In this work, the laser-based synthesis and characterization of Mo nanoparticles formed using Kr–F laser pulse photolysis of the vapor of Mo(CO)6 diluted by argon at room temperature were carried out. The time-resolved laser-induced incandescence (Ti–Re LII) technique was applied for the sizing of aerosolized particle inside of the quartz reactor. The samples of synthesized Mo nanoparticles were analyzed by transmission electron microscopy (TEM). The particle sizes measured by Ti–Re LII were found to be in a range of 3–13 nm in dependence on excimer Kr–F laser pulse energy and number of pulses. The temperature time behavior of laser-heated nanoparticles was observed by two-color pyrometry at the wavelengths 400 and 610 nm. The maximum particle temperature attained at high laser fluences was attributed to evaporation temperature and was found to be around 3,900 K unlike the boiling temperature of bulk Mo (4,800 K). The probable influence of nanoparticle properties on the results of Ti–Re LII sizing and nanoparticle oxidation in air on the results of TEM measurements is discussed.
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