Ultra-small multifunctional KGdF4:Tm3+,Yb3+ nanoparticles with near-infrared to near-infrared upconversion are synthesized. The average sizes of KGdF4:Tm3+ 2%, Yb3+ 20% core-only and KGdF4:Tm3+ 2%, Yb3+ 20%/KGdF4 core–shell nanoparticles are ∼3.7 nm and ∼7.4 nm, respectively, which fall within the reported optimal sizes (<10 nm) for bioimaging probes. The excitation and emission at 980 and 803 nm are favorable to deeper tissue penetration and reduced autofluorescence. The weak upconversion luminescence of the ultra-small core-only nanoparticles is overcome by the use of the core–shell approach. The magnetic mass susceptibility and magnetization of the ultra-small core-only and core–shell nanoparticles were determined, and are close to those of large nanoparticles (26 and 50 nm) used for magnetic resonance imaging and bio-separation. There is no variation in the magnetic properties with the nanoparticles’ sizes between the core-only (∼3.7 nm) and core–shell (∼7.4 nm) nanoparticles, which differs from the size-dependent luminescence. The oleate-capped core–shell nanoparticles were further encapsulated with a PEG-phospholipid shell to endow them with dispersibility in water, which is indispensable for future biological applications.
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