Skip to main content

Advertisement

Log in

Preparation, characterization and mechanical properties of continuous mullite fibers derived from the diphasic sol-gel route

  • Original Paper: Fundamentals of sol-gel and hybrid materials processing
  • Published:
Journal of Sol-Gel Science and Technology Aims and scope Submit manuscript

Abstract

In the present work, continuous mullite fibers were fabricated through the diphasic sol-gel route using aluminum isopropoxide (AIP) and aluminum nitrate (AN) as the alumina sources and colloidal silica as the silica source. Fiber processing was achieved via draw-spinning method. Amorphous inorganic mullite fibers with smooth and dense features, as well as designed chemical composition and uniform elemental distribution, were obtained by pyrolysis of the continuous precursor fibers at the ending temperature of 800 °C in air. The microstructure and mechanical properties of the samples sintered at elevated temperatures were investigated. Differential thermal analysis (DTA) showed two exothermic peaks at 978 and 1271 °C assigned to the crystallization of γ-Al2O3 and mullite phase, respectively. X-ray powder diffraction (XRD) results verified the typical phase transformation route of diphasic mullite while sintering. Transmission electron microscopy (TEM) and scanning electron microscopy (SEM) showed a rapid grain growth after the mullite phase had formed. As the sintering temperatures increased, the filament tensile strength of the mullite fibers first increased and then decreased, reaching a maximum value of 934 MPa at 1000 °C.

Highlights

  • Continuous and homogeneous mullite fibers were prepared through the diphasic sol-gel route.

  • Alumina sol fabricated by AIP and AN was used to prepare diphasic mullite sol for the first time.

  • Smooth and dense surface remained at 900_1100 °C due to the small γ-Al2O3 grains.

  • Rapid grain growth occurred after 1200 °C was ascribed to the formation of mullite phase.

  • A maximum tensile strength of 934 MPa was acquired after sintering the fibers at 1000 °C.

This is a preview of subscription content, log in via an institution to check access.

Access this article

Price excludes VAT (USA)
Tax calculation will be finalised during checkout.

Instant access to the full article PDF.

Fig. 1
Fig. 2
Fig. 3
Fig. 4
Fig. 5
Fig. 6
Fig. 7
Fig. 8
Fig. 9

Similar content being viewed by others

References

  1. Bunsell AR, Berger MH (2000) Fine diameter ceramic fibres. J Eur Ceram Soc 20:2249–2260

    Article  Google Scholar 

  2. Deléglise F, Berger MH, Jeulin D, Bunsell AR (2001) Microstructural stability and room temperature mechanical properties of the Nextel 720 fibre. J Eur Ceram Soc 21:569–580

    Article  Google Scholar 

  3. Schawaller D, Clauß B, Buchmeiser MR (2012) Ceramic filament fibers - a review. Macromol Mater Eng 297:502–522

    Article  Google Scholar 

  4. Almeida RSM, Bergmüller EL, Eggert BGF, Tushtev K, Schumacher T, Lührs H, Clauß B, Grathwohl G, Rezwan K (2016) Thermal exposure effects on the strength and microstructure of a novel mullite fiber. J Am Ceram Soc 99:1709–1716

    Article  Google Scholar 

  5. Schneider H (2005) Basic Properties of Mullite. In: Schneider H, Komarneni S (eds) Mullite. Wiley-VCH, Weinheim, p 141–215

  6. Dong X, Chen Z, Guo A, Liu J, Wang X, Chen C (2018) Mechanical and interfacial behavior of single mullite fiber and mullite fiber-based porous ceramics. Ceram Int 44:14446–14456

    Article  Google Scholar 

  7. Okada K, Yasohama S, Hayashi S, Yasumori A (1998) Sol-gel synthesis of mullite long fibres from water solvent systems. J Eur Ceram Soc 18:1879–1884

    Article  Google Scholar 

  8. Song KC (1998) Preparation of mullite fibers from aluminum isopropoxide-aluminum nitrate-tetraethylorthosilicate solutions by sol-gel method. Mater Lett 35:290–296

    Article  Google Scholar 

  9. Cividanes LS, Campos TMB, Rodrigues LA, Brunelli DD, Thim GP (2010) Review of mullite synthesis routes by sol-gel method. J Sol-Gel Sci Technol 55:111–125

    Article  Google Scholar 

  10. Chen X, Gu L (2009) Sol-gel dry spinning of mullite fibers from AN/TEOS/AIP system. Mater Res Bull 44:865–873

    Article  Google Scholar 

  11. Zhang Y, Ding Y, Gao J, Yang J (2009) Mullite fibres prepared by sol-gel method using polyvinyl butyral. J Eur Ceram Soc 29:1101–1107

