The Study of the Influence of ZrO<sub>2</sub> Precursor Type and the Temperature of Annealing on the Crystallization of the Tetragonal Polymorph of ZrO<sub>2</sub> in Zirconia-Silica Gels
Materials of the ZrO<sub>2</sub>-SiO<sub>2</sub> system were obtained by the sol-gel method applying two different types of ZrO<sub>2</sub> precursors: zirconium (IV) n-propoxide Zr(OC<sub>3</sub>H<sub>7</sub>)<sub>4</sub> and z...
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MDPI AG
2022-11-01
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| Online Access: | https://www.mdpi.com/2310-2861/8/11/724 |
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| author | Anna Adamczyk |
| author_facet | Anna Adamczyk |
| author_sort | Anna Adamczyk |
| collection | DOAJ |
| description | Materials of the ZrO<sub>2</sub>-SiO<sub>2</sub> system were obtained by the sol-gel method applying two different types of ZrO<sub>2</sub> precursors: zirconium (IV) n-propoxide Zr(OC<sub>3</sub>H<sub>7</sub>)<sub>4</sub> and zirconium (IV) acetate Zr(OOC<sub>2</sub>H<sub>3</sub>)<sub>4</sub> (organic acetic acid salt) while commonly used tetraethoxysilane TEOS was selected as SiO<sub>2</sub> introducing one. ZrO<sub>2</sub> concentration in synthesized samples varied from 20% to 50% (mol.). After drying for 28 days, all gels were annealed at 500 °C, 1000 °C, and 1200 °C in air. FTIR spectroscopy together with XRD diffraction was selected as the two main structure research methods. SEM microscopy was applied to analyze the local chemical compositions of samples and to observe the morphology of gels’ surfaces. The analysis of FTIR spectra and XRD diffraction patterns allowed us to recognize different ZrO<sub>2</sub> polymorphs which appeared in the samples depending strongly as well on ZrO<sub>2</sub> precursor type as on the temperature of annealing. Samples synthesized by using the zirconium (IV) n-propoxide contained both cubic and tetragonal zirconia phases in general but showed the tendency of the increasing <i>t</i>-ZrO<sub>2</sub> content in gels richer in ZrO<sub>2</sub> and heated up to 1200 °C. However, in materials obtained applying zirconium (IV) acetate, the first detected at 500 °C phase was <i>t</i>-ZrO<sub>2</sub> which was then conversing to <i>m</i>-ZrO<sub>2</sub> form with the increasing temperature in case of samples rich in ZrO<sub>2</sub>. Meanwhile, <i>t</i>-ZrO<sub>2</sub> was the predominant phase in samples of the lower content of ZrO<sub>2</sub> but annealed at higher temperatures. By the analysis of changes in band profiles and positions, one can draw conclusions that the structure of studied samples is mostly built up of an amorphous silica matrix, in which different types of zirconia polymorphs create their own crystal lattice. The presence of the particular polymorph depends strongly on the type of zirconia precursor and the temperature of annealing. |
| first_indexed | 2024-03-09T19:03:09Z |
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| spelling | doaj.art-0607472c4f0c4194a4e1e5be31d6115a2023-11-24T04:46:46ZengMDPI AGGels2310-28612022-11-0181172410.3390/gels8110724The Study of the Influence of ZrO<sub>2</sub> Precursor Type and the Temperature of Annealing on the Crystallization of the Tetragonal Polymorph of ZrO<sub>2</sub> in Zirconia-Silica GelsAnna Adamczyk0Faculty of Materials Science and Ceramics, AGH University of Science and Technology, Al. Mickiewicza 30, 30-059 Kraków, PolandMaterials of the ZrO<sub>2</sub>-SiO<sub>2</sub> system were obtained by the sol-gel method applying two different types of ZrO<sub>2</sub> precursors: zirconium (IV) n-propoxide Zr(OC<sub>3</sub>H<sub>7</sub>)<sub>4</sub> and zirconium (IV) acetate Zr(OOC<sub>2</sub>H<sub>3</sub>)<sub>4</sub> (organic acetic