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ZnFe layered double hydroxide (LDH) was synthesized through which the [AuCl4](-) anions were directly intercalated in situ. Low temperature calcination converts the [AuCl4](-) intercalated LDH into an intimately mixed ZnFe metal oxides containing favorably dispersed Au nanoparticles. The unique microstructure exhibited substantially improved photocatalytic activity by more than 40 times compared to the baseline material intercalated with [CO3](2-). Such improvement is unprecedented among noble metal decorated photocatalyst materials and is elucidated based on the mechanisms of morphology evolution.

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