Carbon nanoparticles (CNPs) have emerged as one of the most promising nanomaterials due to their distinct optoelectronic properties for a diverse range of applications in the area of electronics, energy conversion/ storage, and bio-imaging. The uniqueness in terms of functions and properties of the CNPs gets more interesting as it changes distinctly with a change in the shape, size, and dimensionality of these nanoparticles. The synthetic methods reported until now involves high-temperature (>100 °C) processes, which often results in uncontrolled shape, size, and polydispersity. In this work, we focus on the development of a low-temperature synthetic method for the preparation of fluorescent carbon nanoparticles allowing precise control over the shape, size, and properties by dispersion polymerization of acetylene as a precursor. The shape- and size-tunable nanoparticles were synthesized in a single step with dispersion polymerization by Glaser-Hay coupling. The shape and size of the resulting carbon nanoparticles are controlled by changing different reaction parameters such as temperature, reaction time and pressure. The control over the different reaction parameters allows us to obtain monodisperse CNPs in spherical (and tubular) shape with a size in the range of 25 nm to 250 nm. The use of low-temperature methods (RT < T < 70 °C) also allows us to overcome the limitations associated with current methods. After isolation, CNPs were characterized by microscopy techniques to analyze their shape and size. The nanoparticles were further characterized to by various techniques for chemical composition, structure, morphology, and optical properties. The residual alkynes in the CNPs' structure were exploited for further post-functionalization/graphitization to yield multifunctional CNPs, which were fluorescent in the blue region.