Synthesis, characterization, mechanical and magnetic characteristics of Gd<sup>3+</sup> /PO<sub>4</sub> <sup>3</sup> <sup>-</sup> substituted zircon for application in hard tissue replacements.

M, Ezhilan; Alam, M Mushtaq; Vijayalakshmi, U; Gupta, Somlee; Dhayalan, Arunkumar; Kannan, S · J Biomed Mater Res B Appl Biomater · 2024

biomechanical · Level V

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Abstract

The study reports on the use of sol-gel technique to yield zircon type [Zr<sub>(1-0.1-x)</sub> GdxTi<sub>0.1</sub> ] [(SiO<sub>4</sub> )<sub>1-x</sub> (PO<sub>4</sub> )<sub>x</sub> ] solid solution. Titanium has been used as a mineralizer to trigger zircon formation while equimolar concentrations of Gd<sup>3+</sup> and PO<sub>4</sub> <sup>3-</sup> were added to determine their accommodation limits in the zircon structure. The crystallization of t-ZrO<sub>2</sub> as a dominant phase alongside the crystallization of m-ZrO<sub>2</sub> and zircon were detected at 1200°C while their further annealing revealed the formation of zircon as a major phase at 1300°C. Heat treatment at 1400°C revealed the formation of zircon-type solid solution [Zr<sub>(1-0.1-x)</sub> Gd<sub>x</sub> Ti<sub>0.1</sub> ][(SiO<sub>4</sub> )<sub>1-x</sub> (PO<sub>4</sub> )<sub>x</sub> ] comprising the accommodation of 10 mol.% of Gd<sup>3+</sup> /PO<sub>4</sub> <sup>3-</sup> at the zircon lattice. Beyond 10 mol.% of Gd<sup>3+</sup> /PO<sub>4</sub> <sup>3-</sup> , the crystallization of GdPO<sub>4</sub> as a secondary phase is noticed. Structural analysis revealed the expansion of zircon lattice due to the simultaneous occupancy of Gd<sup>3+</sup> /PO<sub>4</sub> <sup>3-</sup> for the corresponding Zr<sup>4+</sup> /SiO<sub>4</sub> <sup>4-</sup> sites. The mechanical strength of single-phase zircon solid solution was higher in comparison to that of multiphase materials, namely in the presence of GdPO<sub>4</sub> formed as a secondary phase in samples with added equimolar Gd<sup>3+</sup> /PO<sub>4</sub> <sup>3-</sup> contents beyond 10 mol.%. Nevertheless, the paramagnetic behavior of the samples demonstrated a steady surge as a function of enhanced Gd<sup>3+</sup> content.

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