Fabrication of $Y_2O_3-ZrO_2$ and $CaO-ZrO_2$ Fibers by Sol-Gel Process and Their Phase Characterization by Raman Microprobe

졸-겔법에 의한 $Y_2O_3-ZrO_2$계와 $CaO-ZrO_2$계 섬유의 제조 및 Raman Microprobe에 의한 상분석

  • 황진명 (인하대학교 무기재료공학과) ;
  • 은희태 (인하대학교 무기재료공학과) ;
  • 권혁기 (인하대학교 무기재료공학과)
  • Published : 1994.01.01

Abstract

ZrO2 fibers were fabricated by means of the Sol-Gel process using Zr(O-nC3H7)4-H2O-C2H5OH-HNO3 solution as a starting material. The optimum experimental parameters such as molar ratio of starting materials, concentration, temperature, viscosity, the amounts of stabilizer and the pH of solution were determined. The experimentally determined optimum variables which produce good ZrO2 fibers were used to manufacture the Y2O3-and CaO-ZrO2 fibers. The amounts of Y2O3 and CaO were varied within the range from 1.5~5 mol% and 3~15 mol% respectively. The phase transformation and microstructural evolution of the fabricated ZrO2 gel fibers were investigated after heat treatments up to 120$0^{\circ}C$ by X-ray diffraction, Raman microprobe spectroscopy, SEM, and specific surface area and pore volume measurements. From the analysis of X-ray diffraction and Raman spectra, the phase of heat treated Y2O3-and CaO partially stabilized ZrO2 gel fibers(Y2O3:2.5~3 mol%, CaO:6~9 mol%) were identified as a tetragonal phase up to 100$0^{\circ}C$. The maximum tensile strength of 2.5Y2O3-97.5ZrO2 and 6CaO-94ZrO2 (in mol%) fibers heat treated at 100$0^{\circ}C$ for 1 hr was found be 1.3~2 GPa with diameters of 10~20 ${\mu}{\textrm}{m}$.

Keywords

References

  1. Ultrastructural Processing of Ceramics, Glasses and Composites Fabrication of Zirconia Fibers from Sol-Gels E. Leory(et al.);L.L. Hench(ed.);D.R. Ulrich(ed.)
  2. J. Mater. Sci. v.15 Preparation of Glass Fibres of the ZrO₂-SiO₂and Na₂O-ZrO₂-SiO₂Systems from Metal Alkoxide and their Resistance to Alkaline Solution K. Kamiya(et al.)
  3. J. Non-Cryst. Solids. v.56 Preparation of Amorphous ZrO₂Fibers by Unidirectional Freezing of Gel T. Kokubo(et al.)
  4. Ceram. Eng. Sci. Proc. v.10 no.9;10 Preparation of Zirconia Fibers by Sol-Gel Method S.M. Sim;D.E. Clark
  5. J. Mater. Sci. Lett. v.9 Zirconia Fibers from the Zirconium n-Propoxide-Acetylacetone-Water-Isopropanol System G. De(et al.)
  6. J. Kor Ceram. Soc. v.23 no.4 Preparation of ZrO₂Fibers by Sol-Gel Process and its Properties H. Kim(et al.)
  7. Yogyo Kyokaishi v.92 no.12 Preparation of Fibrous ZrO₂and CaO-ZrO₂from Zirconium Alkoxide by Sol-Gel Method K. Kamiya(et al.)
  8. J. Mater. Sci. v.25 Synthesis of Polycrystalline Zirconia Fibre with Organozirconium Precursor T. Yogo
  9. Ceram. Bull. v.70 no.4 Hydrolysis Method for Preparing Zirconia Fibers C. Sakurai(et al.)
  10. J. Am. Ceram. Soc. v.54 no.5 Infrared and Raman Spectra of Zirconia Polymorphs C.M. Phillippi;K.S. Mazdiyasni
  11. J. Am. Ceram. Soc. v.57 no.1 Raman Scattering Study of the Crystallization and Phase Transformations of ZrO₂ V.G. Keramidas;W.B. White
  12. J. Am. Ceram. Soc. v.60 no.7-8 Temperature Dependence of the Raman Spectra of ZrO₂ M. Ishigame;T. Sakurai
  13. J. Am. Ceram. Soc. v.68 no.8 Phase Characterization of Partially Stabilized Zirconia by Raman Spectroscopy C.H. Perry;D.W. Liu
  14. J. Phys. Chem. Solids v.42 Structure Disorder and Phase Transitions in ZrO₂-Y₂O₃ System A. Feinberg;C.H. Perry
  15. J. Am. Ceram. Soc. v.55 no.6 Phase Analysis Zirconia Systems R.C. Garvie;P.S. Nicholson
  16. J. Phys. Chem. v.69 no.4 The Occurrence of Metastable Tetragonal Zirconia as a Crystallite Size Effect R.C. Garvie
  17. 三重大學大學院 工學硏究科 工業化學專攻 修土論文 ゾル-ゲル法によるガラス 纖維作製の基礎と複合體へ の應用硏究 橋本忠本
  18. Metal Alkoxide D.C. Bradley(et al.)