• Vol 8, No 8 (2017)
  • Metalurgy and Material Engineering

Formation and Particle Growth of TiO2 in Silica Xerogel Glass Ceramic During a Sintering Process

H Aripin, Joni I Made, Seitaro Mitsudo, Sudiana I Nyoman, Edvin Priatna, Nundang Busaeri, Svilen Sabchevski

Cite this article as:
Aripin, H., I Made, J., Mitsudo, S., I Nyoman, S., Priatna, E., Busaeri, N., Sabchevski, S., 2017. Formation and Particle Growth of TiO2 in Silica Xerogel Glass Ceramic During a Sintering Process. International Journal of Technology. Volume 8(8), pp.1507-1515
H Aripin - Department of Electrical Engineering, Faculty of Engineering, Siliwangi university, Tasikmalaya, Indonesia
Joni I Made Nano Technology and Graphene Research Center (NTGRC), Padjadjaran University, Bandung, Indonesia
Seitaro Mitsudo Research Center for Development of Far Infrared Region (FIR Center), University of Fukui, Fukui, Japan
Sudiana I Nyoman Department of Physics, Faculty of Mathematics and Natural Sciences, University of Haluoleo, Kendari, Indonesia
Edvin Priatna Department of Electrical Engineering, Faculty of Engineering, Siliwangi University, Tasikmalaya, Indonesia
Nundang Busaeri Department of Electrical Engineering, Faculty of Engineering, Siliwangi University, Tasikmalaya, Indonesia
Svilen Sabchevski Lab. Plasma Physics and Engineering, Institute of Electronics of the Bulgarian Academy of Sciences, Bulgaria.
Email to Corresponding Author


This investigation presents the synthesis procedure and the results of an investigation of the crystallite growth of TiO2 and the formation of Si–O–Ti bonds in novel silica xerogel (SiO2) glass ceramic produced from an amorphous SX derived from sago waste ash. The composition had been prepared by adding various amounts of TiO2, from 20 wt% to 80 wt%, into the amorphous SiO2, and then a series of samples were sintered at 1200°C for 2 hours. The influence of the content of TiO2 and the sintering temperature on the properties of TiO2, namely crystallite size and formation of Si–O–Ti bonds, has been studied in detail. The properties of the produced ceramics have been characterized on the basis of the experimental data obtained using X-ray diffraction (XRD) and Fourier transform infrared (FTIR) spectroscopy. It has been found that an addition of SiO2 confers an appreciable effect on the quantity of Si–O–Ti bonds. The interpretation of the XRD pattern allows one to explain the increase in the crystallite size of rutile TiO2 by a decreased quantity of Si–O–Ti bonds.

Composite of TiO2-SiO2; Crystallite size; Silica xerogel; Si–O–Ti bond; Rutile TiO2; TiO2


We have successfully developed a novel composite ceramic by incorporating TiO2 in silica xerogel converted from sago waste ash. In the experiments, the content of TiO2 and the sintering temperature have been varied in order to study their influence on the properties of the produced ceramic. The results have confirmed that a complete transformation from the anatase to the rutile TiO2 phase occurs at 1200°C. A significant effect of SiO2 on the crystalline growth of rutile TiO2 is clearly observed at lower concentrations of SiO2, a finding which has not been reported before (Aripin et al., 2016). It has also been found that the formation of large quantities of Si–O–Ti bonds results in a significant decrease in the size of rutile crystallites. The results presented in this work show that the incorporation of 20 wt% to 80 wt% TiO2 into SiO2 at a temperature of 1200°C causes an appreciable effect on the crystallite size of rutile TiO2.


This research was supported by a fund of the Siliwangi University through the Project of Research for Guru Besar in 2016 (Contract number: 1140/D3/PL/2016) and was carried out in collaboration with the Nano Technology and Graphene Research Center (NTGRC), Padjadjaran University. The authors would like to thank the research team from the NTGRC for kindly helping to prepare the sintering of the samples.


Affandi, S., Setyawan, H., Winardi, S., Purwanto, A., Balgis, R., 2009. A Facile Method for Production of High-purity Silica Xerogels from Bagasse Ash. Advanced Powder Technology, Volume 20, pp. 468–472

Aripin, H.,  Mitsudo, S.,  Sudiana, I.N.,  Tani, S., Sako, K., Fujii, Y., Saito, T., Idehara, T., Sabchevski, S., 2011. Rapid Sintering of Silica Xerogel Ceramic Derived from Sago Waste Ash using Sub-millimeter Wave Heating with a 300 GHz CW Gyrotron. J. Infrared Millimeter and Terahertz Waves, Volume 32, pp. 867–876

Aripin, H., Mitsudo, S., Sudiana, I.N., Busaeri, N., Sunendar, B., Sabchevski, S., 2016. Structural Characterization of a Glass Ceramic Developed from TiO2 and a Novel Material-silica Xerogel Converted from Sago Waste Ash. Materials Science Forum, Volume 872, pp. 81–86

Aripin, H., Mitsudo, S., Prima, E.S., Sudiana, I.N., Tani, S., Sako, K., Fujii, Y., Saito, T.,  Idehara, T., Sano, S., Sunendar, B., Sabchevski, S., 2012. Structural and Microwave Properties of Silica Xerogel Glass-ceramic Sintered by Sub-millimeter Wave Heating using a Gyrotron. J. Infrared Millimeter and  Terahertz Waves, Volume 33, pp. 1149–1162

Aripin, H., Mitsudo, S., Sudiana, I.N., Priatna, E., Kikuchi, H., Sabchevski, S., 2016. Densification Behavior of SnO2-glass Composites Developed from Silica Xerogel and SnO2. International Journal of Technology, Volume 7(3), pp. 401–440

