Nanoscaled ZnO was synthesized by an electrochemical process using zinc or Al-alloyed zinc electrodes in an aqueous system with acetic acid as a conductive salt. Depending on the synthetical parameters, the precipitated precursor solids were found to consist of various compounds such as zincite, presumably
δ-Zn(OH)
2
, β
1
-Zn(OH)
2
, ε-Zn(OH)
2
, Zn
5
(CO
3
)
2
(OH)
6
and, in case an Al-alloyed electrode was used for the synthesis, Zn
0.71
Al
0.29
(OH)
2
(CO
3
)
0.145
·xH
2
O. The intermediate solids served as precursors for the subsequent thermal treatment resulting in zincite powders with various morphologies. Depending on the processing conditions, zincite was formed between 100 and 260 °C with a mean crystallite size between 6 and 25 nm. Selected zincite powders were pressed to pellets, sintered at temperatures between 900 and 1,100 °C and characterized by measurements of the electrical bulk conductivities, yielding values up to 1.69 S cm
−1
in samples with 1.24 wt% Al. Comparison with samples prepared by precipitation methods showed that the latter had values of up to 44 S cm
−1
.