The morphology of metal oxide nanostructures influences the response of the materials in a given application. In addition to changing the composition, doping can also modify the morphology of a host nanomaterial. Herein, we determine the effect of dopant concentration, reaction temperature, and reaction time on the morphology and assembly of Cox
O nanoparticles synthesized through non-aqueous sol-gel in benzyl alcohol. With the increase of the atom % of cobalt incorporated from 0 to 15, the shape of the nanoparticles changes from near spherical, to irregular, and finally to triangular. The tendency of the particles to assemble increases in the same direction, with Co0.05
O consisting of non-assembled particles, whereas Co0.15
O consists of triangular nanoparticles forming spherical structures. The morphology and assembly process are also sensitive to the reaction temperature. The assembly process is found to occur during the nucleation or the early stages of particle growth. The cobalt ions promote the change in the shape during the growth stage of the nanoparticles.
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