Arun, D., Merline Shyla, J., Xavier, F.P., 2012. Synthesis and Characterization of TiO2/SiO2 Nano Composites for Solar Cell Applications. Applied Nanoscience, Volume 2, pp 429–436

Aziz, R.A., Sofyan, I., 2009. Synthesis of TiO2-SiO2 Powder and Thin Film Photocatalysts by Sol Gel Method. Indian Journal of Chemistry, Volume 48A, pp. 951–957

Balachandaran, K., Venckatesh, R., Sivaraj, R., 2010. Synthesis of Nano TiO2-SiO2 Composite using Sol-gel Method: Effect on Size, Surface Morphology and Thermal Stability. International Journal of Engineering Science and Technology, Volume 2, pp. 3695–3700

Chen, Y., Lee, C., Yeng, M., Chiu, H., 2003. The Effect of Calcination Temperature on the Crystallinity of TiO2 Nanopowders. Journal of Crystal Growth, Volume 247, pp. 363–370

CRC Handbook of Chemistry and Physics, 2006. ed., Lide D.R., Taylor and Francis, Boca Raton, Internet version, Available online at http://wwwhbcnetbasecom 

Duy, P.P., Kim, K.K., Cao, V.T., Van, Q.V., Thi, T.V., 2014. Preparation and Structural Characterization of Sol-gel-derived Silver Silica Nanocomposite Powders. International Journal of Materials Science and Applications, Volume 3, pp. 147–151

El-Toni, A.M., Yin, S., Sato, T., 2006. Control of Silica Shell Thickness and Microporosity of Titania–silica Core–shell Type Nanoparticles to Depress the Photocatalytic Activity of Titania. Journal of Colloid and Interface Science, Volume 300, pp. 123–130

JCPDS-International Centre for Diffraction Data, 1997. PCPDFWIN: Volume 1.30

Mahyar, A., Ali Behnajady, M., Modirshahla, N., 2010. Characterization and Photocatalytic Activity of SiO2-TiO2 Mixed Oxide Nanoparticles Prepared by Sol Gel Method. Indian Journal of Chemistry, Volume 49A, pp. 1593–1600

Marinela, S., Hyun Choia, D., Heuguet, R., Agrawala, D., Lanagana, M., 2013. Broadband Dielectric Characterization of TiO2 Ceramics Sintered through Microwave and Conventional Processes. Ceramics International, Volume 39, pp. 299–306

Nilchi, A., Janitabar-Darzi, S., Rasouli-Garmarodi, S., 2011. Sol-gel Preparation of Nanoscale TiO2/SiO2 Composite for Eliminating of Con Red Azo Dye. Materials Sciences and Applications, Volume 2, pp. 476–480

Riazian, M., Montazeri, N., Biazar, E., 2011. Nano Structural Properties of TiO2-SiO2. Oriental Journal of Chemistry, Volume 27, pp. 907–910

Shumaila, I., Rahman, R.A., Riaz, S., Naseem, S., Othaman, Z., Saeed, M.A., 2015. High Surface Area SiO2-TiO2 Nano-composite as pH Sensor. Sensor and Actuator B: Chemical, Volume 221, pp. 993–1002

Syahrial, A.Z., Priyono, B., Yuwono, A.H., Kartini, E., Jodi, H., Johansyah, 2016. Synthesis of Lithium Titanate (Li4Ti5O12) by Addition of Excess Lithium Carbonate (Li2CO3) in Titanium Dioxide (TiO2) Xerogel. International Journal of Technology, Volume 7(3), pp. 392–400

Vishwas, M., Narasimha Rao, K., Arjuna Gowda, K.V., Chakradhar, R.P.S., 2011. Optical, Electrical and Dielectric Properties of TiO2–SiO2 Films Prepared by a Cost Effective Sol–gel Process. Spectrochimica Acta Part A, Volume 83, pp. 614–617

Viswanath, R.N., Ramasamy, S., 1998. Study of TiO2 Nanocrystalline in TiO2-SiO2 Composites. Colloid and Surface A, Volume 133, pp. 49–56

Wagh, P.B., Ingale, S.V., 2002. Comparison of Some Physico-chemical Properties of Hydrophilic and Hydrophobic Silica Aerogels. Ceramic International, Volume 28, pp. 43–50

Wang, X., Masumoto, H., Someno, Y., Hirai, T., 1999. Microstructure and Optical Properties of Amorphous TiO2–SiO2 Composite Films Synthesized by Helicon Plasma Sputtering. Thin Solid Films, Volume 338, pp.105–110

Xue, S.H., Xie, H., Ping, H.,  Li, Q., Su, B.,  Fu, Z., 2015. Induced Transformation of Amorphous Silica to Cristobalite on Bacterial Surfaces. RSC Advances, Volume 5, pp. 71844–71848

Yang, L., Lai, Y., Chen, J.S., Tsai, P.H., 2005. Compositional Tailored Sol-Gel SiO2–TiO2 Thin Films: Crystallization, Chemical Bonding Configuration, and Optical Properties. Journal of Material Research, Volume 20, pp. 3141–3149

Yang, S., Gao, L., 2006. Facile and Surfactant-free Route to Nanocrystalline Mesoporous Tin Oxide. Journal of the American Ceramic Society, Volume 89, pp. 1742–1744

Yuwono, A.H., Zhang, Y., Wang, J., 2010. Investigating the Nanostructural Evolution of TiO2 Nanoparticles in the Sol-gel Derived TiO2-Polymethyl Methacrylate Nanocomposites. International Journal of Technology, Volume 1(1), pp. 11–19