| Summary: | In the present work, AgCl microcrystals were obtained by solvothermal crystallization to investigate the effect of H<sup>+</sup>, Na<sup>+</sup>, K<sup>+</sup>, and different shape-tailoring agents (non-ionic: polyvinylpyrrolidone vs. anionic: sodium dodecyl sulfate) on the textural and photocatalytic properties of the samples. The crystallization process resulted in secondary products, such as Ag<sub>x</sub>O or Ag, AgClO<sub>3</sub>, AgClO<sub>4</sub>, which were further transformed during the photocatalytic tests. The most efficient photocatalyst (assessed for methyl orange degradation) was synthesized using HCl, as a chloride source and polyvinylpyrrolidone, as a shape-tailoring agent. Therefore, the ability of polyvinylpyrrolidone to enhance the photocatalytic activity was also investigated, and it was found that the addition of 0.6 g polyvinylpyrrolidone resulted in the most efficient photocatalyst. Moreover, Ag<sub>x</sub>O, being a charge separator, could play a critical role in the photocatalytic process, while reversibly transforming to Ag back and forth.
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