Recent Advances in the Construction of Energy Storage Functional Materials Utilizing Electrochemical Exfoliation and Dispersion Technology

Abstract

Electrochemical exfoliation (ECE) and dispersion technologies, as typical top-down electrochemical methods, exhibit outstanding advantages of being green, efficient, controllable, and scalable in the preparation of functional nanomaterials. ECE leverages an “intercalation–exfoliation” mechanism for the efficient and controllable production of few-/single-layer two-dimensional (2D) materials for energy storage. Electrochemical dispersion (ECD) is an efficient one-step method to prepare metal-based electrode nanomaterials, utilizing synergistic anodic oxidation and electric double-layer effects to transform bulk raw materials into functionalized nanomaterials with better dispersibility. This review systematically analyzes the electrochemical formation mechanisms of these two ways for synthesizing electrode materials under both direct current (DC) and alternating current (AC) power supplies. It centers on the mechanistic principles of two key approaches: the use of ECE to control the structure and properties of 2D layered electrodes, and the application of ECD to synthesize and optimize functionalized metal-based materials for energy storage devices. As promising electrochemical strategies for nanomaterial synthesis, ECE and ECD offer considerable promise for constructing and tailoring the properties of advanced energy storage electrodes.

Keywords

electrochemical technology / energy storage materials / formation mechanism / structural transformation

References

[1] S. M. Oja, M. Wood, and B. Zhang., “Nanoscale Electrochemistry,” Analytical Chemistry 85 (2012): 473–486.

[2] W. Chen, Y. Wu, Y. Jiang, et al., “Catalyst Selection Over an Electrochemical Reductive Coupling Reaction Toward Direct Electrosynthesis of Oxime From NO_(x) and Aldehyde,” Journal of the American Chemical Society 146 (2024): 6294–6306.

[3] Y. Fang, X. Li, J. Li, et al., “Janus Electrochemical Exfoliation of Two-Dimensional Materials,” Journal of Materials Chemistry A 7 (2019): 25691–25711.

[4] K. S. Novoselov, A. K. Geim, S. V. Morozov, et al., “Two-Dimensional Gas of Massless Dirac Fermions in Graphene,” Nature 438 (2005): 197–200.

[5] A. S. Mayorov, R. V. Gorbachev, S. V. Morozov, et al., “Micrometer-Scale Ballistic Transport in Encapsulated Graphene at Room Temperature,” Nano Letters 11 (2011): 2396–2399.

[6] M. F. El-Kady, Y. Shao, and R. B. Kaner, “Graphene for Batteries, Supercapacitors and Beyond,” Nature Reviews Materials 1 (2016): 16033.

[7] K. S. Novoselov, V. I. Fal'ko, L. Colombo, P. R. Gellert, M. G. Schwab, and K. Kim, “A Roadmap for Graphene,” Nature 490 (2012): 192–200.

[8] S. Yang, A. G. Ricciardulli, S. Liu, et al., “Ultrafast Delamination of Graphite into High-Quality Graphene Using Alternating Currents,” Angewandte Chemie, International Edition 56 (2017): 6669–6675.

[9] Y. Zhang, Y. Xu, Y. Niu, W. Hou, and R. Liu, “Highly Efficient Dual-Electrode Exfoliation of Graphite Into High-Quality Graphene via Square-Wave Alternating Currents,” Chemical Engineering Journal 456 (2023): 140977.

[10] Y. Zhang, W. Hou, R. Chang, X. Yao, and Y. Xu, “Ultrafast Alternating-Current Exfoliation Toward Large-Scale Synthesis of Graphene and Its Application for Flexible Supercapacitors,” Journal of Colloid and Interface Science 654 (2024): 246–257.

[11] X. Yin, C. S. Tang, Y. Zheng, et al., “Recent Developments in 2D Transition Metal Dichalcogenides: Phase Transition and Applications of the (Quasi-)Metallic Phases,” Chemical Society Reviews 50 (2021): 10087–10115.

[12] X. Duan and H. Zhang, “Introduction: Two-Dimensional Layered Transition Metal Dichalcogenides,” Chemical Reviews 124 (2024): 10619–10622.

