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By solid-phase synthesis, macrocrystalline Cu2 − δZn2 − xSnxS4 − ySey monograin powders have been prepared, the chemical composition of which was shown by XRD and Raman spectroscopy to be different in powder fractions of different sizes formed during the synthesis. The influence of synthesis conditions on the decay kinetics of photogenerated charge carriers in different fractions has been studied using the frequency–time-resolved microwave photoconductivity method. The characteristic photoresponse half-life, τ1/2, increased with increasing grain size. The smallest values of the lifetime were observed for the fraction with sizes of 50–70 μm (τ1/2 <5 ns), and the largest values were for the fraction with a grain size of 70–90 μm (τ1/2 ~ 12 ns). [ABSTRACT FROM AUTHOR]