Journal of Sol-Gel Science and Technology

, Volume 89, Issue 2, pp 426–435 | Cite as

The effect of calcination rate on the structure of mesoporous bioactive glasses

  • Saidur Rahman
  • Andrew Mendonca
  • Adel AlhalawaniEmail author
  • Deanna Polintan
  • Owen M. Clarkin
  • Mark R. Towler
Original Paper: Fundamentals of sol-gel and hybrid materials processing


Mesoporous bioactive glasses (MBGs) are designed to have high specific surface area. They are formulated by a sol–gel process to formulate the glass followed by calcination. This study evaluates how calcination heating rate influences the porous architecture, and thereby the specific surface area, of MBGs. MBGs of molar ratio 80:15:5 for SiO2:CaO:P2O5 were calcined using both low (1 °C/min) and high (20 °C/min) heating rates, termed as L-MBG and H-MBG, respectively. The results obtained from small-angle X-ray diffraction (SAXRD) confirm that the MBGs possess 2D hexagonal (P6mm) spacing groups and wide-angle XRD confirms the amorphicity of both MBGs. Energy-dispersive X-ray spectroscopy and X-ray photoelectron spectroscopy confirm that both batches of MBGs have similar chemical composition. Fourier transform infrared spectroscopy identifies the same functional groups present in both batches. However, transmission electron microscopy indicates that H-MBG samples exhibited discontinuities in their ordered channel structure, confirmed by the lower SAXRD peak intensity of H-MBG compared to L-MBG. These discontinuities led to a reduced surface area. L-MBG exhibits more than quadruple the surface area and double the pore volume (373.87 m2/g and 0.27 cm3/g) of H-MBG (85.91 m2/g and 0.13 cm3/g), measured through Brunauer, Emmett, and Teller nitrogen adsorption analysis. This higher surface area resulted in a significant (p < 0.05) increase in the quantity of ion release from the L-MBGs compared to the H-MBGs. It is concluded that the application of a low heating rate during calcination, of the order of 1 °C/min, is more likely to result in ordered mesoporous bioactive glasses with high surface area and pore volume than MBG samples processed at a higher heating rate.


  • Calcination rate (low or high) has no effect on the chemical composition of mesoporous bioactive glasses (MBGs).

  • Calcination rate influences the physical structure of MBGs.

  • Low calcination rate (1 °C/min) results in more ordered MBGs with higher surface area and pore volume compared to high calcination rate (20 °C/min).


Mesoporous bioactive glasses Sol–gel Calcination heating rate Glass surface area Glass pore volume 



The authors would like to thank the Canadian Institute of Health Research (CIHR) Project grant series [appl. # 366716. A novel approach to treating hemorrhage with mesoporous bioactive glasses] for Mr. Md. Saidur Rahman and Mr. Andrew Mendonca’s graduate stipends. We also appreciate the financial assistance of Ryerson’s Mechanical and Industrial Engineering Department for early assistance with Mr. Rahman’s stipend. We also would like to thank Audrey Darabie (University of Toronto, Department of Cell and Systems Biology) for her assistance with TEM. The BET analysis was carried out at the Nano Research Facility in Dublin City University which was funded under the Programme for Research in Third Level Institutions (PRTLI) cycle 5. The PRTLI is co-funded through the European Regional Development Fund (ERDF), part of the European Union Structural Funds Programme 2011–2015.

Compliance with ethical standards

Conflict of interest

Professor Mark R. Towler has received research grants from Canadian Institute of Health Research (CIHR), Project grant series [appl. # 366716. A novel approach to treating hemorrhage with mesoporous bioactive glasses]. The authors declare that they have no conflict of interest.


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Copyright information

© Springer Science+Business Media, LLC, part of Springer Nature 2018

Authors and Affiliations

  • Saidur Rahman
    • 1
    • 2
  • Andrew Mendonca
    • 2
    • 3
  • Adel Alhalawani
    • 1
    • 2
    Email author
  • Deanna Polintan
    • 2
    • 3
  • Owen M. Clarkin
    • 4
  • Mark R. Towler
    • 1
    • 2
  1. 1.Department of Mechanical and Industrial EngineeringRyerson UniversityTorontoCanada
  2. 2.Li Ka Shing Knowledge InstituteSt. Michael’s HospitalTorontoCanada
  3. 3.Department of Biomedical EngineeringRyerson UniversityTorontoCanada
  4. 4.School of Mechanical & Manufacturing EngineeringDublin City UniversityDublinIreland

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