[13] L. Li, D. Zhang, J. Deng, Y. Gou, and J. Fang, “Electrochemical Exfoliation of Two-Dimensional Layered Black Phosphorus and Applications,” Journal of Energy Chemistry 49 (2020): 365–374.

[14] A. Ambrosi, Z. Sofer, and M. Pumera, “Electrochemical Exfoliation of Layered Black Phosphorus into Phosphorene,” Angewandte Chemie, International Edition 56 (2017): 10443–10445.

[15] N. Kumar, R. Aepuru, S.-Y. Lee, and S.-J. Park, “Recent Advances in Phosphorene: A Promising Material for Supercapacitor Applications,” Materials Science and Engineering: R: Reports 163 (2025): 100932.

[16] C. Shu, P. D. J. Zhou, P. D. Z. Jia, et al., “Electrochemical Exfoliation of Two-Dimensional Phosphorene Sheets and Its Energy Application,” Chemistry—A European Journal 28 (2022): e202200857.

[17] F. Solaimany, A. Dashan, H. Pezeshk-Fallah, G. Khoorgami, and B. Ramezanzadeh, “2D MXene Nanosheets Latest Advances in Electrochemical Applications Including Energy Storage and Supercapacitors,” Journal of Energy Storage 111 (2025): 115341.

[18] J. Pang, R. G. Mendes, A. Bachmatiuk, et al., “Applications of 2D MXenes in Energy Conversion and Storage Systems,” Chemical Society Reviews 48 (2019): 72–133.

[19] S. Kumar, “Fluorine-Free MXenes: Recent Advances, Synthesis Strategies, and Mechanisms,” Small 20 (2023): 2308225.

[20] Y. Wei, P. Zhang, R. A. Soomro, Q. Zhu, and B. Xu, “Advances in the Synthesis of 2D MXenes,” Advanced Materials 33 (2021): 2103148.

[21] Q. Weng, X. Wang, X. Wang, Y. Bando, and D. Golberg, “Functionalized Hexagonal Boron Nitride Nanomaterials: Emerging Properties and Applications,” Chemical Society Reviews 45 (2016): 3989–4012.

[22] X. Lu, H. Xue, H. Gong, et al., “2D Layered Double Hydroxide Nanosheets and Their Derivatives Toward Efficient Oxygen Evolution Reaction,” Nano-Micro Letters 12 (2020): 86.

[23] J. Yu, Q. Wang, D. O'Hare, and L. Sun, “Preparation of Two Dimensional Layered Double Hydroxide Nanosheets and Their Applications,” Chemical Society Reviews 46 (2017): 5950–5974.

[24] Y. Li, X. Yu, Y. Fan, et al., “Electrochemical Exfoliation of the Two-Dimensional Conjugated Metal-Organic Framework for High-Performance Urea Electrooxidation,” ACS Nano 19 (2025): 18781–18790.

[25] J. Wang, N. Li, Y. Xu, and H. Pang, “Two-Dimensional MOF and COF Nanosheets: Synthesis and Applications in Electrochemistry,” Chemistry—A European Journal 26 (2020): 6402–6422.

[26] P. L. Taberna, S. Mitra, P. Poizot, P. Simon, and J. M. Tarascon, “High Rate Capabilities Fe₃O₄-Based Cu Nano-Architectured Electrodes for Lithium-Ion Battery Applications,” Nature Materials 5 (2006): 567–573.

[27] N. Yabuuchi, K. Kubota, M. Dahbi, and S. Komaba, “Research Development on Sodium-Ion Batteries,” Chemical Reviews 114 (2014): 11636–11682.

[28] M. Jing, Y. Yang, Y. Zhu, et al., “Alternating Voltage Induced Porous Co₃O₄ Sheets: An Exploration of Its Supercapacity Properties,” RSC Advances 5 (2015): 177–183.

[29] M. Jing, Z. Ding, H. Hou, et al., “Alternating Voltage Induced Electrochemical Synthesis of Three-Dimensionalization Copper Oxide for Lithium-Ion Battery Application,” Chemical Physics Letters 653 (2016): 30–34.

[30] A. B. Kuriganova, C. A. Vlaic, S. Ivanov, D. V. Leontyeva, A. Bund, and N. V. Smirnova, “Electrochemical Dispersion Method for the Synthesis of SnO₂ as Anode Material for Lithium Ion Batteries,” Journal of Applied Electrochemistry 46 (2016): 527–538.

