Pratyush
Chettri

Optimization of Nb4C3Tx MXene Synthesis for Improved Yield and Flake Quality STEM

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Pratyush Chettri

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MXenes are a promising family of two-dimensional transition metal carbides and nitrides with high electrical conductivity and composition- dependent properties, making them applicable in energy storage, catalysis, and electromagnetic shielding. They are typically produced by selectively etching aluminum from MAX phases using acidic solutions. The resulting layered MXene structure is intercalated with guest molecules to expand the interlayer spacing and promote delamination of layers into a colloidal solution of single-to-few layer MXene flakes. Though great progress has been made in MXene synthesis since their discovery in 2011, thicker-layered MXenes such as M4C3Tx remain relatively underexplored due to greater structural rigidity which poses challenges for etching and delamination. Our study focuses on the synthesis of Nb4C3Tx MXene from Nb4AlC3 MAX precursor and aims to optimize the process for yield and quality of resulting delaminated flakes. We systematically varied parameters for each step of the synthesis process and measured relevant outcomes. We first varied the HCl concentration and duration for MAX phase pre-treatment and identified conditions that fully removed any impurities present. We then explored etching conditions - reaction time, temperature, and HF-HCl concentration - and determined combinations that resulted in complete conversion of MAX to layered MXene by measuring interlayer spacing changes and Al removal. Finally, we tested multiple intercalation and delamination methods using various bases and salts. The resulting MXene flakes were characterized to assess quality and synthesis yield. Through this process we identified an optimized synthesis path for higher flake quality and yield of Nb4C3Tx MXene. Keywords: Optimization; MXene; New

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Purdue University / 2025

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Pratyush Chettri

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