Influence of Crucible Materials and Pre-Treatments on Nanocrystalline Na₂ZrO₃ Formation during Zirconia Recovery for Dental Applications

Abstract:

The structures of sodium zirconate were studied in this research, which formed after the alkali fusion process. In this process, zircon is decomposed using sodium hydroxide (NaOH) at high temperatures to separate zirconium from impurities, resulting in high-purity zirconia which has potential as a dental material. The study aims to control the formation of Na₂ZrO₃ phase and to minimize the reactions between Zircon, NaOH, and crucible materials, such as porcelain, silicon carbide (SiC), and alumina to prevent contamination. To enhance reaction efficiency, a pre-treatment process was introduced, including wet milling and NaOH leaching. Then, the pre-treated zircon sand was reacted with NaOH in a 1 ZrSiO₄ : 6 NaOH molar ratio. Results showed color changes in the crucibles, indicating interactions between crucible materials and NaOH. But there is no change observed in alumina crucible which means that it is not reacted with either NaOH or ZrSiO₄. Different pre-treatment and crucible materials influenced the crystal size of Na₂ZrO₃ phase which give the lowest crystal size of 24.69 nm when using porcelain crucible. After the recovery process was finished high-purity full tetragonal zirconia phase is achieved which can be further processed as a artificial dental application. In artificial tooth application, pure zirconia with high strength is needed, thus controlling crystal and grain sizes is a crucial factor which affect the properties.

• Periodical: Journal of Metastable and Nanocrystalline Materials (Volume 42)
• Pages: 35-43
• DOI: https://doi.org/10.4028/p-jB9waX
• Online since: November 2025
• Authors: Yoga Masdya, Mudzakkir Dioktyanto, Andyan Rafi Setopratama, Maharani Wahyuning Tyas, Nurul Taufiqu Rochman, Triwikantoro Triwikantoro*
• Keywords: Alkali Fusion, Crucible, Crystal Size, Natrium Zirconate, Zircon

References

[1] S. Raghavan et al., "Ta2O5/Nb2O5 and Y2O3 Co-doped Zirconias for Thermal Barrier Coatings," J. Am. Ceram. Soc., vol. 87, no. 3, p.431–437, 2004.

[2] J. Kašpar and P. Fornasiero, "Nanostructured materials for advanced automotive de-pollution catalysts," J. Solid State Chem., vol. 171, no. 1–2, p.19–29, 2003.

DOI: 10.1016/S0022-4596(02)00141-X

[3] J. Nawrocki, C. J. Dunlap, P. W. Carr, and J. A. Blackwell, "New Materials for Biotechnology: Chromatographic Stationary Phases Based on Zirconia," Biotechnol. Prog., vol. 10, no. 6, p.561–573, 1994.

DOI: 10.1021/bp00030a001

[4] Y. Mizutani et al., "From rare earth doped zirconia to 1 kW solid oxide fuel cell system," J. Alloys Compd., vol. 408–412, p.518–524, 2006.

DOI: 10.1016/j.jallcom.2004.12.177

[5] R. P. Vitti, A. Catelan, M. Amaral, and R. R. Pacheco, Zirconium in dentistry. Elsevier Ltd, 2019.

DOI: 10.1016/B978-0-08-102476-8.00014-1

[6] H. Aldila and Triwikantoro, "Size Variations of Zircon Sand in Synthesis Zirconia Using Alkali Fusion - Coprecipitation Method," Proceeding Int. Conf. Res. Implement. Educ. Math. Sci. 2015, no. May, p.37–43, 2015, [Online]. Available: http://eprints.uny.ac.id/id/eprint/21037.

[7] A. M. Abdelkader, A. Daher, and E. El-Kashef, "Novel decomposition method for zircon," J. Alloys Compd., vol. 460, no. 1–2, p.577–580, 2008.

DOI: 10.1016/j.jallcom.2007.06.032

[8] M. Abdullah, T. Triwikantoro, C. Umamah, and H. J. Andi, "THE effect of ph and calcination temperature on the zro2 phase formation from natural zircon sand of kereng pangi," J. Neutrino, vol. 13, no. 2, p.39–48, 2021.

DOI: 10.18860/neu.v13i2.10507

[9] K. A. El Barawy, S. Z. El Tawil, and A. A. Francis, "Alkali fusion of zircon sand," Trans. Institutions Min. Metall. Sect. C Miner. Process. Extr. Metall., vol. 109, no. JAN./APR., p.49–56, 2000.

DOI: 10.1179/mpm.2000.109.1.49

[10] C. F. Burmeister and A. Kwade, "Process engineering with planetary ball millss", Chem. Soc. Rev., vol. 42, no. 18, p.7660–7667, 2013.

DOI: 10.1039/c3cs35455e

[11] H. X. Kho, S. Bae, S. Bae, B.-W. Kim, and J. S. Kim, "Planetary Ball Mill Process in Aspect of Milling Energy," J. Korean Powder Metall. Inst., vol. 21, no. 2, p.155–164, 2014.

DOI: 10.4150/kpmi.2014.21.2.155

[12] A. W. Handoko, D. Darsono, and D. Darmanto, "Aplikasi Metode Self Potential untuk Pemetaan Sebaran Lindi di Wilayah Tempat Pembuangan Akhir (TPA) Putri Cempo Surakarta", Indones. J. Appl. Phys., vol. 6, no. 01, p.13, 2016.

DOI: 10.13057/ijap.v6i01.1792

[13] A. Daulay, Andriayani, Marpongahtun, and S. Gea, "Extraction silica from rice husk with naoh leaching agent with temperature variation burning rice husk", Rasayan J. Chem., vol. 14, no. 3, p.2125–2128, 2021.

DOI: 10.31788/RJC.2021.1436351

[14] A. A. Madfa, F. A. Al-Sanabani, N. H. Al-Qudami, J. S. Al-Sanabani, and A. G. Amran, "Use of Zirconia in Dentistry: An Overview", Open Biomater. J., vol. 5, no. 1, p.1–7, 2014.

DOI: 10.2174/1876502501405010001

[15] J. Liu, J. Song, T. Qi, C. Zhang, and J. Qu, "Controlling the formation of Na2ZrSiO5 in alkali fusion process for zirconium oxychloride production", Adv. Powder Technol., vol. 27, no. 1, p.1–8, 2016.

DOI: 10.1016/j.apt.2015.08.005

[16] S. A. Hassanzadeh-Tabrizi, "Precise calculation of crystallite size of nanomaterials: A review" J. Alloys Compd., vol. 968, no. August, p.171914, 2023.

DOI: 10.1016/j.jallcom.2023.171914

[17] C. Suryanarayana, "Mechanical alloying and milling", Prog. Mater. Sci., vol. 46, no. 1–2, p.1–184, 2001, doi: 10.1016/S0079-6425(99)00010-9. 18] M. Rabiei, A. Palevicius, A. Monshi, S. Nasiri, A. Vilkauskas, and G. Janusas, "Comparing methods for calculating nano crystal size of natural hydroxyapatite using X-ray diffraction," Nanomaterials, vol. 10, no. 9, p.1–21, 2020.

DOI: 10.3390/nano10091627

[19] M. S. Hossain, M. Mahmud, M. Bin Mobarak, S. Sultana, M. A. A. Shaikh, and S. Ahmed, "New analytical models for precise calculation of crystallite size: application to synthetic hydroxyapatite and natural eggshell crystalline materials," Chem. Pap., vol. 76, no. 11, p.7245–7251, 2022.

DOI: 10.1007/s11696-022-02377-9