Influence of calcination temperature on the structure of freeze-dried silica gel

동결건조 실리카 젤의 구조에 미치는 하소온도의 영향

  • 최성준 (부산대학교 재료공학부) ;
  • 박상희 (가야대학교 세라믹공학과) ;
  • 박홍채 (부산대학교 재료공학부)
  • Published : 2003.04.01

Abstract

The influence of calcination temperature on the pore structure of freeze dried silica gel derived from tetraethyl orthosilicate (TEOS) was investigated using $N_2$adsorption and mercury intrusion techniques. Freeze dried material contained not only 4-6 nm sized mesopores and 6-10 $\mu\textrm{m}$ sized macropores, but minor micropores. The change of pore structure due to the increase of calcination temperature was dependant upon the degree of densification.

Tetraethyl orthosilicate (TEOS)로부터 유도된 동결건조 실리카 젤의 기공구조에 미치는 하소온도의 영향이 질소 등온흡착 및 수은압입법에 의하여 조사되었다. 동결건조물은 다소간의 마이크로기공을 함유하고 있었으나 주로 4~6nm 크기의 매크로기공 및 7~20$\mu\textrm{m}$ 크기의 매크로기공으로 구성되어 있었다. 하소온도의 증가에 따른 기공구조변화는 치밀화 정도에 의존하였다.

Keywords

References

  1. J. Non-Cryst. Soilds v.121 Structural evolution during sintering of optical sol-gel silica W.L. Vasconcelos;R.T. DeHoff;L.L. Hench https://doi.org/10.1016/0022-3093(90)90116-4
  2. J. Non-Cryst. Soilds v.121 Densification of sol-gel silica constant rate theting, isothermal and step heat treatments L.C. Klein;T.A. Gallo https://doi.org/10.1016/0022-3093(90)90115-3
  3. Ceramic Transactions v.31 D.M. Smith;R. Deshpande-C.J. Berinker;K. Ishixaki(ed.)(et al.)
  4. J. Non-Cryst. Soilds v.144 Pore stucture evolution in sillca gel during aging/drying. III. Effects of surface tension R. Desphpande;D.-W. Hua;D.M. Smith;C.J. Brinker https://doi.org/10.1016/S0022-3093(05)80380-1
  5. Science in Ceramics v.4 F.J. Schnellter;F.R. Monforte;W.W. Rhodes;G.H. Stewart(ed.)
  6. Ceramic Powder Science II F. Dogan;H. Hausner;G.L. Messing(ed.);E.R. Fuller, Jr.(ed.);H. Hausner(ed.)
  7. Science ceramics F.J. Schnettler;F.R. Fuller;Monforte;W.W. Rhodes;G.H. Stewart(ed.);
  8. J. Non-Cryst. Solids. v.121 From sol-gel to aerogels and cryogels G.M. Pajonk;M. Repellin-Lacrols;S. Abournabasse;J. Chaoiki;D. Klvana https://doi.org/10.1016/0022-3093(90)90106-V
  9. J. Non-Cryst. Soilds v.142 Pore structure evolution in silica gel during aging/drying. II. Effect of pore fluids P.J. Davis;C.J. Brinker;D.M. Smith;R.A. Assink https://doi.org/10.1016/S0022-3093(05)80026-2
  10. Nature v.127 Coherent expanded aerogels and jellies S.S. Kistler
  11. Ultrastructure Processing of Ceramics, Glasses and Compisites M. Prassas;L.L. Hench;L.L. Hench(ed.);D.R. Ulrich(ed.)
  12. J. Non-Cryst. Soilds v.100 Attempts to avoid cracks during drying T. Mizuno;H. Nagata;S. Manabe https://doi.org/10.1016/0022-3093(88)90024-5
  13. J. Non-Cryst. Soilds v.170 Control of the porous structure of silica gel by the preparation pH and drying M.K. Titulaer;M.J. Denexter;H. Talsma;J.B.H. Jansen;J.W. Gues https://doi.org/10.1016/0022-3093(94)90037-X
  14. J. Porus Mater v.5 Role of drying techiques on the development of porosity in silica gels S. Rajeshkumar;G.M. Anikumar;S. Ananthakumar;K.G.K. Warrier https://doi.org/10.1023/A:1009625914689
  15. J. Sol-Gel Sci. Tecknol v.15 Influence of the drying technique on the structure of silica gels S.V. Kalinin;L. I. Kheifets;A.I. Mamchik;A. G. Knot'ko;A.A. Veregel https://doi.org/10.1023/A:1008771829173
  16. Mater. Lett. v.46 Calcining silica gels ar different drying stages W.L. Huang;K.M. Liang;S.R. Gu https://doi.org/10.1016/S0167-577X(00)00156-7
  17. X-ray Diffraction B.D. Cullity
  18. J. Am. Chem. Soc. v.73 no.1 The determination of pore volume and area distributions in porus substances. I. computations from nitrogen isotherms E.P. Barrett;L.G. Jpyner;P.P. Halenda https://doi.org/10.1021/ja01145a126
  19. J. Am. Chem. Chem. Soc. v.60 Adsorption of gaese in multimolecular layers S. Brunauar;P.H. Emmett;E.J. Teller https://doi.org/10.1021/ja01269a023
  20. J. Non-cryst. Soilds v.180 Infrares study of $SiO_2$ sol to gel evolution and gel aging J.L. Rehspringer;D. Niznansky https://doi.org/10.1016/0022-3093(94)00484-6
  21. J. Chem. Phys. v.62 Surface funtionality of amorphous silica by infrared sepctroscope R.S. McDonald https://doi.org/10.1021/j150568a004
  22. Infrared Spectra of Inorganic Compounds (3800~44$cm{-1}$) R.A. Nyquist;R.O. Kagel
  23. Pure & Appl. Chem v.57 Repriting physisorption data for gas/soild systems with specical reference to the determination of surface area and porosity K.S.W. Sing;D.H. Everett;R.A.W. Haul;L. Moscou;R.A. Pierotti;J. Rouquerol;T. Siemieniewska