In the search for alternative anode materials for Li-ion batteries with high power densities, titanium(IV) oxide has emerged as an attractive candidate in recent years. Pristine and Fe-doped titanium dioxide nanoparticles were synthesized using a solvothermal route employing titanium(IV) tert-butoxide and acetic acid as the capping agent. The use of acetic acid provides a scalable synthesis medium that avoids difficulties in removing the entraining agent, often encountered with longer-chain carboxylic acids. The synthesis incorporates a one-pot carbon- and copper-coating strategy designed to improve the electronic conductivity of the composites. Fe-doping and coating strategies both demonstrated improved electrochemical performance in Li-ion half-cells over extended cycling.