Non-Isothermal Dehydration Kinetics of Diphasic Mullite Precursor Gel

Document Type : Research Article


1 Central University of South Bihar, Gaya, INDIA

2 Maulana Abul Kalam Azad University of Technology, Kalyani, INDIA


Aluminosilicate gel precursor having mullite composition was synthesized from inorganic salts of aluminum and silicon by employing the sol-gel method. Chemical analysis, surface area, and bulk density measurements were performed to characterize the dried gel. The course of the palletization was examined by FT-IR analysis which confirmed the diphasic nature of the gel. SEM and XRD analysis were performed to study microstructure and phase development. ThermoGravimetric (TG) analysis of the dried gel was performed at multiple heating rates and from the results obtained; kinetics of thermal dehydration was studied by applying Friedman differential and Kissinger-Akahira-Sunose integral isoconversional procedures. It was observed that the total dehydration process of the gel was accomplished by two different stages and both the stages followed second-order rate kinetics. The first stage was assigned to the dehydration of silicon hydroxide gel whereas the second stage was associated with aluminum hydroxide gel dehydration.


Main Subjects

[1] Catauro M., Dell’Era A., Ciprioti S. V., Synthesis, Structural, Spectroscopic and Thermoanalytical Study of Sol-Gel Derived SiO2-CaO-P2O5 Gel and Ceramic Materials, Thermochim. Acta., 625: 20-27 (2016).
[2] H-Escolano M., Ramis X., J-Morales A., J-Diaz M., Suay J., Study of the Thermal Degradation of Bioactive Sol-Gel Coatings for the Optimization of its Curing Process, J. Therm. Anal. Calorim., 107: 499-508 (2012).
[3] Biedunkiewicz A., Gabriel U., Figiel P., Grzesiak D., Application of Thermal Analysis in Nanotechnology,  J. Therm. Anal. Calorim., 101: 701-706 (2010).
[4] Maitra S., Das S., Ray R., Mitra N. K., Role of Some Transition Metal Cations on the Kinetics of Thermadehydration of Synthetic Zeolites, Ceram. Int., 34: 485-490 (2008). 
[5] Budrugeac P., Muşat V., Segal E., Non-Isothermal Kinetic Study on the Decomposition of Zn Acetate-Based Sol-Gel Precursor, J. Therm. Anal. Calorim., 88: 699-702 (2007).
[6] Want B., Ahmad F., Kotru P.N., Dielectric and Thermal Characteristics of Gel Grown Single Crystals of Ytterbium Tartrate Trihydrate, J. Mater. Sci., 42: 9324-9330 (2007).
[7] Jankovic B., Adnadevic B., Jovanovic J., Non-Isothermal Kinetics of Dehydration of Equilibrium Swollen poly(acrylic acid) hydrogel, J. Therm. Anal. Calorim., 82: 7-13 (2005).
[9] Vendange V., Colomban P., How to Tailor the Porous Structure of Alumina and Aluminosilicate Gels and Glasses, J. Mater. Res., 11: 518-528 (1996).
[10] Sinko K., Poppl L., Transformation of Aluminosilicate Wet Gel to Solid State, J. Solid. State. Chem., 165: 111-118 (2002).
[11] Leivo J., Meretoja V., Vippola M., Levänen E., Vallittu P., Mäntylä T.A., Sol–Gel Derived Aluminosilicate Coatings on Alumina as Substrate for Osteoblasts, Acta. Biomater., 2: 659-668 (2006).
[12] Leivo J., Lindén M., Rosenholm J.M., Ritola M., Teixeira C.V., Levänen E., Mäntylä, T.A., Evolution of Aluminosilicate Structure and Mullite Crystallization from Homogeneous Nanoparticulate Sol–Gel Precursor with Organic Additives, J. Eur. Ceram. Soc., 28: 1749-1762 (2008).
[13] Li S., Zhao X., An Y., Deng W., Hou G., Hao E., Zhou H., Chen J., Effect of Deposition Temperature on the Mechanical, Corrosive and Tribological Properties of Mullite Coating, Ceram. Int., 44: 6719-6729 (2018).   
[14] Islam S., Bidin N., Riaz S., Naseem S., Sanagi M. M., Low Temperature Sol-Gel Based Erbium Doped Mullite Nanoparticles: Structural and Optical Properties, J. Taiwan Inst. Chem. Eng., 70: 366-373 (2017).  
[15] Kaya C., Butler E.G., Selcuk A., Boccaccini A.R., Lewis M.H., Mullite (Nextel™ 720) Fibre-Reinforced Mullite Matrix Composites Exhibiting Favourable Thermomechanical Properties, J. Eur. Ceram. Soc., 22: 2333-2342 (2002).
[16] Mileiko S.T., Serebryakov A.V., Kiiko V.M., Kolchin A.A., Kurlov V.N., Novokhatskaya N.I., Single Crystalline Mullite Fibres Obtained by the Internal Crystallisation Method: Microstructure and Creep Resistance, J. Eur. Ceram. Soc., 29: 337-345 (2009).
[18] Vyazovkin S., Burnham A.K., Criado J.M., Pérez-Maqueda L.A., Popescu C., Sbirrazzuoli N., ICTAC Kinetics Committee Recommendations for Performing Kinetic Computations on Thermal Analysis Data, Thermochim. Acta., 520: 1-19 (2011).
[19] Velyana G., Zvezdova D., Vlaev L., Non-Isothermal Kinetics of Thermal Degradation of Chitin, J. Therm. Anal. Calorim., 111: 763-771 (2013).
[20] Roy J., Bandyapadhyay N., Das S., Maitra S., Studies on the Formation of Mullite from Diphasic Al2O3-SiO2 Gel by Fourier Transform Infrared Spectroscopy, Iran. J. Chem. Chem. Eng. (IJCCE), 30: 65-71 (2011).
[21] Roy J., Maitra S., Synthesis and Characterization of Sol-Gel Derived Chemical Mullite, J. Ceram. Sci. Tech., 5: 57-62 (2014). 
[22] Luo Y.R., “Comprehensive Handbook of Chemical Bond Energies”, CRC Press, Boca Raton, FL (2007).