Determination of the Nucleation and Crystallization Parameters for Making Nanoporous Titanium Phosphate Glass-ceramics


1 Material Engineering, Malayer University

2 Materials Science & Engineering, Tabriz University


Nanoporous glass-ceramics were prepared with composition 45CaO-25TiO2-35P2O5 (mol%). Two molar percent of Na2O was added as a flux to the composition. With the aforementioned composition, glass melted and crystallized into glass-ceramics containing β-Ca3(PO4)2 and CaTi4(PO4)6 as the main phases. The differential thermal analysis (DTA) was conducted to determine the suitable temperatures for nucleation and crystallization. Various times were examined for nucleation and the best nucleation time was chosen. The microstructure of final nucleated sample was observed by Scanning Electron Microscopy (SEM). Then, the glasses were crystallized and identified by X-ray Diffraction (XRD).The microstructures of crystallized specimens were studied by SEM.The glass-ceramics were leached in HCl, resulting β-Ca3(PO4)2 was dissolved out leaving a porous structure as CaTi4(PO4)6. It was found that specific surface area and average pore size diameter of the nanoporous glass-ceramics were controlled by the correct choice of heat treatment parameters. Using the optimal conditions for the production of nanoporous glass-ceramics with minimum pore size, 26 m2 and 12.3  were obtained for the specific surface area and pore diameter, respectively.


Main Subjects

1. Hosono, H. and Abe, Y., "Porous glass-ceramics composed of a titanium phosphate crystal skeleton: A review", Journal of Non-Crystalline Solids, Vol. 190, (1995), 185–197.

2. Hosono, H., Zhang, Z. and Abe, Y., "Porous Glass-Ceramic in the CαO–TiO2–P2O5 System", Journal of the American Ceramic Society, Vol. 72, (1989), 1587–1590.

3. Soleimani, F. and Rezvani, M., "The effects of CeO2 addition on crystallization behavior and pore size in microporous calcium titanium phosphate glass ceramics", Materials Research Bulletin, Vol. 47, (2012), 1362–1367.

4. Ray, C.S. and Day, D.E., "Identifying internal and surface crystallization by differential thermal analysis for the glass-tocrystal transformations", Thermochimica Acta, Vol. 280, (1996), 163–174.

5. Arias-Egido, E. Sola, D., Pardo, J.A., Martínez, J.I., Cases, R. nd Peña, J.I., "On the control of optical transmission of aluminosilicate glasses manufactured by the laser floating zone technique", Optical Materials Express, Vol. 6, (2016), 2413– 2421.

6. Baird, J.A., Santiago-Quinonez, D., Rinaldi, C. and Taylor, L. S., "Role of Viscosity in Influencing the Glass-Forming Ability of Organic Molecules from the Undercooled Melt State" Pharmaceutical Research, Vol. 29, (2012), 271–284.

7. Hu, L. and Jiang, Z., "Relation between low temperature viscosity and crystallization kinetics of glasses", Materials Research Bulletin, Vol. 26, (1991), 421–425.

8. Thieme, K., Avramov, I. and Rüssel, C., "The mechanism of deceleration of nucleation and crystal growth by the small addition of transition metals to lithium disilicate glasses", Scientific Reports, Vol. 6, (2016), 25451.

9. Hosono, H., Sakai, Y. and Abe, Y., "Pore size control in porous glass-ceramics with skeleton of NASICON-type crystal CaTi4(PO4)6", Journal of Non-Crystalline Solids, Vol. 139, (1992), 90–92.

10. Kousaka, Y., Nomura, T. and Alonso, M., "Simple model of particle formation by homogeneous and heterogeneous nucleation", Advanced Powder Technology, Vol. 12, (2001), 291–309.

11. Soleimani, F., Aghaei, A.R., Zakeri, M., Eshraghi, M.J. and Alizadeh, M., "Production of glass-ceramic from high frequency induction melted cordierite glass", Journal of Non-Crystalline Solids, Vol. 429, (2015), 219–225.

12. Banijamali, S., Aghaei, A.R. and Yekta, B.E., "Improving glassforming ability and crystallization behavior of porous glassceramics in CaO–Al2O3–TiO2–P2O5 system", Journal of Non- Crystalline Solids, Vol. 356, (2010), 1569–1575.

Volume 3, Issue 3
Summer 2017
Pages 26-31
  • Receive Date: 23 August 2017
  • Revise Date: 14 July 2019
  • Accept Date: 12 December 2017