Microwave synthesis of upconverting nanoparticles with bis(2-ethylhexyl) adipate

Despite efforts to develop effective upconverting nanoparticle (UCNP) synthesis methods, there is still a need for approaches that are accessible and up-scalable while reproducibly providing fine control of UCNP size, crystallinity, and luminescence. This work presents a one-pot microwave-assisted strategy for synthesizing NaYF₄:Yb³⁺/Er³ UCNPs. A premixed rare earth (RE) solution in oleic acid (OA) was used to enhance repeatability while testing various synthesis conditions. The stock solution aliquots were mixed with OA and bis(2-ethylhexyl) adipate (BEHA), a polycarboxylic ester with a high boiling point, high thermal stability, and moderately polar character that facilitated rapid microwave heating at an average rate (room temperature to 300 °C) up to 60 °C min⁻¹. Combinations of BEHA concentration and high-temperature reaction time were identified for consistently producing cubic and hexagonal UCNPs with narrow size distributions in the tens and hundreds of nanometers. After washing, the resulting UCNPs were dispersible in aqueous media without further processing. This straightforward, accessible, and repeatable microwave-assisted synthesis method holds potential for scaling up the production of UCNPs with well-defined size and crystallinity.