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This review was devoted to outlining the use and potential increasing application of the Design of Experiment (DoE) approach to the rational and planned synthesis of inorganic nanomaterials, with a particular focus on polycrystalline nanostructures (metal and alloys, oxides, chalcogenides, halogenides, etc.) produced by sustainable wet chemistry routes based on a multi-parameter experimental landscape. After having contextualised the stringent need for a rational approach to inorganic materials’ synthesis, a concise theoretical background on DoE is provided, focusing on its statistical basis, shortly describing the different sub-methodologies, and outlining the pros and cons of each. In the second part of the review, a wider section is dedicated to the application of DoE to the rational synthesis of different kinds of chemical systems, with a specific focus on inorganic materials.