NaFe(SO4)2 materials partially substituted with SeO42−, HPO42− and PO3F2− were prepared and investigated as possible cathode materials for sodium-ion batteries. Neutron diffraction and Raman spectroscopy studies confirmed the successful incorporation of SeO42− and HPO42−, while the Raman studies suggested that significant hydrolysis of PO3F2− had occurred during the synthesis. The effective diffusion coefficients were determined from conductivity and electrochemical kinetics studies, showing low Na ion diffusion. Galvanostatic and cyclic voltammetry investigations demonstrated more significant degradation and a narrowing of the electrochemical stability window for the doped materials, which was most significant for the SeO4 and HPO4 doped samples. Therefore, while doped NaFe(SO4)2 were successfully prepared, the best electrochemical performance was shown for the undoped system.