Efforts to mass-produce high-quality graphene sheets are crucial for advancing its practical and industrial applications across various fields. In this study, we present an innovative electrochemical exfoliation method designed to enhance graphene quality and increase yield. Our approach combines two key techniques: expanding the tightly packed graphite interlayer used as the electrode medium and precisely controlling voltage polarity. The dual-exfoliation technique optimizes the use of anions and cations of varying sizes in the electrolyte to facilitate meticulous intercalation, allowing ions to penetrate deeply and evenly into the graphite interlayer. The newly designed dual-exfoliation technique using biased switching polarity minimizes the generation of oxygen-containing radicals, while the incorporation of expanded graphite accelerates exfoliation speed and reduces oxidation, maintaining high graphene purity. With these improvements, we produced 1–3 layer graphene sheets with minimal defects ( ID/IG ≈ 0.13) and high purity (C/O ratio ≈ 20.51), achieving a yield 3.1 times larger than previously reported methods. The graphene sheets also demonstrated excellent electrochemical properties in a three-electrode system, with an electrical conductivity of 92.6 S cm− 1, a specific capacitance of 207.4 F g− 1, and a retention of 94.8% after 5,000 charge/discharge cycles, highlighting their superior stability and performance.

Achieving cost-effective and defect-free graphene sheets is highly desirable for sensor devices. Aiming this, few-layer graphene (~ 3) sheets are prepared by an electrochemical exfoliation with [NMP] [ HSO4] electrolyte (i.e., Bronsted acidic ionic liquid). A novel approach for the effective exfoliation of graphene sheets is demonstrated by (i) simultaneously applying a constant potential through an electrochemical cell (with different electrolyte concentrations) and (ii) together with sonication. The exfoliated graphene sheets are characterized through state-of-the-art techniques and sprayed on a glass substrate at optimum conditions. Thus, the transparent conducting sensor device is fabricated with a suitable contact electrode and used for ammonia vapor sensing and the sensor performances are highly dependent on the concentration of the ionic liquid used during the electrochemical exfoliation. The sensing response and limit of detection for the exfoliated graphene-based film were calculated as 3.56% and 432 ppb, respectively. Further studies indicated that the fabricated sensors are more selective towards ammonia molecules with quick response and recovery times.

The synthesis of graphene and graphene quantum dots (GQDs) employing various approaches with a range of precursors, chemicals, and parameters has been reported. Most of the top-down and bottom-up techniques employ strong and hazardous chemical environments, complicated and tedious procedures, are time-consuming, and often require special equipment. Another drawback of the techniques reported is the production of agglomerated, inhomogeneous, and non-dispersible graphene in aqueous solvents or organic solvents, thus limiting its application. This work specifically and comprehensively describes the electrochemical exfoliation of graphene and GQDs, which is often considered as a simple one-step, facile, non-hazardous, and highly efficient technique yet favourable for mass production. A brief discussion on the advantageous and challenges of the electrochemical technique and applications of the electrochemically exfoliated graphene and GQDs is also presented.