In this study, a facile one-pot solid-state synthesis method is developed to shed light on the metal-enhanced fluorescence (MEF) effect in carbon quantum dots (CQDs) and gold nanoparticles (AuNPs) hybrid materials. This is one of the few studies on the solid-state synthesis of N-doped CQDs/gold hybrid nanomaterials. We have conducted various sets of experiments to reveal the role of individual reagents during the nucleation and growth of nanoparticles. We have demonstrated that the addition of a small amount of gold salt illustrates a paramount effect (10 3 -fold) in photoluminescence intensity. This effect is ascribed to MEF, which is caused due to interactions between the excited-state fluorophores and the free surface electrons of metal nanoparticles. It is interesting to note that a further increase of gold yields fluorescence quenching due to a large number of formed AuNPs causing fluorescence resonance energy transfer. By adjusting the volume ratio of gold salt and CD precursors, it is possible to obtain the CQDs−AuNPs hybrid with the highest fluorescence, which produces extensive visible light under 460 nm excitation. Synthesized materials have been successfully used for imaging human dermal fibroblasts and A549 lung epithelial cells. The dose-dependent cytotoxicity studies reveal that the hybrid structures do not have cytotoxicity.