[31] P. Tao, S. Yao, F. Liu, B. Wang, F. Huang, and M. Wang, “Recent Advances in Exfoliation Techniques of Layered and Non-Layered Materials for Energy Conversion and Storage,” Journal of Materials Chemistry A 7 (2019): 23512–23536.

[32] J. E. Cloud, K. McCann, K. A. P. Perera, and Y. Yang, “A Simple Method for Producing Colloidal Palladium Nanocrystals: Alternating Voltage-Induced Electrochemical Synthesis,” Small 9 (2013): 2532–2536.

[33] J. Liu, W. Huang, S. Chen, S. Hu, F. Liu, and Li Zelin Li, “Facile Electrochemical Dispersion of Bulk Rh into Hydrosols,” International Journal of Electrochemical Science 4 (2009): 1302–1308.

[34] G. Zhang, M. Jing, L. He, et al., “One-Pot Alternating Current Synthesis of SnO₂ Based Composite With Enhanced Diffusion Kinetic Behaviors for Lithium-Ion Batteries,” Journal of Central South University 31 (2025): 4424–4436.

[35] M. Jing, Y. Yang, Y. Zhu, H. Hou, Z. Wu, and X. Ji, “An Asymmetric Ultracapacitors Utilizing α-Co(OH)₂/Co₃O₄ Flakes Assisted by Electrochemically Alternating Voltage,” Electrochimica Acta 141 (2014): 234–240.

[36] M. Jing, J. Wang, H. Hou, et al., “Carbon Quantum Dot Coated Mn₃O₄ With Enhanced Performances for Lithium-ion Batteries,” Journal of Materials Chemistry A 3 (2015): 16824–16830.

[37] M. Jing, H. Hou, Y. Yang, et al., “Electrochemically Alternating Voltage Induced Mn₃O₄/Graphite Powder Composite With Enhanced Electrochemical Performances for Lithium-Ion Batteries,” Electrochimica Acta 155 (2015): 157–163.

[38] C. V. Le, M. Ju, T. T. T. Nguyen, H. Lee, and H. Yoon, “Hetero-Layered 2D Materials: Scalable Preparation and Energy Applications,” Materials Science and Engineering: R: Reports 163 (2025): 100937.

[39] O. A. Petrii, “Electrosynthesis of Nanostructures and Nanomaterials,” Russian Chemical Reviews 84 (2015): 159–193.

[40] A. Vartanian, “Speeding Up Simulations in Solids,” Nature Reviews Materials 6 (2021): 654.

[41] J. E. Cloud, T. S. Yoder, N. K. Harvey, K. Snow, and Y. Yang, “A Simple and Generic Approach for Synthesizing Colloidal Metal and Metal Oxide Nanocrystals,” Nanoscale 5 (2013): 7368.

[42] P. Yu, S. E. Lowe, G. P. Simon, and Y. L. Zhong, “Electrochemical Exfoliation of Graphite and Production of Functional Graphene,” Current Opinion in Colloid & Interface Science 20 (2015): 329–338.

[43] X. Lu, M. Cai, X. Wu, et al., “Controllable Synthesis of 2D Materials by Electrochemical Exfoliation for Energy Storage and Conversion Application,” Small 19 (2023): 2206702.

[44] H. Lee, J. I. Choi, J. Park, S. S. Jang, and S. W. Lee, “Role of Anions on Electrochemical Exfoliation of Graphite Into Graphene in Aqueous Acids,” Carbon 167 (2020): 816–825.

[45] I. Khakpour, A. Rabiei Baboukani, A. Allagui, and C. Wang, “Bipolar Exfoliation and In Situ Deposition of High-Quality Graphene for Supercapacitor Application,” ACS Applied Energy Materials 2 (2019): 4813–4820.

[46] A. M. Abdelkader, I. A. Kinloch, and R. A. Dryfe, “Continuous Electrochemical Exfoliation of Micrometer-Sized Graphene Using Synergistic Ion Intercalations and Organic Solvents,” ACS Applied Materials & Interfaces 6 (2014): 1632–1639.

