Abstract: | Synthesis of mini‐sized carbon nitride nanosheets (CNNSs) by traditional methods remains a challenge. Herein, size‐tunable and uniform mini‐sized CNNSs are synthesized by hydrothermal carbonization of a single polyethyleneimine (PEI) precursor. The as‐obtained mini‐sized CNNSs possess uniform size, good hydrophilicity and abundant nitrogen active sites, which not only exhibit double excitation‐ and pH‐dependent fluorescence behaviors, but also two‐photon excitation fluorescence. áThe resulting CNNSs display low toxicity and can be efficiently delivered into live cells for two‐photon fluorescence imaging, offering great potential as fluorescence probes in biochemical applications. |