Kinetics of Crystallization and Microstructural Evolution of Commercial Fluorophlogopite Machinable Glass- Ceramics in the System SrO∙4MgO∙Al2O3∙ 6SiO2∙2MgF2 with Varying in B2O3

Year : 2025 | Volume : 12 | Issue : 03 | Page : 1 16
    By

    Priyabrata Manna,

  • Chandan Santra,

  • Tapas Kumar Ghosh,

  • P.K. Maiti,

  • Totan Ghosh,

  1. Assistant Professor, Department of Chemistry, Brainware University, 398, Ramkrishnapur Road, Barasat, Kolkata, West Bengal, India
  2. , Department of Chemistry, Brainware University, 398, Ramkrishnapur Road, Barasat, Kolkata, West Bengal, India
  3. Assistant Professor, Department of General Science & Huminities Calcutta Institute of Technology, Uluberia- Howrah, West Bengal, India
  4. Associate Professor, Ceramic Engineering Division, Department of Chemical Technology, University of Calcutta, 92 A. P. C. Road, Kolkata, West Bengal,, India
  5. Assistant Professor, Department of Applied Chemistry, Maulana Abul Kalam Azad University of Technology, Simhat, Haringhata, West Bengal, India

Abstract

Glass materials based on fluorophlogopite stoichiometry with varying concentrations of B₂O₃ were synthesized using the melt-casting method, followed by heat treatment at different crystallization temperatures. The resulting glass and glass–ceramic samples were characterized using differential thermal analysis (DTA), scanning electron microscopy (SEM), X-ray diffraction (XRD), and Fourier-transform infrared (FT-IR) spectroscopy. Kinetic analysis revealed that the activation energies required for the formation of glass–ceramics were 192.77 kJ mol⁻¹ and 210.47 kJ mol⁻¹, as calculated by the Kissinger and Ozawa methods, respectively. XRD analysis indicated the formation of strontium fluorophlogopite and strontium aluminum silicate as the predominant crystalline phases at elevated heat treatment temperatures. These phases exhibited high aspect ratios and an interlocking microstructure, as confirmed by SEM observations. FT-IR spectra of the glass samples with higher B₂O₃ content revealed the coexistence of B–O bonds in both BO₄ tetrahedral and BO₃ trigonal coordination, along with AlO₄ and SiO₄ tetrahedral units forming the glass network structure. The combined analysis of thermal, structural, and spectroscopic data highlights the influence of B₂O₃ concentration and heat-treatment parameters on the microstructural evolution and crystallization kinetics of fluorophlogopite-based glass–ceramics. This study demonstrates that optimizing the B₂O₃ content and controlled heat treatment enables the formation of interlocked crystalline phases with enhanced mechanical stability, offering potential for high-temperature and dielectric applications in advanced material systems.

Keywords: Glass-ceramics, powder XRD, SEM, crystallization temperature, microstructure

[This article belongs to Journal of Thin Films, Coating Science Technology & Application ]

How to cite this article:
Priyabrata Manna, Chandan Santra, Tapas Kumar Ghosh, P.K. Maiti, Totan Ghosh. Kinetics of Crystallization and Microstructural Evolution of Commercial Fluorophlogopite Machinable Glass- Ceramics in the System SrO∙4MgO∙Al2O3∙ 6SiO2∙2MgF2 with Varying in B2O3. Journal of Thin Films, Coating Science Technology & Application. 2025; 12(03):1-16.
How to cite this URL:
Priyabrata Manna, Chandan Santra, Tapas Kumar Ghosh, P.K. Maiti, Totan Ghosh. Kinetics of Crystallization and Microstructural Evolution of Commercial Fluorophlogopite Machinable Glass- Ceramics in the System SrO∙4MgO∙Al2O3∙ 6SiO2∙2MgF2 with Varying in B2O3. Journal of Thin Films, Coating Science Technology & Application. 2025; 12(03):1-16. Available from: https://journals.stmjournals.com/jotcsta/article=2025/view=233837