[47] D. Chernysheva, C. Vlaic, I. Leontyev, et al., “Synthesis of Co₃O₄/CoOOH via Electrochemical Dispersion Using a Pulse Alternating Current Method for Lithium-Ion Batteries and Supercapacitors,” Solid State Sciences 86 (2018): 53–59.

[48] H. Aghamohammadi, R. Eslami-Farsani, M. Torabian, and N. Amousa, “Recent Advances in One-Pot Functionalization of Graphene Using Electrochemical Exfoliation of Graphite: A Review Study,” Synthetic Metals 269 (2020): 116549.

[49] Y. Yang, H. Hou, G. Zou, et al., “Electrochemical Exfoliation of Graphene-Like Two-Dimensional Nanomaterials,” Nanoscale 11 (2019): 16–33.

[50] F. Liu, C. Wang, X. Sui, et al., “Synthesis of Graphene Materials by Electrochemical Exfoliation: Recent Progress and Future Potential,” Carbon Energy 1 (2019): 173–199.

[51] W. Li, C. Yu, X. Tan, Z. Wang, and J. Qiu, ““Electric-Field-Triggered Graphene Production: From Fundamental Energy Applications to Perspectives,” Accounts of Materials Research 3 (2022): 175–186.

[52] I. Ali, P. V. Oskin, T. P. Dyachkova, et al., “Advances in One-Step Functionalization of Graphene Oxide During Electrochemical Graphite Exfoliation,” Journal of Materials Science 60 (2025): 13156–13190.

[53] J. M. Munuera, J. I. Paredes, S. Villar-Rodil, et al., “High Quality, Low Oxygen Content and Biocompatible Graphene Nanosheets Obtained by Anodic Exfoliation of Different Graphite Types,” Carbon 94 (2015): 729–739.

[54] J. Liu, C. K. Poh, D. Zhan, et al., “Improved Synthesis of Graphene Flakes From the Multiple Electrochemical Exfoliation of Graphite Rod,” Nano Energy 2 (2013): 377–386.

[55] A. M. Abdelkader, A. J. Cooper, R. A. W. Dryfe, and I. A. Kinloch, “How to Get Between the Sheets: A Review of Recent Works on the Electrochemical Exfoliation of Graphene Materials From Bulk Graphite,” Nanoscale 7 (2015): 6944–6956.

[56] M. Coroş, F. Pogăcean, M.-C. Roşu, et al., “Simple and Cost-Effective Synthesis of Graphene by Electrochemical Exfoliation of Graphite Rods,” RSC Advances 6 (2016): 2651–2661.

[57] J. Mei, Z. Qiu, T. Gao, et al., “Insights into the Conductive Network of Electrochemical Exfoliation With Graphite Powder as Starting Raw Material for Graphene Production,” Langmuir 39 (2023): 4413–4426.

[58] K. Chen, D. Xue, and S. Komarneni, “Nanoclay Assisted Electrochemical Exfoliation of Pencil Core to High Conductive Graphene Thin-Film Electrode,” Journal of Colloid and Interface Science 487 (2017): 156–161.

[59] G. Wei, W. Su, Z. Wei, X. Fan, J. Liu, and C. Yan, “Electrocatalytic Effect of the Edge Planes Sites at Graphite Electrode on the Vanadium Redox Couples,” Electrochimica Acta 204 (2016): 263–269.

[60] S. Lim, N. Lingappan, and W. Lee, “Biased Dual-Exfoliation Technique With Expanded Graphite for High-Quality Few-Layer Graphene Sheets in Electrochemical Exfoliation,” Carbon Letters 35 (2025): 1205–1220.

[61] J. Chen, M. Perez-Page, Z. Ji, Z. Zhang, Z. Guo, and S. Holmes, “One Step Electrochemical Exfoliation of Natural Graphite Flakes Into Graphene Oxide for Polybenzimidazole Composite Membranes Giving Enhanced Performance in High Temperature Fuel Cells,” Journal of Power Sources 491 (2021): 229550.

[62] D. He, A. J. Marsden, Z. Li, R. Zhao, W. Xue, and M. A. Bissett, “A Single Step Strategy to Fabricate Graphene Fibres via Electrochemical Exfoliation for Micro-Supercapacitor Applications,” Electrochimica Acta 299 (2019): 645–653.

