Effect Of The Composition Of The Etching System MF-HCl (M = Li+, Na+, NH4+) on the gas-sensitive properties of Ti3C2Tх/Tioх nanocomposites

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Resumo

The influence of the nature of MF-HCl etching systems (M = Li+, Na+, NH4+) on the process of synthesis of Ti3C2Tx MXenes on the basis of Ti3AlC2 MAX-phase, microstructure, phase purity, interlayer distance, composition of functional surface groups, thermal behavior and yield of the obtained products has been studied. The room temperature sensing properties of Ti3C2Tx receptor layers deposited by microplotter printing were studied with respect to a wide range of gas analytes (H2, CO, NH3, NO2, NO2, O2, benzene, acetone, methane and ethanol). Increased sensitivity to ammonia was revealed for the MXenes obtained by exposure to hydrochloric acid solutions of sodium and ammonium fluorides and to carbon monoxide for the sample synthesized using the LiF-HCl system. High responses (~20–30% to 100 ppm NO2) were observed for all three receptor materials, but sensor recovery processes were significantly hampered. To improve the sensing characteristics, Ti3C2Tx sensing layers were subjected to relatively low-temperature heat treatment in an air atmosphere to form Ti3C2Tx/TiOx nanocomposites. It was found that a high and selective oxygen response at very low operating temperatures (125-175°C) was observed for the MXenes partially oxidized, which is particularly characteristic of the material produced using the HCl-NaF system.

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Sobre autores

E. Simonenko

Kurnakov Institute of General and Inorganic Chemistry of the Russian Academy of Sciences; D.I. Mendeleev Russian University of Chemical Technology

Autor responsável pela correspondência
Email: ep_simonenko@mail.ru
Rússia, Moscow, 119991; Moscow, 125047

A. Mokrushin

Kurnakov Institute of General and Inorganic Chemistry of the Russian Academy of Sciences

Email: ep_simonenko@mail.ru
Rússia, Moscow, 119991

I. Nagornov

Kurnakov Institute of General and Inorganic Chemistry of the Russian Academy of Sciences

Email: ep_simonenko@mail.ru
Rússia, Moscow, 119991

V. Sapronova

Kurnakov Institute of General and Inorganic Chemistry of the Russian Academy of Sciences; D.I. Mendeleev Russian University of Chemical Technology

Email: ep_simonenko@mail.ru
Rússia, Moscow, 119991; Moscow, 125047

Yu. Gorban

Kurnakov Institute of General and Inorganic Chemistry of the Russian Academy of Sciences; D.I. Mendeleev Russian University of Chemical Technology

Email: ep_simonenko@mail.ru
Rússia, Moscow, 119991; Moscow, 125047

Ph. Gorobtsov

Kurnakov Institute of General and Inorganic Chemistry of the Russian Academy of Sciences

Email: ep_simonenko@mail.ru
Rússia, Moscow, 119991

T. Simonenko

Kurnakov Institute of General and Inorganic Chemistry of the Russian Academy of Sciences

Email: ep_simonenko@mail.ru
Rússia, Moscow, 119991

N. Simonenko

Kurnakov Institute of General and Inorganic Chemistry of the Russian Academy of Sciences

Email: ep_simonenko@mail.ru
Rússia, Moscow, 119991

N. Kuznetsov

Kurnakov Institute of General and Inorganic Chemistry of the Russian Academy of Sciences

Email: ep_simonenko@mail.ru
Rússia, Moscow, 119991

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2. 1. X-ray images of the initial MAX phase of Ti3AlC2 (black) and maxene samples of Ti3C2Tx obtained using LiF (blue), NaF (green) and NH4F (red).

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3. 2. Raman spectra of the initial powders of Ti3C2Tx maxenes obtained using MF–HCl etching systems, where M = Li+ (blue), Na+ (black) and NH+4 (red).

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4. Fig. 3. Microstructure of Ti3C2Tx powder obtained using the LiF–HCl system according to SEM (a–g) and TEM (d–z) data.

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5. Fig. 4. Microstructure of Ti3C2Tx powder obtained using the NaF–HCl system according to SEM (a–g) and TEM (d–z) data.

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6. 5. Microstructure of Ti3C2Tx powder obtained using the NH4F–HCl system according to SEM (a–g) and TEM (d–z) data.

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7. Fig. 6. DSC (red) and TGA (blue) curves in the air flow of Maxene Ti3C2Tx samples obtained using the LiF–HCl (a), NaF–HCl (b) and NH4F–HCl (c) systems; the insets show the superposition of TGA curves in air and argon.

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8. 7. Diagram of the selectivity of layers of individual Ti3C2Tx maxenes obtained using LiF (green), NaF (red) and NH4F (blue), made up of responses (S1, %) to various gases (100 ppm CO, benzene, acetone, ethanol, NH3, as well as 1000 ppm CH4, H2 and 10% O2), detection was performed at room temperature.

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9. 8. Raman spectra of Ti3C2Tx maxene layers obtained using LiF (blue), NaF (black) and NH4F (red) after their partial oxidation as a result of heat treatment in air at temperatures of 150 (a) and 200°C (b).

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10. 9. Responses (S2) to 10% O2 at an operating temperature of 125°C for Ti3C2Tx/TiOx nanocomposites based on Ti3C2Tx maxenes synthesized in the LiF–HCl (blue), NaF–HCl (black) and NH4F–HCl (red) systems after their partial oxidation at a temperature of 150°C.

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11. Fig. 10. Ti3C2Tx/TiOx selectivity diagram based on maxenes obtained using LiF, NaF and NH4F, compiled from responses (S2) to various gases (100 ppm CO, benzene, acetone, ethanol, NH3; 1000 ppm CH4, H2; 10% O2) (a); responses to 1-20% O2 (b) and their dependence on oxygen concentration (c). The oxidation temperature of the maxene layers is 200 °C, the detection temperatures for samples obtained using LiF and NaF are 150 °C, and for a sample obtained using NH4F, 175 C.

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