The preparation and application of hydrophobic carbon dots (HCDs) are now the hotspots in the field of nanomaterials. This paper reports the fast synthesis of long-wavelength-emitting HCDs (yellow-emitting, λ em = 541 nm) through a solid-phase route, with l -cysteine hydrochloride anhydrous and citric acid as carbon sources and dicyclohexylcarbodiimide as a dehydrating agent, reacting at 180 °C for 40 min, with a quantum yield of 30%. The solid-phase route avoids the usage of organic reagents during the synthesis process and is thus environmentally friendly. The obtained HCDs can be simply separated into HCDs-L (less density) and HCDs-W (higher density) with differences in physical (polarity, density), optical, and chemical properties. The differences in HCDs-L, HCDs-W, and water-soluble CDs (WCDs) were compared through various characterization methods, and the synthesis and luminescence mechanisms of HCDs were investigated. Meanwhile, HCDs were employed in the fields of LED lamp production and solid fluorescent shaping material. The prepared HCDs were then modified into WCDs through the liposomal embedding method. The HCDs prepared by the new solid-phase route exhibit stable and highly efficient photoluminescence ability and will have a promising outlook in their applications in various fields.
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