A FACILE ELECTROCHEMICAL EXFOLIATION METHOD [1-3] HAS BEEN INTRODUCED FOR SELECTIVE, HIGHLY PURE AND LARGE SCALE SYNTHESIS OF LUMINESCENT GRAPHENE QUANTUM DOTS (GQDS), CARBON NANODOTS (CDS) AND THEIR HYBRID. FOR THIS PURPOSE, AN AMPEROMETRIC DETECTION SYSTEM HAS BEEN SELECTED DURING APPLYING AN OPTIMUM DIRECT CURRENT (DC) POTENTIAL (+8.50 V) BETWEEN A TWO-ELECTRODE SYSTEM INCLUDING STAINLESS STEEL AS CATHODE AND GRAPHITE ROD AS ANODE UNDER OPTIMIZED CONDITION I.E. PH 7.0, 0.5M AND 1.0 M NACL SOLUTION. THE SYNTHESIZED CARBON NANOMATERIALS HAS BEEN CHARACTERIZED USING ANALYTICAL TECHNIQUES SUCH AS FOURIER-TRANSFORM INFRARED (FT-IR), TRANSMISSION ELECTRON MICROSCOPY (TEM), SCANNING ELECTRON MICROSCOPY (SEM), X-RAY DIFFRACTION (XRD), PARTICLE SIZE ANALYZER (PSA), XPS MEASUREMENTS, RAMAN SPECTROSCOPY, ETC. ACCORDING TO THE RESULTS, NO NANOMATERIALS ARE PRECIPITATED ATTIME SCALES LOWER THAN ~15 S, DUE TO THE UNSATURATION OF THE ELECTROLYTE SOLUTION. ACCORDING TO THE MICROSCOPIC IMAGES, THE CDS ARE THEN CONSIDERED AS THE UNIT CELL OF GQDS. THE COLOR OF THE ELECTROLYTE SOLUTION IS THEN CHANGED TO YELLOW DURING THE FORMATION OF LUMINESCENCE CDS.COAGULATION OF CDS LEADS TO THE FORMATION OF QCDS AT 20-45 S TIME DURATION AND ~1.0 M NACL SOLUTION. ACCORDING TO THE SCANNING ELECTRON MICROSCOPY (SEM), THE AVERAGE INTER-LAYER THICKNESS OF GQDS IS EVALUATED TO ~60 NM. IN THIS STUDY, AGING OF THE ELECTROCHEMICAL REACTION AS WELL AS ENHANCING THE ELECTROLYTE CONCENTRATION TO ~1.0 M NACL SEPARATES THE GQD’S SHEETS DURING THE SONICATION PROCESS AS WELL AS INTERCALATION OF THE NACL THAT RESULTS TO GET HYBRID (MIXTURE) OF CDS AND GQDS AT 300-600 S TIME DURATION AND PURE CDS AT TIMES HIGHER THAN ~600 S.