Study of the Synthesis of Zirconia Powder from Zircon Sand obtained from Zircon Minerals Malaysia by Caustic Fusion Method

Istikamah Subuki(1*), Mimi Fazzlinda Mohsin(2), Muhammad Hussain Ismail(3), Fazira Suriani Mohamed Fadzil(4)

(1) Faculty of Chemical Engineering, Universiti Teknologi MARA, 40450 Shah Alam, Selangor, Malaysia
(2) Faculty of Chemical Engineering, Universiti Teknologi MARA, 40450 Shah Alam, Selangor, Malaysia
(3) Faculty of Mechanical Engineering, Universiti Teknologi MARA, 40450 Shah Alam, Selangor, Malaysia
(4) Industrial Centre of Innovation Nanotechnology, SIRIM Industrial Research, Lot 34, Jl. Hi-Tech 2/3, Kulim Hi-Tech Park, 09000 Kulim, Kedah, Malaysia
(*) Corresponding Author


The zircon powder from Zircon Minerals Malaysia is a pure premium grade zircon sand milled 1.5 µm that contain ZrSiO4, ZrO2, HfO2, SiO2, Al2O3, TiO2, and Fe2O3. The monoclinic zirconia powders were synthesized from the zircon sand of Zircon Minerals Malaysia, by caustic fusion method at calcination temperatures between 500 °C to 800 °C. The as-synthesized zirconia was characterized through X-Ray diffraction (XRD), scanning electron microscopy (SEM), thermogravimetric and differential thermal analysis (TG-DTA), and X-Ray fluorescence (XRF) techniques. The XRD results show two monoclinic phases of microcrystalline zirconia. Zirconia that was calcined at 600 °C obtained the highest value of ZrO2, which was 54.48%; followed by zirconia calcined at 700 °C, 800 °C, and 500 °C, which obtained the ZrO2 values of 53.58%, 52.41%, and 51.53%, respectively, based on the XRF analysis. As-synthesized zirconia showed monoclinic phases where the surface areas were 0.0635 m2/g, 0.135 m2/g, 0.0268 m2/g, and 0.0288 m2/g, for zirconia calcined at temperatures of 500 °C, 600 °C, 700 °C, and 800 °C, respectively. The surface structure of the powder that had been calcined at 600 C showed similarities with the commercial zirconia. The similarities of the synthesized zirconia and commercial zirconia showed that the zirconia powder could be synthesized using zircon sand by caustic fusion method, even though the content of zirconia was lower compared to that of the commercial zirconia powder.


zirconia; zircon sand; monoclinic; caustic fusion method

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[1] Sommers, A., Wang, Q., Han, X., T'Joen, C., Park, Y., and Jacobi, A., 2010, Ceramics and ceramic matrix composites for heat exchangers in advanced thermal systems—A review, Appl. Therm. Eng., 30 (11-12), 1277–1291.

[2] Gerhardt, L.C., and Boccaccini, A.R., 2010, Bioactive glass and glass-ceramic scaffolds for bone tissue engineering, Materials, 3 (7), 3867–3910.

[3] Mihai, L.L., Parlatescu, I., Gheorghe, C., Andreescu, C., Bechir, A., Pacurar, M., and Cumpata, C.N., 2014, In vitro study of the effectiveness to fractures of the aesthetic fixed restorations achieved from zirconium and alumina, Rev. Chim., 65 (6), 725–729.

[4] Bocanegra-Bernal, M.H., and de la Torre, S.D., 2002, Phase transitions in zirconium dioxide and related materials for high performance engineering ceramics, J. Mater. Sci., 37 (23), 4947–4971.

[5] Daou, E.E., 2014, The zirconia ceramic: Strengths and weaknesses, Open Dent. J., 8, 33–42.

[6] Della Bona, A., Pecho, O.E., and Alessandretti, R., 2015, Zirconia as a dental biomaterials, Materials, 8 (8), 4978–4991.

[7] Sōmiya, S., and Akiba, T., 1999, Hydrothermal zirconia powders: A Bibliography, J. Eur. Ceram. Soc., 19 (1), 81–87.

[8] Kljajević, L., Matović, B., Radosavljević-Mihajlović, A., Rosić, M., Bosković, S., and Devečerski, A., 2011, Preparation of ZrO2 and ZrO2/SiC powders by carbothermal reduction of ZrSiO4, J. Alloys Compd., 509 (5), 2203–2215.

