Skip to main content
SpringerLink
Log in

Rheological behavior, molecular structure of precursor and evolution mechanism: zirconia fibers from polyaceticzirconium precursors

  • Original Paper
  • Published:
Journal of Sol-Gel Science and Technology Aims and scope Submit manuscript

Abstract

Polycrystalline zirconia fibers with dense surface and good flexibility were achieved from polyaceticzirconium (abbreviated as PEZ) precursor fibers followed by steam pretreatment and post-calcination. PEZ was synthesized via a one-pot solid–liquid reaction between basic zirconium carbonate and glacial acetic acid in methanol. Rheological behavior of the precursor sol with different concentrations was investigated, the power law model was used to describe the rheological behavior more accurately, and the relationship between the rheology and the spinnability of sol was discussed particularly. For the polymeric structure of PEZ, acetic acid was used as chelating agent and the carboxyl group was acted as a bidentate bridging ligand, which was speculated by FT-IR analysis. The effect of the pretreatment atmosphere on the evolution of the precursor fibers and the microstructure of the final fibers was discussed. The acetate group was removed in the form of molecules, and the final fibers preheated under steam atmosphere had better densification and flexibility than those were not. In addition, crystallization process, phase composition and thermal decomposition were investigated by XRD, Raman spectra and TG/DSC.

Graphical Abstract

The preheated atmosphere exerts an important influence on the densification and flexibility of zirconia fibers. Under steam atmosphere, acetate group in the precursor fibers is removed in the form of molecules and zirconia fibers sintered at 1050 °C for 2 h have a dense surface. However, zirconia fibers not subjected to the steam pretreatment have a large number of voids on the surface due to the decomposition of the organics. Furthermore, the fibers preheated under steam atmosphere have better flexibility than those were not. Therefore, pretreatment under steam atmosphere is essential for the preparation of the dense and flexible fibers.

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

Access this article

Log in via an institution

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

Instant access to the full article PDF.

Institutional subscriptions

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. Miura N, Jin H, Wama R, Nakakubo S, Elumalai P, Plashnitsa VV (2011) Novel solid-state manganese oxide-based reference electrode for YSZ-based oxygen sensors. Sens Actuators B Chem 152:261–266

    Article  Google Scholar 

  2. Abakevičienė B, Žalga A, Tautkus S, Pilipavičius J, Navickas E, Kareiva A, Tamulevičius S (2012) Synthesis of YSZ thin films by the novel aqueous sol-gel citrate-precursor method. Solid State Ion 225:73–76

    Article  Google Scholar 

  3. Courtin E, Boy P, Piquero T, Vulliet J, Poirot N, Laberty-Robert C (2012) A composite sol–gel process to prepare a YSZ electrolyte for solid oxide fuel cells. J Power Sources 206:77–83

    Article  Google Scholar 

  4. Jiménez-Borja C, Matei F, Dorado F, Valverde JL (2012) Characterization of Pd catalyst-electrodes deposited on YSZ: influence of the preparation technique and the presence of a ceria interlayer. Appl Surf Sci 261:671–678

    Article  Google Scholar 

  5. Limarga AM, Shian S, Baram M, Clarke DR (2012) Effect of high-temperature aging on the thermal conductivity of nanocrystalline tetragonal yttria-stabilized zirconia. Acta Mater 60:5417–5424

    Article  Google Scholar 

  6. Yogo T (1990) Synthesis of polycrystalline zirconia fibre with organozirconium precursor. J Mater Sci 25:2394–2398

    Article  Google Scholar 

  7. Abe Y, Kudo T, Tomioka H, Gunji T, Nagao Y, Misono T (1998) Preparation of continuous zirconia fibres from polyzirconoxane synthesized by the facile one-pot reaction. J Mater Sci 33:1863–1870

    Article  Google Scholar 

  8. Takahiro G, Hiroshi Y, Takaaki H, Kyoko BK, Yoshimoto A (2000) Preparation of polyzirconoxane from zirconium oxychloride octahydrate and ethylene glycol as a precursor for zirconia ceramics. Appl Organomet Chem 14:119–126

    Article  Google Scholar 

  9. Li J, Jiao X, Chen D (2007) Preparation of Y-TZP ceramic fibers by electrolysis-sol–gel method. J Mater Sci 42:5562–5569

    Article  Google Scholar 

  10. Li J, Jiao X, Chen D (2007) Preparation of Zirconia fibers via a simple aqueous sol–gel method. J Dispers Sci Technol 28:531–535

