

  • Yoon, Ho-Sung;Kim, Chul-Joo;Jang, Hee Dong
    • Korean Chemical Engineering Research
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    • v.46 no.3
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    • pp.506-511
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    • 2008
  • In this study sol-gel and combustion process was surveyed for the preparation of the red $Y_2O_3$: Eu phosphor, and the properties of phosphor was considered. Chelation and hydrolysis in amorphous citrate sol-gel process were completed in initial reaction stage, and water-forming condensation was superior to organic acid-forming condensation. The mole ratio of citric acid to metal ion had to be above to for the progress of sol-gel process. The dried gel powders are mostly amorphous, and crystallize completely at $700^{\circ}C$, and the crystallinity increases with increasing calcining temperature. The luminescence property of the phosphor was analyzed by measuring the emission spectra. The luminescence intensity increases when the calcination temperature and concentration of metal ions in solution increase.

Preparation of Ferroelectric PZT Thin Film by Sol-Gel Processing; (II) Effect of Catalysts on Densification and Crystallization (솔-젤법에 의한 강유전성 PZT 박막의 제조;(II) 치밀화 및 결정화에 미치는 촉매의 영향)

  • 김병호;박성호;김병호
    • Journal of the Korean Ceramic Society
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    • v.32 no.7
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    • pp.783-792
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    • 1995
  • Sol-Gel derived ferroelectric PZT thin films were fabricated on ITO/Glass and Si/SiO2 substrates. In order to investigate the effect of catalysts on the densification and crystallization of PZT thin films, a nitric acid or ammonium hydroxide was added to the PZT stock solution at the state of partial hydrolysis reaction. The measured pH for a stable PZT sol was 5.2~9.3. In case of an acid-catalyzed PZT sol, a highly condensed particulate PZT sol was formed by accelerating the hydrolysis reaction. But weakly branched polymeric PZT sol was formed with a base-catalyzed condition. The difference in densification behavior was not found in the pH range of added catalyst, but the refractive index of PZT thin film was increased rapidly as the annealing temperature increased. The PZT thin film annealed at 54$0^{\circ}C$ for 10 min was fully densified and its refractive index was above 2.4. When the annealing temperature increased, the transition from the pyrochlore phase to perovskite appeared at 54$0^{\circ}C$. The base-catalyzed PZT thin film suppressed to form the pyrochlore phase and proceeded effectively to convert the perovskite phase. This was due to the formation of polymeric molecular structure by controlling the hydrolysis and condensation reaction through the additiion of the ammonium hydroxide.

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Characteristics of SiC Whisker-Reinforced LAS Matrix Composites Fabricated by the Mixed Colloidal Route and the Sol-Gel Process (콜로이드 혼합법 및 Sol-Gel 법에 의해 제조한 SiC 휘스커 강화 LAS 기지 복합체의 특성)

  • 김광수;장현명;정창주;백용기
    • Journal of the Korean Ceramic Society
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    • v.28 no.12
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    • pp.1012-1018
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    • 1991
  • SiC whisker-reinforced LAS matrix composites were developed by a mixed colloidal processing route. An optimization of processing conditions was made using the zeta potential data of silica, boehmite, and SiC whisker dispersions. Similarly, the SiC whisker-reinforced composites were also fabricated by the conventional sol-gel process using the hydrolysis-condensation reaction of relevant metal alkoxides. The composites fabricated by the mixed colloidal processing route were characterized by a uniform spatial distribution of SiC whisker throughout the matrix. The fracture toughness increased from 1.3 MPa.m1/2 for the LAS specimen to 5.0 Mpa.m1/2 for the hot-pressed composite (95$0^{\circ}C$ and 20 MPa for 20 min) containing 20 wt% SiC whisker. The increase in fracture toughness appears to result mainly from the crack deflection and the crack bridging by whiskers with some additional toughenings from the whisker pullout and the matrix prestressing mechanisms.

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$ZrO_2$ Ceramic Fiber Fabrication by Sol-Gel Processing (Sol-Gel법에 의한$ZrO_2$ Ceramic Fiber 제조)

  • ;;W.C. LaCourse
    • Journal of the Korean Ceramic Society
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    • v.27 no.6
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    • pp.824-828
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    • 1990
  • Zirconia gel fibers were fabricated by sol-gel processing using zirconium alkoxides and 2, 4-pentanedione. Their phase transformation and microstructural evolution were studied after heat treatments up to 150$0^{\circ}C$. Tetragonal ZrO2 began to form at 50$0^{\circ}C$ and followed by monoclinic, tetragonal phase during subsequent heat treatments at 1000, 150$0^{\circ}C$ for 1hour respectively. During cooling from 150$0^{\circ}C$, cracks were created, propagated along grain boundaries due to the volume change from tetragonal to monoclinic transformation.

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The Fabrication of Ferroelectric PZT thin films by Sol-Gel Processing (졸-겔법에 의한 강유전성 PZT 박막의 제작)

  • Lee, B.S.;Chung, M.Y.;You, D.H.;Kim, Y.U.;Lee, S.H.;Lee, N.H.;Ji, S.H.;Park, S.H.;Lee, D.C.
    • Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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    • 2002.05c
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    • pp.93-96
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    • 2002
  • In this study, PZT thin films were fabricated using sol-gel processing onto Si/$SiO_2$/Ti/Pt substrates. PZT sol with different Zr/Ti ratio(20/80, 30/70, 40/60, 52/48) were prepared, respectively. The films were fabricated by using the spin-coating method on substrates. The films were heat treated at $450^{\circ}C$, $650^{\circ}C$ by rapid thermal annealing(RTA). The preferred orientation of the PZT thin films were observed by X-ray diffraction(XRD), and Scanning electron microscopy(SEM). All of the resulting PZT thin films were crystallized with perovskite phase. The fine crystallinity of the films were fabricated. Also, we found that the ferroelectric properties from the dielectric constant of the PZT thin films were over 600 degrees, P-E hysteresis constant. And the leakage current densities of films were lower than $10^{-8}A/cm^2$. It is concluded that the PZT thin films by sol-gel process to be convinced of application for ferroelectric memory device.

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