Skip to main page content
U.S. flag

An official website of the United States government

Dot gov

The .gov means it’s official.
Federal government websites often end in .gov or .mil. Before sharing sensitive information, make sure you’re on a federal government site.

Https

The site is secure.
The https:// ensures that you are connecting to the official website and that any information you provide is encrypted and transmitted securely.

Access keys NCBI Homepage MyNCBI Homepage Main Content Main Navigation
. 2020 Jul 13;10(44):26165-26176.
doi: 10.1039/d0ra04824k. eCollection 2020 Jul 9.

Amorphous mesostructured zirconia with high (hydro)thermal stability

Bénédicte Lebeau  1   2 , Issam Naboulsi  3 , Laure Michelin  1   2 , Claire Marichal  1   2 , Séverinne Rigolet  1   2 , Cédric Carteret  4 , Sylvette Brunet  5 , Magali Bonne  1   2 , Jean-Luc Blin  3
Affiliations

Amorphous mesostructured zirconia with high (hydro)thermal stability

Bénédicte Lebeau et al. RSC Adv. .

Abstract

Here, combining the evaporation-induced self-assembly (EISA) method and the liquid crystal templating pathway, mesostructured amorphous zirconium oxides have been prepared by a soft templating method without addition of any heteroelement to stabilize the mesopore framework. The recovered materials have been characterized by SAXS measurements, nitrogen adsorption-desorption analysis and X-ray diffraction (XRD). The obtained mesostructured zirconia exhibits a high thermal stability. An in situ XRD study performed as a function of temperature shows that the amorphous ZrO2, obtained after removal of the pore templating agent (pluronic P123), begins to crystallize in air from 420 °C. Amorphous mesostructured ZrO2 also presents a high hydrothermal stability; these materials are not degraded after 72 hours in boiling water.

PubMed Disclaimer

Conflict of interest statement

There are no conflicts to declare.

Figures

Fig. 1
Fig. 1. Evolution of the SAXS pattern as a function of the P123/Zr(Opr)4 molar ratio (R). The P123 concentration in the acidic solution is fixed to 33 (A), 50 (B) and 60 wt% (C).
Fig. 2
Fig. 2. Variation of the nitrogen adsorption–desorption isotherms with the corresponding mesopores size distribution (inset) as a function of the P123/Zr(Opr)4 molar ratio (R). The P123 concentration in the acidic solution is fixed to 33 (A), 50 (B) and 60 wt% (C).
Fig. 3
Fig. 3. SAXS pattern (A); infrared (B) and Raman (C) spectra of the hybrid mesophase (a) and of the ZrO2 material obtained after ethanol extraction (b).
Fig. 4
Fig. 4. 13C MAS NMR spectra with 1H decoupling of as-synthesized (A) and dehydrated at 70 °C (B) ZrO2 hybrid mesophase.
Fig. 5
Fig. 5. XRD patterns of ZrO2 material obtained after ethanol extraction recorded in the 2θ 28–33° range at various temperatures from 25 °C to 900 °C and after cooling down at 25 °C.
Fig. 6
Fig. 6. Evolution of the SAXS pattern of amorphous mesostructured ZrO2 with the immersion time into boiling water.
Fig. 7
Fig. 7. Nitrogen adsorption–desorption isotherms with the corresponding mesopores size distribution after time of immersion into boiling water of amorphous mesostructured ZrO2.
Fig. 8
Fig. 8. Evolution of the specific surface area (■) and pore volume (◯) of amorphous mesostructured ZrO2 as a function of the immersion time. Lines are just a guide for the eyes.
See this image and copyright information in PMC

References

    1. Inoue Y. Yamazaki H. Bull. Chem. Soc. Jpn. 1987;60:891. doi: 10.1246/bcsj.60.891. - DOI
    1. Jaenicke S. Chuah G. K. Raju V. Nie Y. T. Catal. Surv. Asia. 2008;12:153. doi: 10.1007/s10563-008-9048-2. - DOI
    1. Srinivasan R. and Davis B. H., in Materials Synthesis and Characterization, ed. D. L. Perry, Springer Science+Business Media, New York, 1997, pp. 147–188
    1. Zhang C. Langmuir. 2009;25:7078. doi: 10.1021/la900146y. - DOI - PubMed
    1. Lin C. Zhang C. Lin J. J. Phys. Chem. C. 2007;111:3300. doi: 10.1021/jp066615l. - DOI