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Orthorhombic In 0.5 Sc 1.5 Mo 3 O 12 thin films have been synthesized using the sol-gel spin coating. Influences of post-annealing temperatures on crystal structure, morphology, negative thermal expansion (NTE) and optical performances of the thin films were studied using XRD, SEM, XPS, high-temperature XRD and UV–Vis–NIR spectrophotometer. XRD and SEM results show that as-prepared thin film is in an amorphous state with a smooth and dense surface. Orthorhombic In 0.5 Sc 1.5 Mo 3 O 12 thin films were obtained after post-annealing in 550–750 °C. The higher the annealing temperature in 550–750 °C, the better the crystallinity of orthorhombic In 0.5 Sc 1.5 Mo 3 O 12 thin films. In addition, the grain size of the In 0.5 Sc 1.5 Mo 3 O 12 thin film also grows as the annealing temperature increases. The resulting orthorhombic In 0.5 Sc 1.5 Mo 3 O 12 thin films exhibit anisotropic NTE. Its volumetric coefficient of thermal expansion (CTE) is −3.44 × 10−6 °C−1, while the CTEs in a -, b - and c -axis directions are −4.70 × 10−6 °C−1, 5.37 × 10−6 °C−1, and -4.10 × 10−6 °C−1 in 25–700 °C, respectively. In addition, the transmittance of orthorhombic In 0.5 Sc 1.5 Mo 3 O 12 thin films post-annealed at 750 °C is around 87.75 %–95.03 %. [ABSTRACT FROM AUTHOR]