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La2O3–CeO2–Fe3O4composite nanofibers (LCF NFs) were fabricated via a facile electrospinning - calcination approach, and evaluated as an adsorbent for defluoridation from aqueous solution under batch mode. The pseudo-second-order (PSO) model described defluoridation characteristics well under 20 and 50 mg/L. F−adsorption under 288.15–308.15 K obeyed the Langmuir adsorption isotherm better with the maximum uptakes of 202.43–229.89 mg/g, respectively. The obtained thermodynamics constants involving Gibbs free energies change (ΔG < 0), enthalpy (ΔH9.90 kJ/mol), and entropy (ΔS56.63 J/mol/K) unveiled that the defluoridation process was spontaneous natural as well as endothermic. After four repeated cycles, the developed LCF11 NFs revealed favorable regeneration ability, indicating that LCF11 NFs are auspicious and stable candidates for defluoridation of wastewater.