    Article  Google Scholar 

  12. Sowman HG (1974) Aluminum borate and aluminum borosilicate articles. US Patent 3,795,524.

  13. Schmücker M, Flucht F, Schneider H (1996) High temperature behaviour of polycrystalline aluminosilicate fibres with mullite bulk composition. i. microstructure and strength properties. J Eur Ceram Soc 16:281–285

    Article  Google Scholar 

  14. Wang Y, Cheng H, Liu H, Wang J (2013) Microstructure and room temperature mechanical properties of mullite fibers after heat-treatment at elevated temperatures. Mater Sci Eng A 578:287–293

    Article  Google Scholar 

  15. Wood TE, Wilson DM (1989) Microcrystalline alumina-based ceramic articles. US Patent 4,954,462.

  16. Richards EA, Goodbrake CJ, Sowman HG (1991) Reactions and microstructure development in mullite fibers. J Am Ceram Soc 74:2404–2409

    Article  Google Scholar 

  17. Song KC (1999) Preparation of mullite fibers by the sol-gel method. J Sol-Gel Sci Technol 13:1017–1021

    Article  Google Scholar 

  18. Chen X, Gu L (2009) Spinnablity and structure characterization of mullite fibers via sol-gel-ceramic route. J Non Cryst Solids 355:2415–2421

    Article  Google Scholar 

  19. Liao S, Bai X, Song J, Zhang Q, Ren J, Zhao Y, Wu H (2017) Draw-spinning of kilometer-long and highly stretchable polymer submicrometer fibers. Adv Sci 4:1600480

    Article  Google Scholar 

  20. Leivo J, Lindén M, Rosenholm JM, Ritola M, Teixeira CV, Levänen E, Mäntylä TA (2008) Evolution of aluminosilicate structure and mullite crystallization from homogeneous nanoparticulate sol-gel precursor with organic additives. J Eur Ceram Soc 28:1749–1762

    Article  Google Scholar 

  21. Beran A, Voll D, Schneider H (2001) Dehydration and structural development of mullite precursors: An FTIR spectroscopic study. J Eur Ceram Soc 21:2479–2485

    Article  Google Scholar 

  22. Ksapabutr B, Gulari E, Wongkasemjit S (2004) Sol-gel transition study and pyrolysis of alumina-based gels prepared from alumatrane precursor, Colloids. Surf A Physicochem Eng Asp 233:145–153

    Article  Google Scholar 

  23. Jing C, Zhao X, Zhang Y (2007) Sol-gel fabrication of compact, crack-free alumina film. Mater Res Bull 42:600–608

    Article  Google Scholar 

  24. Dong X, Liu J, Li X, Zhang X, Xue Y, Liu J, Guo A (2017) Electrospun mullite nanofibers derived from diphasic mullite sol, J Am Ceram Soc 100:3425–3433.

  25. Jiang R, Liu H, Yang L, Sun X, Cheng H (2018) Mechanical properties of aluminosilicate fiber heat-treated from 800 °C to 1400 °C: Effects of phase transition, grain growth and defects. Mater Charact 138:120–126

    Article  Google Scholar 

  26. Borer A, Krogseng GP (1973) Method of firing dry spun refractory oxide fibers. US Patent 3,760,049.

Download references

Acknowledgements

We gratefully acknowledge the financial support from the “Chang Jiang Scholars Program” of the Ministry of Education of China (Grant no. T2011119).

Author information

Authors and Affiliations

Authors

Corresponding authors

Correspondence to Juan Wang, Qingshan Cai or Yunzhu Ma.

Ethics declarations

Conflict of interest

The authors declare that they have no conflict of interest.

Additional information

Publisher’s note: Springer Nature remains neutral with regard to jurisdictional claims in published maps and institutional affiliations.

Rights and permissions

Reprints and permissions

About this article

Check for updates. Verify currency and authenticity via CrossMark

Cite this article

Gao, Y., Liu, W., Song, X. et al. Preparation, characterization and mechanical properties of continuous mullite fibers derived from the diphasic sol-gel route. J Sol-Gel Sci Technol 92, 75–83 (2019). https://doi.org/10.1007/s10971-019-05078-0

Download citation

  • Received:

  • Accepted:

  • Published:

  • Issue Date:

  • DOI: https://doi.org/10.1007/s10971-019-05078-0

Keywords

Navigation