Detailed analysis of the synthesis and structure of MAX phase (Mo0.75V0.25)5AlC4 and its MXene (Mo0.75V0.25)5C4

Published

June 27, 2023

Author(s)

Rose Snyder, Mikkel Juelsholt, Curran Kalha, Jason Holm, Elisabeth Mansfield, Tien-Lin Lee, Pardeep Thakur, Aysha Riaz, Benjamin Moss, Anna Regoutz, Christina Birkel

Abstract

MAX phases with the general formula Mn+1AXn are layered carbides, nitrides and carbonitrides with varying stacking sequence of layers of M6X octahedra and the A-element depending on n. While "211" MAX phases (n = 1) are very common, MAX phases with higher n, especially n ≥ 3, have hardly been prepared. This work addresses open questions regarding the synthesis conditions and structure and chemical composition of the relatively new "514" MAX phase. In contrast to literature reports, no oxide is needed to form the MAX phase, yet multiple heating steps at 1,600 °C are required. Using high-resolution X-ray diffraction, the structure of (Mo1-xVx)5AlC4 is thoroughly investigated and Rietveld refinement confirms P-6c2 as the most fitting space group. SEM/EDS and XPS show that the chemical composition of the MAX phase is (Mo0.75V0.25)5AlC4. It was also exfoliated into its MXene sibling (Mo0.75V0.25)5C4 using two different techniques (using only HF and an HF/HCl mixture), which leads to different surface determinations as shown by XPS/HAXPES measurements. Initial investigations of the electrocatalytic properties of both MXene versions show that depending on the etchant, (Mo0.75V0.25)5C4 can reduce hydrogen at 10 mA cm-2 with an overpotential of 166 mV (HF only) or 425 mV (HF/HCl) after the cycling the samples, which make them a potential candidate as an HER catalyst.

Citation

ACS Nano

Volume

17

Issue

13

Pub Type

Journals

Download Paper

https://doi.org/10.1021/acsnano.3c03395

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Keywords

2D materials, advanced materials, synthesis, structure

Citation

Snyder, R. , Juelsholt, M. , Kalha, C. , Holm, J. , Mansfield, E. , Lee, T. , Thakur, P. , Riaz, A. , Moss, B. , Regoutz, A. and Birkel, C. (2023), Detailed analysis of the synthesis and structure of MAX phase (Mo0.75V0.25)5AlC4 and its MXene (Mo0.75V0.25)5C4, ACS Nano, [online], https://doi.org/10.1021/acsnano.3c03395, https://tsapps.nist.gov/publication/get_pdf.cfm?pub_id=936227 (Accessed September 8, 2024)