A highly scalable process has been developed for stabilizing large quantities of the zeta-polymorph of V2O5, a metastable kinetically trapped phase, with high compositional and phase purity. The process utilizes a beta-Cux V2O5 precursor which is synthetized from solution using all-soluble precursors. The copper can be leached from this structure by a room temperature post-synthetic route to stabilize an empty tunnel framework entirely devoid of intercalating cations. The metastable ζ-V2O5 thus stabilized can be used as a monovalent-(Li, Na) or multivalent-(Mg, Ca, Al) ion battery cathode material.