References

  1. Aitken B, Beall GH. Glass-ceramics. Mater Sci Technol. 1994; 11: 269–94.
  2. Beall GA. In: Hench LL, editors. Adv Nucleation Cryst Glass. Am Ceram Soc; 1972; 251.
  3. Machu W. Die physikalischen Eigenschaften des Emails [The physical properties of enamel]. In: Nichtmetallische Anorganische Überzüge [Non-Metallic Inorganic Coatings]. Vienna: Springer; 1952. p. 297-304. doi:10.1007/978-3-7091-5060-3_50. [German].
  4. Grossman DG. Machinable glass-ceramics based on tetrasilisic mica. J Am Ceram Soc. 1972; 55(9): 446–9.
  5. Radonjic LJ, Nicolic LJ. The effect of fluorine source and concentration on the crystallization of machinable glass-ceramics. J Eur Ceram Soc. 1991; 7(1): 11–6.
  6. Beall GH. Mica glass-ceramics. US Patent 3,689,293. 1972.
  7. Hoda SN, Beall GH. Alkaline earth mica glass-ceramics. In: Simmons JH, Uhlmann DR, editors. Adv Ceram. 1982; 2: 287–300.
  8. Beall GH, Hench LL, Freiman SW. Structure, properties, and nucleation of glass-ceramics. In: Adv. Nucleation Cryst. Glasses. J Am Ceram Soc. 1971; 5: 251–61.
  9. Greene K, Pomeroy MJ, Hampshire S, Hill R. Effect of composition on the properties of glasses in the K₂O–BaO–MgO–SiO₂–B₂O₃–MgF₂ system. J Non-Cryst Solids. 2003; 325(1–3): 193–205.
  10. James PF. Glass ceramics: new compositions and uses. J Non-Cryst Solids. 1995; 181(1–2): 1–15.
  11. James PF. In: Simmson JH, Uhlmann DR, Beall GH, editors. Nucleation and Crystallization in Glasses. Vol. 4. Adv Ceram J Am Ceram Soc; 1982.
  12. Honda W, Vogel W, Mortier WJ, Duvigneaud PH, Naessens G, Plumat E. A new type of phlogopite crystal in machinable glass-ceramics. Glass Technol. 1983; 24(6): 318–22.
  13. Mallik A, Maiti PK, Kundu P, Basumajumdar A. Influence of B₂O₃ on the crystallization behavior and microstructure of mica glass-ceramics in the system BaO–4MgO–Al₂O₃–6SiO₂–2MgF₂. J Am Ceram Soc. 2012; 95(11): 3505–3508.
  14. Hu A-M, Li M, Mao D-L. Crystallization of spodumene-diopside in the LAS glass ceramics with CaO and MgO addition. J Therm Anal Calorim. 2007; 90(1): 185–9.
  15. Henry J, Hill RG. Influence of alumina content on the nucleation, crystallization and microstructure of barium fluorphlogopite glass-ceramics. J Mater Sci. 2004; 39(7): 2499–507.
  16. Henry J, Hill RG. The influence of lithia content on the properties of fluorophlogopite glass-ceramics. I. Nucleation and crystallization behavior. J Non-Cryst Solids. 2003; 319(1–2): 1–12.
  17. Uno T, Kasuga T, Nakajima K. High strength mica-containing glass-ceramics. J Am Ceram Soc. 1991; 74(12): 3139–41.
  18. Uno T, Kasuga T, Nakayam S. Mechanical properties of barium mica-containing glass-ceramics. J Eur Ceram Soc. 1992; 100(1159): 315–9.
  19. Uno T, Kasuga T, Nakajima K, Ikushima AJ. Microstructure of Mica-Based Nanocomposite Glass-Ceramics. J Am Ceram Soc. 1993; 76(2): 539–541.
  20. Avrami M. Kinetics of phase change. I. General theory. J Chem Phys. 1939; 7(12): 1103–11.
  21. Avrami M. Kinetics of phase change. II. Transformation-time relations for random distribution of nuclei. J Chem Phys. 1940; 8(2): 212–4.
  22. Avrami M. Kinetics of phase change. III. Granulation, phase change and microstructure. J Chem Phys. 1941; 9(2): 177–84.
  23. Kissinger HE. Variation of peak temperature with heating rates in differential thermal analysis. J Res Natl Bur Stand. 1956; 57(4): 217–21.
  24. Kissinger HE. Reactions kinetics in differential thermal analysis. Anal Chem. 1957; 29(11): 1702–6.
  25. Ozawa T. Temperature control modes in thermal analysis. Pure Appl Chem. 2000; 72(11): 2083–99.
  26. Augis JA, Bennett JE. Calculation of the Avrami parameters for heterogeneous solid state reactions using a modification of the Kissinger method. J Therm Anal. 1978; 13: 283–92.
  27. Perez-Maqueda LA, Criado JM, Malek J. Combined kinetic analysis for the crystallization kinetics of non-crystalline solids. J Non-Cryst Solids. 2003; 320(1–3): 84–91.
  28. Merzbacher CI, White WB. The structure of alkaline earth aluminosilicate glasses as determined by vibrational spectroscopy. J Non-Cryst Solids. 1991; 130(1): 18–34.
Regular Issue Subscription Original Research
Volume 12
Issue 03
Received 08/07/2025
Accepted 17/07/2025
Published 17/09/2025
Publication Time 71 Days
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