Ce 3+ -doped Y 3 Al 5 O 12 (YAG:Ce) nanocrystals were synthesized by a unique solvothermal method, under sub-critical conditions. A home-made autoclave was used, operating in a larger pressure and temperature range than that with conventional commercial equipment and allowing direct in situ photoluminescence (PL) and X-ray absorption characterizations. The study of various synthesis conditions (pressure, temperature, precursor concentration, reaction time) allowed the best reaction conditions to be pinpointed to control YAG:Ce nanocrystal size, as well as crystal quality, and to get efficient optical properties. Without any post thermal treatment, we succeeded in obtaining wellcrystallized YAG:Ce nanocrystals (30-200 nm), displaying typical PL properties of YAG:Ce with a maximal emission at 550 nm. The pristine 100 nm-sized YAG:Ce nanoparticles present an internal quantum yield of about 40 AE 5%. In situ X-ray absorption near edge spectroscopy demonstrates the presence of Ce 4+ in nanocrystals elaborated at high temperature, resulting from the oxidation of Ce 3+ during the crystallization process. † Electronic supplementary information (ESI) available: Additional TEM images and nanocrystal size distribution histograms (.pdf le). A movie for the in situ visualization upon YAG nanocrystal synthesis (.mpeg le). SeeFig. 3 TEM images of YAG:Ce nanocrystals synthesized at different pressure with T ¼ 350 C, [Al] ¼ 0.09 mol L À1 and reaction time ¼ 150 min. Some individual nanocrystals are circled with yellow solid lines. An aggregate is circled with a white dashed line.This journal is
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