This book presents a lucid and systematic exposition of the preparation, characterization, and spectroscopy of carbonaceous nanomaterials and started with the general introduction to nanoscience, review of carbon nanomaterials, and related experimental techniques. This book attempts to highlights to design new, inexpensive, and single step procedure for the bulk synthesis of carbon nanoparticles. Special attention was made to dispersion of carbon nanoparticles in variety of solvents, their growth kinetics, and interaction with surfactants, including common, bio and pulmonary surfactants. Interestingly the observation of fluorescent carbon nanoparticles from organic solvents dispersion without any surface functionalization and their detailed spectroscopic study also presented. This book will be useful for engineers, chemists, and nano-scientists interested to work in the area of carbon nanomaterials for application in their areas and also can be used as a textbook or used by students and carbon research groups on their own as long as they have some basic knowledge of carbon nanomaterials and fluorescence spectroscopy.