We report the successful synthesis of monodispersed Cu₂S nanocrystals and the subsequent formation of highly ordered nanocrystal superlattices. The synthesis is performed under ambient air conditions using simple experimental setups, making the process both accessible and scalable. By systematically tuning the reaction temperature and duration, we demonstrate precise control over the nanocrystal size, which is crucial in achieving uniformity and monodispersity. Furthermore, we uncover a previously unidentified nanocrystal growth mechanism that plays a key role in producing highly monodisperse Cu₂S nanocrystals. This insight into the growth process enhances our fundamental understanding of nanocrystal formation and could be extended to the synthesis of other semiconductor nanomaterials. The self-assembly of these nanocrystals into superlattices is carefully examined using electron diffraction techniques, revealing the presence of pseudo-crystalline structures. The ordered arrangement of nanocrystals within these superlattices suggests strong interparticle interactions and opens up new possibilities to tailor their collective optical, electronic, and mechanical properties for potential applications in optoelectronics, nanomedicine, and energy storage.

We report a simple synthesis process for a wide variety of ultrasmall nanocrystals. Simply immersing a dialysis bag containing an aqueous solution of a metal salt mixed with citric acid in a NaOH solution reservoir for 10 min, nanocrystals measuring only a few nanometers in size are formed inside the dialysis bag. We demonstrated the synthesis of ultrasmall nanocrystals of Co, Ni, Cu, Ag, Au, Pd, Cu₂O, FeO, and CeO₂, and found that the gradual change in pH caused by the diffusion of OH⁻ ions through the dialysis membrane played an essential role in the formation of these nanocrystals. This method can be readily adapted for almost all transition metal elements, providing researchers in the fields of catalysis and nanomedicine an easy access to a wide range of ultrasmall metal and oxide nanocrystals.

Copper-deficient copper selenide (Cu_2−xSe) nanocrystals possess strong near-infrared (NIR) absorption and efficient photothermal conversion, making them attractive candidates for photoacoustic imaging. In this study, Cu_2−xSe nanocrystals with distinct morphologies were synthesized using different selenium precursors and evaluated as photoacoustic contrast agents. Se–oleylamine precursors produced predominantly disk-shaped nanocrystals with average dimensions of approximately 20 nm in diameter and 5 nm in thickness, while Se–TOP/TOPO precursors yielded smaller spherical nanocrystals. Structural characterization by transmission electron microscopy, high-resolution TEM, and selected-area electron diffraction confirmed the formation of highly crystalline copper-deficient Cu_2−xSe nanocrystals with a face-centered cubic crystal structure. UV–Vis–NIR spectroscopy revealed broad optical absorption extending into the NIR region, with morphology-dependent spectral characteristics. Multispectral optoacoustic tomography demonstrated strong photoacoustic signal generation from both nanodisks and nanospheres over a broad wavelength range. In vivo studies using PEGylated Cu_2−xSe nanospheres showed successful lymphatic uptake following hind paw injection and enabled visualization of the draining popliteal lymph node through spectral unmixing of nanoparticle and hemoglobin signals. These results demonstrate that Cu_2−xSe nanocrystals are promising photoacoustic contrast agents for lymphatic imaging and other biomedical imaging applications.