The present invention provides a process for producing a nanosemiconductor luminous material on a liquid-liquid interface, comprising the steps of: a) an oxide of a Group IIB metal and a carboxylic acid with 2-18 carbon atoms or an oleic acid reacting with each other in a solvent at 150-300.degree. C. for 5-30 min, wherein the mol ratio of the oxide to the acid being 1.about.5:5.about.1; b) adding trioctylphosphine oxide and trioctylphosphine with a mol ratio of trioctylphosphine oxide to trioctylphosphine of 10.about.1:1.about.10 and a mol ratio of the total mol numbers of trioctylphosphine oxide to the oxide of 10.about.1:1.about.10; c) adding an aqueous solution of at least one alkaline/alkaline earth metal chalcogenide in a mol ratio of the chalcogenide to the oxide of 10.about.1:1.about.10; and d) reacting at 20-100.degree. C. for 0.5.about.10 h to obtain a sol containing a semiconductor nanoparticle. The produced semiconductor nanoparticle can emit a wavelength-adjustable visible light under a UV lamp.