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A new study on the kinetics of Stöber synthesis by in-situ liquid 29Si NMR

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Abstract

Liquid-state 29Si NMR was used to investigate the hydrolysis and condensation kinetics of ammonia-catalyzed tetraethoxysilane (TEOS) in methanol system. The reactive rate constants were calculated by applying first-order reaction approximation and the steady state approximation theory. The reaction orders with respect to TEOS, ammonia and water were derived, as well as the activation energies and the Arrhenius constants. It was found that the formation of intermediate species Si(OH)(OEt)3 was the rate-limiting step and its reaction rate equation was r TEOS=7.41×10−3[TEOS][NH3]0.333[H2O]0.227. Higher reactive temperature benefited the hydrolysis of TEOS. The results presented here indicated quantificationally that the formation of colloidal SiO2 particles was controlled by the initial hydrolysis of TEOS.

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References

  1. Shingo K, Ikuko Y, Noriko Y (1997) In: Dunn BS, Mackenzzie JD, Pope EJ, Schmidt HK, Yanane M (eds) Sol-Gel Optics IV, SPIE vol. 3136. The international society for optical engineering, Bellingham, Washington

  2. Stöber W, Fink A, Bohn E (1968) J Colloid Interface Sci 26:62

    Article  Google Scholar 

  3. Lee K, Look JL, Harris MT, McCormick AV (1997) J Colloid Interf Sci 194:78

    Article  CAS  Google Scholar 

  4. Matsoukas T, Gulari E (1988) J Colloid Interface Sci 124:252

    Article  CAS  Google Scholar 

  5. Bogush GH, Zukoski CF (1991) J Colloid Interface Sci 142:1

    Article  CAS  Google Scholar 

  6. Harris MT, Brunson RR, Byers CH (1990) J Non-Cryst Solids 121:397

    Article  CAS  Google Scholar 

  7. Green DL, Jayasundara S, Yui-Fai Lam, Harris MT (2003) J Non-Cryst Solids 315:166

    Article  CAS  Google Scholar 

  8. Sadasivan S, Duber AK, Li Y, Rasmussen DH (1998) J Sol-Gel Sci Tech 5:12

    Google Scholar 

  9. Harris RK, Kimber BJ (1974) J Organometal Chem 70:43

    Article  CAS  Google Scholar 

  10. Bailey JK, McCartney ML (1992) Colloids Surf 151:63

    Google Scholar 

  11. Assink RA, Kay BD (1991) Ann Rev Mater Sci 21:491

    Article  CAS  Google Scholar 

  12. Sugahara Y, Okada S, Kuroda K, Kato C (1992) J Non-Cryst Solids 139:25

    Article  CAS  Google Scholar 

  13. Brinker CJ, Scherer GW (1990) Sol-gel science: the physics and chemistry of sol-gel processing. Academic Press, San Diego

  14. Fyfe CA, Aroca PP (1997) J Phys Chem B 101:9504

    Article  CAS  Google Scholar 

  15. Volk L, Richardson W (1977) J Chem Educ 54:95

    Article  CAS  Google Scholar 

  16. David Cater E (1983) J Chem Educ 60:109

    Google Scholar 

  17. Parker AJ (1967) Adv Phys Org Chem 5:173

    Article  CAS  Google Scholar 

  18. Parker AJ (1969) Chem Rev 1:69

    Google Scholar 

  19. Iler RK (1979) The chemistry of silica. Wiley, New York

  20. Keefer KD (1984) In: Brinker CJ, Clark DE Ulrich DR (eds) Better ceramics through chemistry. North-Holland, New York, p 15

  21. Boukari H, Long GG, Harris MT (2000) J Colloid Interf Sci 229:129

    Article  CAS  Google Scholar 

Download references

Acknowledgments

The financial support from the National Key Native Science Foundation (No. 20133040) was gratefully acknowledged.

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Correspondence to Yao Xu.

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Xu, Y., Wu, D., Sun, Y. et al. A new study on the kinetics of Stöber synthesis by in-situ liquid 29Si NMR. J Sol-Gel Sci Technol 42, 13–20 (2007). https://doi.org/10.1007/s10971-006-1518-2

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  • DOI: https://doi.org/10.1007/s10971-006-1518-2

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