[63] S. Yang, S. Brüller, Z.-S. Wu, et al., “Organic Radical-Assisted Electrochemical Exfoliation for the Scalable Production of High-Quality Graphene,” Journal of the American Chemical Society 137 (2015): 13927–13932.

[64] Z. Liu, H. Zhang, M. Eredia, et al., “Water-Dispersed High-Quality Graphene: A Green Solution for Efficient Energy Storage Applications,” ACS Nano 13 (2019): 9431–9441.

[65] H. Lee, K. Lee, M. S. Kim, et al., “Few-Layered Graphene From Cathodic Exfoliation in Binary Solvents and Application as a Protective Layer for Lithium Metal Anodes,” Carbon 230 (2024): 119647.

[66] Y. Zhang, Y. Xu, and R. Liu, “Regulating Cations and Solvents of the Electrolyte for Ultra-Efficient Electrochemical Production of High-Quality Graphene,” Carbon 176 (2021): 157–167.

[67] J. Wu, H. Wang, J. Qiu, K. Zhang, J. Shao, and L. Yan, “Efficient Preparation of High-Quality Graphene via Anodic and Cathodic Simultaneous Electrochemical Exfoliation Under the Assistance of Microwave,” Journal of Colloid and Interface Science 608 (2022): 1422–1431.

[68] Y. Zhang, Y. Xu, R. Liu, and Y. Niu, “Synthesis of High-Quality Graphene by Electrochemical Anodic and Cathodic Co-Exfoliation Method,” Chemical Engineering Journal 461 (2023): 141985.

[69] D. Chen, F. Wang, Y. Li, et al., “Programmed Electrochemical Exfoliation of Graphite to High Quality Graphene,” Chemical Communications 55 (2019): 3379–3382.

[70] Z. Qiu, Z. Liu, J. Miao, et al., “Scalable Production of Electrochemically Exfoliated Graphene by an Extensible Electrochemical Reactor With Encapsulated Anode and Dual Cathodes,” Applied Surface Science 608 (2023): 155211.

[71] J. Mei, Z. Qiu, T. Gao, et al., “Process Regulation of the Electrochemical Exfoliation for Graphene Production With Graphite Powder as Starting Materials,” Journal of Materials Science 58 (2023): 9116–9129.

[72] H. Hashimoto, Y. Muramatsu, Y. Nishina, and H. Asoh, “Bipolar Anodic Electrochemical Exfoliation of Graphite Powders,” Electrochemistry Communications 104 (2019): 106475.

[73] S. La Yoon, H. S. Park, and Y.-P. Jeon, “Synthesis of Highly Crystalline Electrochemically Exfoliated Graphene as a Conductive Additive for Lithium-Ion Batteries,” Carbon Letters 35 (2025): 1113–1124.

[74] M. H. Dalal, C. Y. Lee, and G. G. Wallace, “Simultaneous Anodic and Cathodic Exfoliation of Graphite Electrodes in an Aqueous Solution of Inorganic Salt,” ChemElectroChem 8 (2021): 3168–3173.

[75] Y. Zhang and Y. Xu, “Simultaneous Electrochemical Dual-Electrode Exfoliation of Graphite Toward Scalable Production of High-Quality Graphene,” Advanced Functional Materials 29 (2019): 1902171.

[76] H. Huang, F. Zhou, P. Lu, et al., “Design and Construction of Few-Layer Graphene Cathode for Ultrafast and High-Capacity Aluminum-Ion Batteries,” Energy Storage Materials 27 (2020): 396–404.

[77] L. Liao, H. Ma, H. Liu, Y. Qian, and X. Zhou, “Efficient Fabrication of High-Quality Graphene via Alternating-Current Co-Intercalation and Microwave-Assisted Expansion,” Ceramics International 50 (2024): 34999–35006.

[78] E. T. Bjerglund, M. E. P. Kristensen, S. Stambula, G. A. Botton, S. U. Pedersen, and K. Daasbjerg, “Efficient Graphene Production by Combined Bipolar Electrochemical Intercalation and High-Shear Exfoliation,” ACS Omega 2 (2017): 6492–6499.

[79] L. Bawden, S. P. Cooil, F. Mazzola, et al., “Spin-Valley Locking in the Normal State of a Transition-Metal Dichalcogenide Superconductor,” Nature Communications 7 (2016): 11711.

