The study reports on the use of sol-gel technique to yield zircon type [Zr(1-0.1-x) GdxTi0.1 ] [(SiO4 )1-x (PO4 )x ] solid solution. Titanium has been used as a mineralizer to trigger zircon formation while equimolar concentrations of Gd3+ and PO4 3- were added to determine their accommodation limits in the zircon structure. The crystallization of t-ZrO2 as a dominant phase alongside the crystallization of m-ZrO2 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(1-0.1-x) Gdx Ti0.1 ][(SiO4 )1-x (PO4 )x ] comprising the accommodation of 10 mol.% of Gd3+ /PO4 3- at the zircon lattice. Beyond 10 mol.% of Gd3+ /PO4 3- , the crystallization of GdPO4 as a secondary phase is noticed. Structural analysis revealed the expansion of zircon lattice due to the simultaneous occupancy of Gd3+ /PO4 3- for the corresponding Zr4+ /SiO4 4- sites. The mechanical strength of single-phase zircon solid solution was higher in comparison to that of multiphase materials, namely in the presence of GdPO4 formed as a secondary phase in samples with added equimolar Gd3+ /PO4 3- contents beyond 10 mol.%. Nevertheless, the paramagnetic behavior of the samples demonstrated a steady surge as a function of enhanced Gd3+ content.