Modifying the Stöber Process: Is the Organic Solvent Indispensable?

The Stöber method is one of the most important and fundamental processes for the synthesis of inorganic (nano)materials but has the drawback of using a large amount of organic solvent. Herein, ethanol was used as an example to explore if the organic solvent in a typical Stöber method can be omitted. It was found that ethanol increases the particle size of the obtained silica spheres and aids the formation of uniform silica particles rather than forming a gel. Nevertheless, the results indicated that an organic solvent in the initial synthesis mixture is not indispensable. An initially immiscible synthesis method was discovered, which can replace the organic solvent‐based Stöber method to successfully synthesize silica particles with the same size ranges as the original Stöber process without addition of organic solvents. Moreover, this process can be of further value for the extension to synthesis processes of other materials based on the Stöber process. Organic solvents are not indispensable in the Stöber method and its extensions. Ethanol produced from the hydrolysis of tetraethyl orthosilicate (TEOS) already makes the reactants miscible and completes the synthesis. A simple organic solvent‐free alternative to the Stöber process enables the synthesis of controllable uniform silica spheres and has the potential to be extended to other Stöber process‐based material syntheses.