Athenian pottery, the ceramics produced in the Attica region of Greece between the 6th and 4th centuries B.C., is considered a benchmark technological achievement of the preindustrial world. This work advances our understanding of the firing protocols employed by the ancient Greeks to produce their black-on-red designs by characterizing replicates painted with a refined illite clay and fired under oxidizing/reducing/reoxidizing conditions (three-stage firing). Systematically varying the temperature, atmosphere, and duration of each firing stage within the three-stage firing scheme allowed the conditions necessary to obtain black and red gloss, both of which are observed on ancient vessels, to be determined. The morphology and elemental distribution of particles formed within the gloss thus formed were characterized using transmission electron microscopy and spectrocolorimetric measurements. Comparison of the results obtained from ancient sherds with those obtained from the replicate samples provides a means of estimating the firing conditions used to create the ancient vessels. Show Partial Abstract