Synthesis and characterization of mixed bimetallic layered (Cr,V)C carbide

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Resumo

The paper presents the synthesis of layered complex carbide of the composition (Cr,V)C using reactive spark plasma sintering (SPS-RS) and hydrothermal acid etching. Using SEM and TEM, a detailed study of the macro- and nano-structure at each stage of MAXene synthesis was carried out. The presence of characteristic features of the formation of two-dimensional carbide in the form of particles and fragments of a multilayer structure at the macro- and nanolevel was confirmed. Using EDS and XRD, the elemental and phase composition of the samples was studied, as a result it was found that the initial expected MAX-phase Cr2VAlC2 in the composition of the sample obtained by SPS is absent. At the same time, a phase of mixed bimetallic carbide (Cr,V)C was detected at all stages of synthesis, for which the crystal lattice parameters, including the unit cell volume, change significantly after acid etching. Obvious changes in the bulk and crystalline structure of (Cr,V)C correspond to the formation of two-dimensional nanoparticles in the synthesized material. The magnetic characteristics study showed that all samples have magnetic hysteresis with relatively low values of coercivity and remanence to saturation magnetization ratio. Low-temperature measurements showed a slight increase in magnetic moment with decreasing temperature for the sample obtained under reaction SPS conditions before acid etching in HF, without significant changes in magnetic behavior of the samples.

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Sobre autores

E. Papynov

Far Eastern Federal University

Autor responsável pela correspondência
Email: papynov@mail.ru
Rússia, Vladivostok

A. Ognev

Far Eastern Federal University; Sakhalin State University

Email: papynov@mail.ru
Rússia, Vladivostok; Yuzhno-Sakhalinsk

M. Gurin

Far Eastern Federal University

Email: papynov@mail.ru
Rússia, Vladivostok

N. Ivanov

Far Eastern Federal University

Email: papynov@mail.ru
Rússia, Vladivostok

O. Shichalin

Far Eastern Federal University; Sakhalin State University

Email: papynov@mail.ru
Rússia, Vladivostok; Yuzhno-Sakhalinsk

A. Lembikov

Far Eastern Federal University

Email: papynov@mail.ru
Rússia, Vladivostok

M. Sobirov

Far Eastern Federal University

Email: papynov@mail.ru
Rússia, Vladivostok

K. Rogachev

Far Eastern Federal University

Email: papynov@mail.ru
Rússia, Vladivostok

A. Samardak

Far Eastern Federal University

Email: papynov@mail.ru
Rússia, Vladivostok

A. Samardak

Far Eastern Federal University; Sakhalin State University

Email: papynov@mail.ru
Rússia, Vladivostok; Yuzhno-Sakhalinsk

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2. Fig. 1. SEM images of the structure of the sample obtained by IPS: A, B, C – local areas of enlarged scale.

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3. Fig. 2. TEM images of the structure of the sample obtained by IPS: A, B – local areas of increased scale.

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4. Fig. 3. SEM images of the sample structure after acid etching: A, B, C – local areas of enlarged scale.

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5. Fig. 4. TEM images of the sample structure after acid etching: A, B – local areas of enlarged scale.

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6. Fig. 5. EDS analysis of the sample surface before (a) and after acid etching (b).

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7. Fig. 6. Experimental and simulated X-ray diffraction profiles for a sample obtained by IPS.

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8. Fig. 7. Experimental and simulated X-ray diffraction profiles for a sample of layered complex chromium-vanadium carbide.

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9. Fig. 8. Magnetic hysteresis loops of the studied samples (a) (the inset shows a loop for a sample of two-dimensional nanoparticles of the composition (Cr,V)C) and normalized loops (b).

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10. Fig. 9. Magnetic hysteresis loops for samples before (a) and after (b) acid etching (layered complex carbide of composition (Cr,V)C). The red line indicates magnetic hysteresis loops obtained at room temperature, the blue line – at 100 K.

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11. Fig. 10. Cooling curves in the zero ZFC field (a) and in the FC field (b) for all samples.

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