[80] Z. Fan, Z. Geng, W. Fang, et al., “Characteristics of Transition Metal Dichalcogenides in Optical Pumped Modulator of Terahertz Wave,” AIP Advances 10 (2020): 045304.

[81] X. Li and H. Zhu, “Two-Dimensional MoS₂: Properties, Preparation, and Applications,” Journal of Materiomics 1 (2015): 33–44.

[82] D. Voiry, A. Mohite, and M. Chhowalla, “Phase Engineering of Transition Metal Dichalcogenides,” Chemical Society Reviews 44 (2015): 2702–2712.

[83] R. Yang, Y. Fan, Y. Zhang, et al., “2D Transition Metal Dichalcogenides for Photocatalysis,” Angewandte Chemie, International Edition 62 (2023): 2218016.

[84] M. A. Py and R. R. Haering, “Structural Destabilization Induced by Lithium Intercalation in MoS2 and Related Compounds,” Canadian Journal of Physics 61 (1983): 76–84.

[85] D. F. Carrasco, S. García-Dalí, S. Villar-Rodil, J. M. Munuera, E. Raymundo-Piñero, and J. I. Paredes, “NbSe2 Nanosheets/Nanorolls Obtained via Fast and Direct Aqueous Electrochemical Exfoliation for High-Capacity Lithium Storage,” ACS Applied Energy Materials 6 (2023): 7180–7193.

[86] Y. Li, K. Chang, Z. Sun, et al., “Selective Preparation of 1T- and 2H-Phase MoS₂ Nanosheets With Abundant Monolayer Structure and Their Applications in Energy Storage Devices,” ACS Applied Energy Materials 3 (2020): 998–1009.

[87] H. H. Huang, X. Fan, D. J. Singh, and W. T. Zheng, “Recent Progress of TMD Nanomaterials: Phase Transitions and Applications,” Nanoscale 12 (2020): 1247–1268.

[88] W. Wu, C. Zhang, L. Zhou, S. Hou, and L. Zhang, “High Throughput Synthesis of Defect-Rich MoS₂ Nanosheets via Facile Electrochemical Exfoliation for Fast High-Performance Lithium Storage,” Journal of Colloid and Interface Science 542 (2019): 263–268.

[89] N. Liu, P. Kim, J. H. Kim, J. H. Ye, S. Kim, and C. J. Lee, “Large-Area Atomically Thin MoS₂ Nanosheets Prepared Using Electrochemical Exfoliation,” ACS Nano 8 (2014): 6902–6910.

[90] A. Martínez-Jódar, S. Villar-Rodil, J. M. Munuera, et al., “Two-Dimensional MoS₂ Nanosheets Derived From Cathodic Exfoliation for Lithium Storage Applications,” Nanomaterials 14 (2024): 932.

[91] R. Hu, Z. Huang, B. Wang, H. Qiao, and X. Qi, “Electrochemical Exfoliation of Molybdenum Disulfide Nanosheets for High-Performance Supercapacitors,” Journal of Materials Science: Materials in Electronics 32 (2021): 7237–7248.

[92] S. García-Dalí, J. I. Paredes, J. M. Munuera, et al., “Aqueous Cathodic Exfoliation Strategy Toward Solution-Processable and Phase-Preserved MoS₂ Nanosheets for Energy Storage and Catalytic Applications,” ACS Applied Materials & Interfaces 11 (2019): 36991–37003.

[93] A. Ejigu, I. A. Kinloch, E. Prestat, and R. A. W. Dryfe, “A Simple Electrochemical Route to Metallic Phase Trilayer MoS₂: Evaluation as Electrocatalysts and Supercapacitors,” Journal of Materials Chemistry A 5 (2017): 11316–11330.

[94] R. Naz, W. Abbas, Q. Liu, et al., “Covalent Functionalization of Electrochemically Exfoliated 1T-MoS₂ Nanosheets for High-Performance Supercapacitor Electrode,” Journal of Alloys and Compounds 951 (2023): 169944.

[95] M. B. Dines, “Lithium Intercalation via n-Butyllithium of the Layered Transition Metal Dichalcogenides,” Materials Research Bulletin 10 (1975): 287–291.