    Article  Google Scholar 

  11. Abe Y, Tomioka H, Gunji T, Nagao Y, Misono T (1994) A one-pot synthesis of polyzirconoxane as a precursor for continuous zirconia fibres. J Mater Sci Lett 13:960–962

    Article  Google Scholar 

  12. Pullar RC, Taylor MD, Bhattacharya AK (2001) The manufacture of partially-stabilised and fully-stabilised zirconia fibres blow spun from an alkoxide derived aqueous sol-gel precursor. J Eur Ceram Soc 21:19–27

    Article  Google Scholar 

  13. Lu Q, Chen D, Jiao X (2002) Preparation and characterization of dense Pb1−xLaxTiO3 (x = 0.0–0.2) fibers through the sol-gel-related solvothermal process. J Mater Chem 12:687–690

    Article  Google Scholar 

  14. Zhang H, Hang Y, Qin Y, Yang J, Wang B (2014) Synthesis and characterization of sol–gel derived continuous spinning alumina based fibers with silica nano-powders. J Eur Ceram Soc 34:465–473

    Article  Google Scholar 

  15. Tsai MT (2002) Effects of hydrolysis processing on the character of forsterite gel fibers. Part I: preparation, spinnability and molecular structure. J Eur Ceram Soc 22:1073–1083

    Article  Google Scholar 

  16. Zhu LY, Yu G, Wang XQ, Xu D (2009) Preparation and characterization of TiO2 fiber with a facile polyorganotitanium precursor method. J Colloid Interface Sci 336:438–442

    Article  Google Scholar 

  17. Liu HY, Hou XQ, Wang XQ, Wang YL, Xu D, Wang C, Du W, Lü MK, Yuan DR (2004) Fabrication of high-strength continuous zirconia fibers and their formation mechanism study. J Am Ceram Soc 87:2237–2241

    Article  Google Scholar 

  18. Liu H-Y, Chen Y, Liu G-S, Pei S-G, Liu J-Q, Ji H, Wang R-D (2013) Preparation of high-quality zirconia fibers by super-high rotational centrifugal spinning of inorganic sol. Mater Manuf Process 28:133–138

    Article  Google Scholar 

  19. Sacks MD, Sheu R-S (1987) Rheological properties of silica sol-gel materials. J Non Cryst Solids 92:383–396

    Article  Google Scholar 

  20. Sakka S, Kamiya K (1982) The sol-gel transition in the hydrolysis of metal alkoxides in relation to the formation of glass fibers and films. J Non Cryst Solids 48:31–46

    Article  Google Scholar 

  21. Kamiya K, Yoko T (1986) Synthesis of SiO2 glass fibres from Si(OC2H5)4-H2O-C2H5OH-HCl solutions through sol–gel method. J Mater Sci 21:842–848

    Article  Google Scholar 

  22. Kozuka H, Kuroki H, Sakka S (1988) Flow characteristics and spinnability of sols prepared from silicon alkoxide solution. J Non Cryst Solids 100:226–230

    Article  Google Scholar 

  23. Wolf C, Rüssel C (1992) Sol–gel formation of zirconia: preparation, structure and rheology of sols. J Mater Sci 27:3749–3755

    Article  Google Scholar 

  24. de Sá Costa B, dos Reis Coimbra JS, Martins MA, Garcia-Rojas EE, Telis-Romero J, De Oliveira EB (2013) Rheological behavior of binary aqueous solutions of poly(ethylene glycol) of 1500 g mol−1 as affected by temperature and polymer concentration. J Chem Eng Data 58:838–844

    Article  Google Scholar 

  25. Zhang LM, Zhou JF, Hui PS (2005) Thickening, shear thinning and thixotropic behavior of a new polysaccharide-based polyampholyte in aqueous solutions. Colloids Surf A 259:189–195

    Article  Google Scholar 

  26. Yang H, Ruan J, Zou J, Wu Q, Zhou Z, Zhou Z (2009) Rheological responses of fumed silica suspensions under steady and oscillatory shear. Sci China Ser E Technol Sci 52:910–915

    Article  Google Scholar 

  27. Raghavan SR, Khan SA (1997) Shear-thickening response of fumed silica suspensions under steady and oscillatory shear. J Colloid Interface Sci 185:57–67

