This study presents a facile and rapid method for synthesizing novel Layered Double Hydroxide (LDH) nanoflakes, exploring their application as a photocatalyst, and investigating the influence of condensed phosphates’ geometric linearity on their photocatalytic properties. Herein, the MgO film, obtained by plasma electrolysis of AZ31 Mg alloys, was modified by growing an LDH film, which was further functionalized using cyclic sodium hexametaphosphate (CP) and linear sodium tripolyphosphate (LP).