[96] Z. Zeng, T. Sun, J. Zhu, et al., “An Effective Method for the Fabrication of Few-Layer-Thick Inorganic Nanosheets,” Angewandte Chemie, International Edition 51 (2012): 9052–9056.

[97] R. Yang, L. Mei, Q. Zhang, et al., “High-Yield Production of Mono- or Few-Layer Transition Metal Dichalcogenide Nanosheets by an Electrochemical Lithium Ion Intercalation-Based Exfoliation Method,” Nature Protocols 17 (2022): 358–377.

[98] G. Eda, H. Yamaguchi, D. Voiry, T. Fujita, M. Chen, and M. Chhowalla, “Photoluminescence From Chemically Exfoliated MoS₂,” Nano Letters 11 (2011): 5111–5116.

[99] X. Li, “Customizing MXenes,” Matter 6 (2023): 2519–2522.

[100] Y. Gogotsi, “The Future of MXenes,” Chemistry of Materials 35 (2023): 8767–8770.

[101] L. Zheng, H. Li, E. Kovalska, et al., “Electrochemical Exfoliation of Layered Non-van der Waals Crystals into 2D Nanosheets: MAX Phases and Beyond,” Small 21 (2025): 2408801.

[102] P. P. Michałowski, M. Anayee, T. S. Mathis, et al., “Oxycarbide MXenes and MAX Phases Identification Using Monoatomic Layer-by-Layer Analysis With Ultralow-Energy Secondary-Ion Mass Spectrometry,” Nature Nanotechnology 17 (2022): 1192–1197.

[103] C. Zhou, X. Zhao, Y. Xiong, et al., “A Review of Etching Methods of MXene and Applications of MXene Conductive Hydrogels,” European Polymer Journal 167 (2022): 111063.

[104] A. Shayesteh Zeraati, S. A. Mirkhani, P. Sun, M. Naguib, P. V. Braun, and U. Sundararaj, “Improved Synthesis of Ti₃C₂T_x MXenes Resulting in Exceptional Electrical Conductivity, High Synthesis Yield, and Enhanced Capacitance,” Nanoscale 13 (2021): 3572–3580.

[105] B. Anasori and M. Naguib, “Two-Dimensional Mxenes,” MRS Bulletin 48 (2023): 238–244.

[106] W. Bi, S. Li, W. Wang, et al., “MXenes and Their Composites as Electrodes for Sodium Ion Batteries,” Energy Storage Materials 71 (2024): 103568.

[107] J. Zhou, S. Lin, Y. Huang, et al., “Synthesis and Lithium Ion Storage Performance of Two-Dimensional V₄C₃ MXene,” Chemical Engineering Journal 373 (2019): 203–212.

[108] M. Naguib, J. Halim, J. Lu, et al., “New Two-Dimensional Niobium and Vanadium Carbides as Promising Materials for Li-Ion Batteries,” Journal of the American Chemical Society 135 (2013): 15966–15969.

[109] M. Naguib, M. Kurtoglu, V. Presser, et al., “Two-Dimensional Nanocrystals Produced by Exfoliation of Ti₃AlC₂,” Advanced Materials 23 (2011): 4248–4253.

[110] K. C. Chan, X. Guan, T. Zhang, et al., “The Fabrication of Ti₃C₂ and Ti₃CN MXenes by Electrochemical Etching,” Journal of Materials Chemistry A 12 (2024): 25165–25175.

[111] J. Chen, M. Chen, W. Zhou, et al., “Simplified Synthesis of Fluoride-Free Ti₃C₂T_x via Electrochemical Etching Toward High-Performance Electrochemical Capacitors,” ACS Nano 16 (2022): 2461–2470.

[112] L. Liu, H. Zschiesche, M. Antonietti, et al., “In Situ Synthesis of MXene With Tunable Morphology by Electrochemical Etching of MAX Phase Prepared in Molten Salt,” Advanced Energy Materials 13 (2022): 202203805.

[113] M. Ostermann, M. Piljević, E. Akbari, et al., “Pulsed Electrochemical Exfoliation for an HF-Free Sustainable MXene Synthesis,” Small 21 (2025): 2500807.

