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A gas-phase route such as molecular layer deposition has been applied for the first time to create a monolayer of metalorganic Eu(III) molecules on NiO oxide layer. The surface of the as-deposited NiO layer is activated using H 2 O/O 2 vapors, and then functionalized by anchoring molecules of the Eu complex working at different temperatures to favor the chemisorption process. The effects of the activation process and of the MLD temperature on the chemisorption of the Eu complex were evaluated through in-depth X-ray photoelectron and luminescence spectroscopy studies. These analyses allowed to define the stoichiometry of the Eu moiety chemisorbed on the surface and the optimization of an impressive strategy to the synthesis of hybrid metalorganic/inorganic systems. The hybrid system's luminescence properties have proved the monolayer's energy conversion phenomena and produced further information about the local environment around the Eu(III) anchored as a complex on the NiO surface. [Display omitted] • MLD has been applied for the first time to the synthesis of a monolayer on oxide substrates. • XPS measurements have confirmed the chemisorption of the Eu molecules to the NiO film substrate. • Luminescence measurements have proved the monolayer's energy conversion properties. • This approach represents a facile, time-saving method, scalable at industrial level, to produce hybrid inorganic/metalorganic systems. [ABSTRACT FROM AUTHOR]