[9] Yamagata, C., Andrade, J.B., Ussui, V., de Lima, N.B., and Paschoal, J.O.A., 2008, High purity zirconia and silica powders via wet process: Alkali fusion of zircon sand, Mater. Sci. Forum, 591-593, 771–776.

[10] Götsch, T., Wallisch, W., Stöger-Pollach, M., Klötzer, B., and Penner, S., 2016, From zirconia to yttria: Sampling the YSZ phase diagram using sputter-deposited thin films, AIP Adv., 6 (2), 025119.

[11] Rahmawati, F., Permadani, I., Soepriyanto, S., Syarif, D.G., and Heraldy, E., 2014, Double steps leaching and filtration in caustic fusion method to produce zirconia from local zircon concentrate, Proceedings of the 2014 International Conference on Physics and its Applications (ICOPIA-14), 99–102.

[12] Rahmawati, F., Permadani, I., Heraldy, E., Syarif, D.G., and Soepriyanto, S., 2016, Structure and morphological analysis of various composition of yttrium doped-zirconia prepared from local zircon sand, J. Phys. Conf. Ser., 776 (1), 012050.

[13] Apriany, K., Permadani, I., Syarif, D.G., Soepriyanto, S., and Rahmawati, F., 2016, Electrical conductivity of zirconia and yttrium-doped zirconia from Indonesian local zircon as prospective material for fuel cells, IOP Conf. Ser.: Mater. Sci. Eng., 107, 012023.

[14] Gusain, D., Singh, P.K., and Sharma, Y.C., 2016, Kinetic and equilibrium modelling of adsorption of cadmium on nano crystalline zirconia using response surface methodology, Environ. Nanotechnol. Monit. Manage., 6, 99–107.

[15] Srinivasan, R., De Angelis, R.J., Ice, G., and Davis, B.H., 1991, Identification of tetragonal and cubic structures of zirconia using synchrotron x-radiation source, J. Mater. Res., 6 (6), 1287–1292.

[16] Oliveira, A.P., and Torem, M.L., 2001, The influence of precipitation variables on zirconia powder synthesis, Powder Technol., 119 (2-3), 181–193.

[17] Gauna, M.R., Conconi, M.S., Gómez, S., Suárez, G., Aglietti, E.F., and Rendtorff, N.M., 2015, Monoclinic-tetragonal zirconia quantification of commercial nanopowder mixtures by XRD and DTA, Ceram.-Silik., 59 (4), 318–325.

[18] Brog, J.P., Chanez, C.L., Crochet, A., and Fromm, K.M., 2013, Polymorphism, what it is and how to identify it: A systematic review, RSC Adv., 3 (38), 16905–16931.

[19] Ning, S., Zhan, P., Xie, Q., Li, Z., and Zhang, Z., 2013, Room-temperature ferromagnetism in un-doped ZrO2 thin films, J. Phys. D: Appl. Phys., 46 (44), 445004.

[20] Simione, D., Baldinozzi, G., Gosset, D., Dutheil, M., Bulou, A., and Hansen, T., 2003, Monoclinic to tetragonal semireconstructive phase transition of zirconia, Phys. Rev. B, 67 (6), 064111.

[21] Zauner, R., 2006, Micro powder injection moulding, Microelectron. Eng., 83 (4-9), 1442–1444.

[22]  Yaqub, A., Savaniu, C., Janjua, N., and Irvine, J., 2013, Preparation via a solution method of La0.2Sr0.25Ca0.45TiO3 and its characterization for anode supported solid oxide fuel cells, J. Mater. Chem. A, 1 (45), 14189–14197.

[23] Stichert, W., and Schüth, F., 1998, Influence of crystallite size on the properties of zirconia, Chem. Mater., 10 (7), 2020–2026.

[24] Chuah, G.K., and Jaenicke, S., 1997, The preparation of high surface area zirconia — Influence of precipitating agent and digestion, Appl. Catal., A, 163 (1-2), 261–273.

[25] Nayak, N.B., and Nayak, B.B., 2016, Temperature-mediated phase transformation, pore geometry and pore hysteresis transformation of borohydride derived in-born porous zirconium hydroxide nanopowders, Sci. Rep., 6, 26404.

[26] Buyakova, S., Sablina, T., and Kulkov, S., 2015, Porosity and mechanical properties of zirconium ceramics, AIP Conf. Proc., 1688 (1), 030009.

[27] Manivasakan, P., Rajendran, V., Rauta, P.R., Sahu, B.B., and Panda, B.K., 2011, Synthesis of monoclinic and cubic ZrO2 nanoparticles from zircon, J. Am. Ceram. Soc., 94 (5), 1410–1420.


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