First published: 30 March 2025 https://doi.org/10.1002/smll.202500807
Pulsed Electrochemical Exfoliation for an HF-FreeSustainable MXene Synthesis
Markus Ostermann1, Marko Piljevi´c1,2, Elahe Akbari 3, Prathamesh Patil 1, Veronika Zahorodna 4, Ivan Baginskiy 4, Oleksiy Gogotsi 4, Carsten Gachot 5, Manel Rodríguez Ripoll 2, Markus Valtiner 1,3 and Pierluigi Bilotto1,5
1 CEST GmbH, Centre for Electrochemical Surface Technology, A-2700 Wiener Neustadt, Austria
2 AC2T research GmbHA-2700 Wiener Neustadt, Austria
3 Applied Interface Physics, TU WienA-1040 Vienna, Austria
4 Carbon-Ukraine (Y-Carbon LLC) 04116 Kyiv, Ukraine
5 Institute of Engineering Design and Product Development, ResearchUnit Tribology (E307-05), TU WienA-1060 Vienna, Austria
MXenes are a 2D materials (2DM) class with high industrialization potential, owing to their superb properties and compositional variety. However, ensuring high etching efficiency in the synthesis process without involving toxic, hazardous or non-sustainable chemicals are challenging. In this work, an upscalable electrochemical MXene synthesis is presented. This novel protocol uses a non-toxic and sustainable sodium tetrafluoroborate/hydrochloric acid (NaBF4/HCl) electrolyte and increases etching efficiency by applying cathodic pulsing via pulse voltammetry. Hydrogen bubble formation restores electrochemical activity, and effectively supports 2D-sheet removal, allowing continuous etching at higher yields in situ. In detail, yields of up to 60% electrochemical MXene (EC-MXene) with no byproducts from a single exfoliation cycle are achieved.
EC-MXene had an excellent quality with high purity as assessed using chemical mapping by scanning electron microscopy with energy dispersive electron spectroscopy (SEM/EDX) and surface termination analysis performed with X-ray photoelectron spectroscopy (XPS) and, for the first time, with low energy ion scattering (LEIS). Further properties of EC-MXenes such as dimensions and adhesion energy of single flakes, vibrational peaks, and interlayer spacing are provided by atomic force microscopy (AFM), X-ray diffraction (XRD), Raman spectroscopy (Raman), and transmission electron microscopy (TEM) respectively. Pulsed electrochemical synthesis is key to surface reactivation at the electrodes' interface, which results in improved exfoliation and quality of EC-MXenes. This paves the way for scaling up and green industrialization of MXenes.
Cite and read more about this work:
M. Ostermann, M. Piljević, E. Akbari, P. Patil, V. Zahorodna, I. Baginskiy, O. Gogotsi, C. Gachot, M. Rodríguez Ripoll, M. Valtiner, P. Bilotto, Pulsed Electrochemical Exfoliation for an HF-Free Sustainable MXene Synthesis. Small 2025, 2500807. https://doi.org/10.1002/smll.202500807
Read more publications on related topics:
MRC and Drexel collaborative article on Scalable MXene synthesis is listed among the most accessed in Advanced Engineering Materials journal for the whole year
This article is also Highly Cited in Web of Science top 1% of all papers in the field. Researchers at Drexel University and the Materials Research Center in Ukraine have designed a system that can be used to make large quantities of the material while preserving its unique properties. The team recently reported in the journal Advanced Engineering Materials that a lab-scale reactor system developed at the Materials Research Center in Kyiv, can convert a ceramic precursor material into a pile of the powdery black MXene titanium carbide, in quantities as large as 50 grams per batch.
Thank you to our collaborators for the amazing joint work recently published in Graphene and 2D Nanomaterials about MXene–silk fibroin composite films aiming to develop materials with tunable electronic and thermal properties
Congratulations to all collaborators with this interesting joint work!
Dr. Oleksiy Gogotsi, director of MRC and Carbon-Ukraine, innovative companies that are among the leaders on the world MXene market, visited 2024 MRS Fall Meeting & Exhibit. together with Dr. Maksym Pogorielov, Head of Advanced Biomaterials and Biophysics Laboratory, University of Latvia.
MRC and Carbon-Ukraine team visited the 3rd International MXene conference held at Drexel University on August 5-8, 2024. Conference brought together the best reserchers and leading experts on MXene field. 
Together with colleagues from the University of Latvia, MRC/Carbone Ukraine, Adam Mickiewicz University, University Clinic Essen, and others, we have developed a novel concept involving the binding of antibodies to MXenes. In our research, we utilized anti-CEACAM1 antibodies to develop targeted photo-thermal therapy for melanoma (in vitro), paving the way for future in vivo studies and clinical trials. For the first time, we demonstrate the feasibility of delivering MXenes specifically targeted to melanoma cells, enabling the effective ablation of cancer cells under near-infrared (NIR) light. This new technique opens up vast potential for the application of MXenes in cancer treatment, diagnostics, drug delivery, and many other medical purposes.
Here we demonstrate a new developed method for depositing Ti3C2Tx MXenes onto hydrophobic electrospun PCL membranes using oxygen plasma treatment. These novel patches hold tremendous potential for providing mechanical support to damaged heart tissue and enabling electrical signal transmission,thereby mimicking the crucial electroconductivity required for normal cardiac function. After a detailed investigation of scaffold-to-cell interplay, including electrical stimulation, novel technology has the potential for clinical application not only for cardiac regeneration, but also as neural and muscular tissue substitutes.
MX-MAP project participants from MRC Dr. Oleksiy Gogotsi and Veronika Zahorodna performed split secondment visit to project partner organization University of Padova (Italy). MX-MAP project works on development of the key strategies for MXene medical applications. 
CanbioSe Project Meeting and Project Workshop was held at European Institute of Membranes (IEM), University of Montpellier, France on September 26-27, 2023. The workshop was focused on the theme of "Commercializing Biosensors, Intellectual Property, and Knowledge Transfer from Academia to Industry.
Dr. Oleksiy Gogotsi and Veronika Zahorodna visited IEEE NAP 2023 conference held in Bratislava on September 10-15, 2023. The prime focus of the IEEE NAP-2023 was on nanoscale materials with emphasis on interdisciplinary research exploring and exploiting their unique physical and chemical proprieties for practical applications.
Director of MRC and Carbon-Ukraine Dr. Oleksiy Gogotsi visited CEST labs in Wiener Neustadt (Low Energy Ion Scattering, Batteries development) and TU Vienna (ELSA, SFA). He meet with Dr. Pierluigi Bilotto, Dr. Chriatian Pichler and their colleagues, discussing novel materials and r&d activities for new technologies.