A novel solid solution, $\left(1-x\right)\mathrm{PbTi}{\mathrm{O}}_3-x\mathrm{TbFe}{\mathrm{O}}_3$ was investigated, with a specific composition of $\mathrm{x}=0.10$ exhibiting a giant negative coefficient of thermal expansion (CTE) of approximately $-68\times {10}^{-6}{}^{\circ }{\mathrm{C}}^{-1}$, with large volume contraction of about 2.5% over the temperature range $25-400{}^{\circ }\mathrm{C}$. The observed negative thermal expansion (NTE) magnitude surpasses that of other ${\mathrm{PbTiO}}_3$-based systems, being more than three times higher than pure ${\mathrm{PbTiO}}_3$. The enhanced NTE is linked to an anomalous change in the c-lattice parameter relative to the a-parameter, indicating structural modifications responsible for this behavior. Further, compositions within the range $0\le \mathrm{x}\le 0.10$ exhibit anomalous behavior in tetragonality retention, attributed to the combined influence of $\mathrm{P}{{\mathrm{b}}^{2+}}^{\prime }\mathrm{s} 6{\mathrm{S}}^2$ lone pair effect and strong Fe–O covalency, affecting structural stability.

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• Electric polarization
• Ferroelectricity
• Polycrystalline materials
• Neutron diffraction
• X-ray diffraction