[114] X. Li, M. Li, Q. Yang, et al., “In Situ Electrochemical Synthesis of MXenes Without Acid/Alkali Usage in/for an Aqueous Zinc Ion Battery,” Advanced Energy Materials 10 (2020): 2001791.

[115] T. Yin, Y. Li, R. Wang, et al., “Synthesis of Ti₃C₂F_x MXene With Controllable Fluorination by Electrochemical Etching for Lithium-Ion Batteries Applications,” Ceramics International 47 (2021): 28642–28649.

[116] M. Shen, W. Jiang, K. Liang, et al., “One-Pot Green Process to Synthesize MXene With Controllable Surface Terminations Using Molten Salts,” Angewandte Chemie, International Edition 60 (2021): 27013–27018.

[117] S. Yang, P. Zhang, F. Wang, et al., “Fluoride-Free Synthesis of Two-Dimensional Titanium Carbide (MXene) Using A Binary Aqueous System,” Angewandte Chemie, International Edition 57 (2018): 15491–15495.

[118] S.-Y. Pang, Y.-T. Wong, S. Yuan, et al., “Universal Strategy for HF-Free Facile and Rapid Synthesis of Two-Dimensional MXenes as Multifunctional Energy Materials,” Journal of the American Chemical Society 141 (2019): 9610–9616.

[119] J. E. Cloud, L. W. Taylor, and Y. Yang, “A Simple and Effective Method for Controllable Synthesis of Silver and Silver Oxide Nanocrystals,” RSC Advances 4, no. 47 (2014): 24551–24559.

[120] M. Jing, H. Hou, Y. Yang, Y. Zhu, Z. Wu, and X. Ji, “Electrochemically Alternating Voltage Tuned CO₂MnO₄/Co Hydroxide Chloride for an Asymmetric Supercapacitor,” Electrochimica Acta 165 (2015): 198–205.

[121] M. Jing, F. Li, M. Chen, F. Long, and T. Wu, “Binding ZnO Nanorods in Reduced Graphene Oxide via Facile Electrochemical Method for Na-Ion Battery,” Applied Surface Science 463 (2019): 986–993.

[122] M. Jing, C. Wang, H. Hou, et al., “Ultrafine Nickel Oxide Quantum Dots Enbedded With Few-Layer Exfoliative Graphene for an Asymmetric Supercapacitor: Enhanced Capacitances by Alternating Voltage,” Journal of Power Sources 298 (2015): 241–248.

[123] L. He, M. Jing, D. Li, et al., “Electrochemically Alternating Voltage Induction and In-Situ Preparation of Tin-Based Multiphase Structures Anode for Sodium-Ion Batteries,” Journal of Alloys and Compounds 976 (2024): 172968.

[124] A. B. Kuriganova, D. V. Leontyeva, and N. V. Smirnova, “On the Mechanism of Electrochemical Dispersion of Platinum Under the Action of Alternating Current,” Russian Chemical Bulletin 64 (2015): 2769–2775.

[125] W. Huang, S. Chen, J. Zheng, and Z. Li, “Facile Preparation of Pt Hydrosols by Dispersing Bulk Pt With Potential Perturbations,” Electrochemistry Communications 11 (2009): 469–472.

[126] M. Jing, H. Hou, C. E. Banks, Y. Yang, Y. Zhang, and X. Ji, “Alternating Voltage Introduced NiCo Double Hydroxide Layered Nanoflakes for an Asymmetric Supercapacitor,” ACS Applied Materials & Interfaces 7, no. 41 (2015): 22741–22744.

[127] D. V. Leontyeva, I. N. Leontyev, M. V. Avramenko, Y. I. Yuzyuk, Y. A. Kukushkina, and N. V. Smirnova, “Electrochemical Dispergation as a Simple and Effective Technique Toward Preparation of NiO Based Nanocomposite for Supercapacitor Application,” Electrochimica Acta 114 (2013): 356–362.

[128] D. V. Chernysheva, I. N. Leontyev, M. V. Avramenko, N. V. Lyanguzov, T. I. Grebenyuk, and N. V. Smirnova, “One Step Simultaneous Electrochemical Synthesis of NiO/Multilayer Graphene Nanocomposite as an Electrode Material for High Performance Supercapacitors,” Mendeleev Communications 31 (2021): 160–162.

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