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Orthorhombic Sc 2 (MoO 4) 3 nanofibers have been prepared by ethylene glycol assisted electrospinning method. The effects of annealing temperature, precursor concentration, spinning distance and solvent on the preparation of Sc 2 (MoO 4) 3 nanofibers were characterized by XRD, SEM, HRTEM, EDX and high-temperature XRD. XRD analysis shows as-prepared nanofibers are amorphous. Orthorhombic Sc 2 (MoO 4) 3 nanofibers can be fabricated after annealing at different temperatures in 500–800 °C for 2 h. The crystallinity of Sc 2 (MoO 4) 3 nanofibers improves and the nanofiber diameter decreases gradually as the annealing temperature increases. However, the nanofiber structure was destroyed at the annealing temperature above 700 °C. Higher precursor concentration results in a slight increase of diameter and decrease in destroying temperature of Sc 2 (MoO 4) 3 nanofibers. Spinning distance also affects the diameter of nanofibers, and the nanofiber diameter decreases as the distance increases. One-dimensional orthorhombic Sc 2 (MoO 4) 3 nanofibers exhibit anisotropic negative thermal expansion. In 25–700 °C, the coefficients of thermal expansion (CTE) of α a , α b and α c are −5.81 × 10−6 °C−1, 4.80 × 10−6 °C−1 and -4.33 × 10−6 °C−1, and the α l of Sc 2 (MoO 4) 3 nanofibers is −1.83 × 10−6 °C−1. [ABSTRACT FROM AUTHOR]