    Article  Google Scholar 

  28. Shao P, Qin M, Han L, Sun P (2014) Rheology and characteristics of sulfated polysaccharides from chlorophytan seaweeds Ulva fasciata. Carbohydr Polym 113:365–372

    Article  Google Scholar 

  29. Deacon GB, Phillips RJ (1980) Relationships between the carbon-oxygen stretching frequencies of carboxylato complexes and the type of carboxylate coordination. Coord Chem Rev 33:227–250

    Article  Google Scholar 

  30. Gazzoli D, Mattei G, Valigi M (2007) Raman and X-ray investigations of the incorporation of Ca2+ and Cd2+ in the ZrO2 structure. J Raman Spectrosc 38:824–831

    Article  Google Scholar 

  31. Uma Maheswari A, Mohan SR, Saravana Kumar S, Sivakumar M (2014) Phase tuning of zirconia nanocrystals by varying the surfactant and alkaline mineralizer. Ceram Int 40:6561–6568

    Article  Google Scholar 

  32. Herrera G, Montoya N, Domenech-Carbo A, Alarcon J (2013) Synthesis, characterization and electrochemical properties of iron-zirconia solid solution nanoparticles prepared using a sol-gel technique. Phys Chem Chem Phys 15:19312–19321

    Article  Google Scholar 

  33. Li M, Feng Z, Ying P, Xin Q, Li C (2003) Phase transformation in the surface region of zirconia and doped zirconia detected by UV Raman spectroscopy. Phys Chem Chem Phys 5:5326–5332

    Article  Google Scholar 

  34. Xu G, Zhang Y-W, Han B, Li M-J, Li C, Yan C-H (2003) Unusual calcination temperature dependent tetragonal–monoclinic transitions in rare earth-doped zirconia nanocrystals. Phys Chem Chem Phys 5:4008–4014

    Article  Google Scholar 

  35. Xu G, Zhang Y-W, Liao C-S, Yan C-H (2004) Doping and grain size effects in nanocrystalline ZrO2–Sc2O3 system with complex phase transitions: XRD and Raman studies. Phys Chem Chem Phys 6:5410–5418

    Article  Google Scholar 

  36. Quintard PE, Barbéris P, Mirgorodsky AP, Merle-Méjean T (2002) Comparative lattice-dynamical study of the raman spectra of monoclinic and tetragonal phases of zirconia and hafnia. J Am Ceram Soc 85:1745–1749

    Article  Google Scholar 

Download references

Acknowledgments

The authors acknowledge the financial support of the National Natural Science Foundations of China (Grant Nos. 51472144, 51372140 and 51102155), the Fundamental Research Funds of Shandong University (Grant No. 2015JC022) and the Youth Scientist Fund of Shandong Province (BS2011CL025).

Author information

Authors and Affiliations

  1. State Key Laboratory of Crystal Materials and Institute of Crystal Materials, Shandong University, Jinan, 250100, People’s Republic of China

    Hongjing Liu, Benxue Liu, Xinqiang Wang, Luyi Zhu, Cong Feng, Guanghui Zhang & Dong Xu

Authors
  1. Hongjing Liu
    View author publications

    You can also search for this author in PubMed Google Scholar

  2. Benxue Liu
    View author publications

    You can also search for this author in PubMed Google Scholar

  3. Xinqiang Wang
    View author publications

    You can also search for this author in PubMed Google Scholar

  4. Luyi Zhu
    View author publications

    You can also search for this author in PubMed Google Scholar

  5. Cong Feng
    View author publications

    You can also search for this author in PubMed Google Scholar

  6. Guanghui Zhang
    View author publications

    You can also search for this author in PubMed Google Scholar

  7. Dong Xu
    View author publications

    You can also search for this author in PubMed Google Scholar

Corresponding authors

Correspondence to Luyi Zhu or Dong Xu.

Rights and permissions

Reprints and permissions

About this article

Check for updates. Verify currency and authenticity via CrossMark

Cite this article

Liu, H., Liu, B., Wang, X. et al. Rheological behavior, molecular structure of precursor and evolution mechanism: zirconia fibers from polyaceticzirconium precursors. J Sol-Gel Sci Technol 76, 482–491 (2015). https://doi.org/10.1007/s10971-015-3797-y

Download citation

  • Received:

  • Accepted:

  • Published:

  • Issue Date:

  • DOI: https://doi.org/10.1007/s10971-015-3797-y

Keywords

Search

Navigation