Abstract
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.
Highlights
Inorganic materials’ synthesis, remarkably boosted by the requirement for robust, reproducible, and up-scalable approaches to materials’ development, supporting the energetic transition and renewable energies’ conversion and storage, is currently experiencing an actual renaissance aimed at matching a sustainable and green approach to synthesis with the demand for highly performing, stable, long-lasting, cost-effective and possibly multifunctional inorganic materials [1–4]
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 produced by sustainable wet chemistry routes based on a multi-parameter experimental landscape
The mentioned combined effect of temperature and pressure on dielectric constant, viscosity, and density of a suspension used for hydrothermal synthesis [16–18] would firstly require a deep understanding of the relation between temperature and pressure on the mentioned chemical–physical properties of the dispersing medium and secondly of the influence these experimental parameters have on the dissolution/reprecipitation phenomena occurring during the synthesis and eventually on the outcomes of the synthesis itself, in terms of crystallinity and built crystalline phase, composition, and yield of the product(s) [14,15,19,20]
Summary
Inorganic materials’ synthesis, remarkably boosted by the requirement for robust, reproducible, and up-scalable approaches to materials’ development, supporting the energetic transition and renewable energies’ conversion and storage (e.g., catalysts, fuel cells, batteries, photovoltaics, etc.), is currently experiencing an actual renaissance aimed at matching a sustainable and green approach to synthesis with the demand for highly performing, stable, long-lasting, cost-effective and possibly multifunctional inorganic materials [1–4]. The chemist approaches the research to optimise well-established and known recipes by continuously tuning and optimizing previous results and achievements This safer approach, simple and generally well accepted by literature, is, resource and time consuming and experimentally demanding, when different parameters contribute in an interrelated fashion to affect the synthesis output, though their specific role is hardly identified. To reduce the experimental effort required for the synthesis optimisation, instead of a time- and resources-demanding systematic screening of all involved experimental parameters, a more rational approach is required In this regard, a well-established and promising methodology, based on statistics, is the Design of Experiments (DoE) [25–29] in which an impartial multi-variable analysis is carried out, thoroughly uncorrelated from user know-how, aseptic and focused only to boost the product yield in terms of sustainability (both environmental as well as economic) and efficiency, where the full experimental space can be truly explored.
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