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Abstract In this work, we present a study of the Langmuir film formation composed of hydrophobic carbon quantum dots (hCQDs). We studied the kinetics of hCQDs pyrolysis and optimized the reaction time for maximum photoluminescence. The resulting hCQDs were analyzed by transmission electron microscopy, X-ray photoemission spectroscopy and grazing-incidence X-ray diffraction. The process of monolayer formation was studied by monitoring surface pressure, surface potential, elastic modulus and Brewster angle microscopy in real time under continuous compression conditions. The monolayer transferred onto a silicon wafer was examined on the nano- and micro-scales by means of atomic force microscopy and confocal fluorescence microscopy, respectively.