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<p>Industrial scaleup of MXene synthesis has faced many challenges, both in the process safety and nanosheet yield. As a step toward the scalability of MXenes, we carried out a one-to-one comparison of the industrial scalability and application performance of two methods for producing Ti<sub>3</sub>C<sub>2</sub>T<sub><i>z</i></sub> MXenes: LiF-HCl acid etching and Lewis acid molten salt etching. This study had an emphasis on nanoscale structure, electrical conductivity, electromagnetic interference (EMI) shielding and supercapacitive properties, yield, and process scalability, both at the etched clay stage and delaminated nanosheet stage. This comparison was completed in parallel with the same starting MAX phase, chemicals, and processing equipment, where necessary. The synthesis process influences the structure and terminal groups of MXenes, altering properties and performance. Notably, the electrical conductivity was superior for acid-etched nanosheets at 2200 S/cm, compared to salt-etched nanosheets at 0.66 S/cm. For EMI shielding effectiveness and capacitance, acid-etched nanosheets performed the highest. The yield of the acid-etched nanosheets was ~ 50% and salt-etched nanosheets was 15%. The acid-etched process was scaled up with a small business partner from 1-g to 200-g MAX phase, with similar properties and yield. When the salt-etching process was scaled up to 25&#xa0;g of MAX, the properties remained similar to the 1&#xa0;g batch, with a lower yield of ~ 5%. Although the acid-etching process was better for most metrics, the molten salt-etching method is still in its infancy and has advantages regarding process safety.</p>

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Ti3C2Tz MXene MILD acid etching versus CuCl2 molten salt etching: properties, scaleup, and degradation analysis

  • 期刊论文

  • 发表日期：

    2025年6月1日

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  • Savannah E. Pas,
  • Kailash Arole,
  • Stefano A. Micci-Barreca,
  • Yufan Zhang,
  • Ramu Banavath,
  • Adam T. Ronderos,
  • Milos Dujovic,
  • Denis Johnson,
  • Abdoulaye Djire,
  • Miladin Radovic,
  • Jodie L. Lutkenhaus,
  • Micah J. Green

摘要

Industrial scaleup of MXene synthesis has faced many challenges, both in the process safety and nanosheet yield. As a step toward the scalability of MXenes, we carried out a one-to-one comparison of the industrial scalability and application performance of two methods for producing Ti3C2Tz MXenes: LiF-HCl acid etching and Lewis acid molten salt etching. This study had an emphasis on nanoscale structure, electrical conductivity, electromagnetic interference (EMI) shielding and supercapacitive properties, yield, and process scalability, both at the etched clay stage and delaminated nanosheet stage. This comparison was completed in parallel with the same starting MAX phase, chemicals, and processing equipment, where necessary. The synthesis process influences the structure and terminal groups of MXenes, altering properties and performance. Notably, the electrical conductivity was superior for acid-etched nanosheets at 2200 S/cm, compared to salt-etched nanosheets at 0.66 S/cm. For EMI shielding effectiveness and capacitance, acid-etched nanosheets performed the highest. The yield of the acid-etched nanosheets was ~ 50% and salt-etched nanosheets was 15%. The acid-etched process was scaled up with a small business partner from 1-g to 200-g MAX phase, with similar properties and yield. When the salt-etching process was scaled up to 25 g of MAX, the properties remained similar to the 1 g batch, with a lower yield of ~ 5%. Although the acid-etching process was better for most metrics, the molten salt-etching method is still in its infancy and has advantages regarding process safety.