acid salt) while commonly used tetraethoxysilane TEOS was selected as SiO<sub>2</sub> introducing one. ZrO<sub>2</sub> concentration in synthesized samples varied from 20% to 50% (mol.). After drying for 28 days, all gels were annealed at 500 °C, 1000 °C, and 1200 °C in air. FTIR spectroscopy together with XRD diffraction was selected as the two main structure research methods. SEM microscopy was applied to analyze the local chemical compositions of samples and to observe the morphology of gels’ surfaces. The analysis of FTIR spectra and XRD diffraction patterns allowed us to recognize different ZrO<sub>2</sub> polymorphs which appeared in the samples depending strongly as well on ZrO<sub>2</sub> precursor type as on the temperature of annealing. Samples synthesized by using the zirconium (IV) n-propoxide contained both cubic and tetragonal zirconia phases in general but showed the tendency of the increasing <i>t</i>-ZrO<sub>2</sub> content in gels richer in ZrO<sub>2</sub> and heated up to 1200 °C. However, in materials obtained applying zirconium (IV) acetate, the first detected at 500 °C phase was <i>t</i>-ZrO<sub>2</sub> which was then conversing to <i>m</i>-ZrO<sub>2</sub> form with the increasing temperature in case of samples rich in ZrO<sub>2</sub>. Meanwhile, <i>t</i>-ZrO<sub>2</sub> was the predominant phase in samples of the lower content of ZrO<sub>2</sub> but annealed at higher temperatures. By the analysis of changes in band profiles and positions, one can draw conclusions that the structure of studied samples is mostly built up of an amorphous silica matrix, in which different types of zirconia polymorphs create their own crystal lattice. The presence of the particular polymorph depends strongly on the type of zirconia precursor and the temperature of annealing.https://www.mdpi.com/2310-2861/8/11/724ZrO<sub>2</sub>-SiO<sub>2</sub> systemsol-gel methodFTIR spectroscopyX-ray diffractionSEM<i>t</i>-ZrO<sub>2</sub> |
| spellingShingle | Anna Adamczyk The Study of the Influence of ZrO<sub>2</sub> Precursor Type and the Temperature of Annealing on the Crystallization of the Tetragonal Polymorph of ZrO<sub>2</sub> in Zirconia-Silica Gels Gels ZrO<sub>2</sub>-SiO<sub>2</sub> system sol-gel method FTIR spectroscopy X-ray diffraction SEM <i>t</i>-ZrO<sub>2</sub> |
| title | The Study of the Influence of ZrO<sub>2</sub> Precursor Type and the Temperature of Annealing on the Crystallization of the Tetragonal Polymorph of ZrO<sub>2</sub> in Zirconia-Silica Gels |
| title_full | The Study of the Influence of ZrO<sub>2</sub> Precursor Type and the Temperature of Annealing on the Crystallization of the Tetragonal Polymorph of ZrO<sub>2</sub> in Zirconia-Silica Gels |
| title_fullStr | The Study of the Influence of ZrO<sub>2</sub> Precursor Type and the Temperature of Annealing on the Crystallization of the Tetragonal Polymorph of ZrO<sub>2</sub> in Zirconia-Silica Gels |
| title_full_unstemmed | The Study of the Influence of ZrO<sub>2</sub> Precursor Type and the Temperature of Annealing on the Crystallization of the Tetragonal Polymorph of ZrO<sub>2</sub> in Zirconia-Silica Gels |
| title_short | The Study of the Influence of ZrO<sub>2</sub> Precursor Type and the Temperature of Annealing on the Crystallization of the Tetragonal Polymorph of ZrO<sub>2</sub> in Zirconia-Silica Gels |
| title_sort | study of the influence of zro sub 2 sub precursor type and the temperature of annealing on the crystallization of the tetragonal polymorph of zro sub 2 sub in zirconia silica gels |
| topic | ZrO<sub>2</sub>-SiO<sub>2</sub> system sol-gel method FTIR spectroscopy X-ray diffraction SEM <i>t</i>-ZrO<sub>2</sub> |
| url | https://www.mdpi.com/2310-2861/8/11/724 |
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