High-Pressure Monosulfide Solid Solution Fe<sub>x</sub>Ni<sub>1−x</sub>S Phases: X-Ray Diffraction Analysis and Raman Spectroscopy

High-pressure high-temperature (HPHT) crystalline monosulfide solid solution (Mss) phases (Fe<sub>x</sub>Ni<sub>1−x</sub>S, x = 0.90, 0.75, 0.50, 0.25), troilite (FeS I), and α-NiS of the Fe-Ni-S system were synthesized at 7 GPa and 900–1550 °C. The structural parameters of t...

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Main Authors: Anna V. Spivak, Ninel Yu. Sharapova, Tatiana V. Setkova, Andrey V. Bobrov, Vitaliy I. Korepanov, Anastasia V. Iskrina, Egor S. Zakharchenko, Mikhail V. Voronin, Natalia A. Drozhzhina
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Language:English
Published: MDPI AG 2024-11-01
Series:Crystals
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Online Access:https://www.mdpi.com/2073-4352/14/11/967
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author Anna V. Spivak
Ninel Yu. Sharapova
Tatiana V. Setkova
Andrey V. Bobrov
Vitaliy I. Korepanov
Anastasia V. Iskrina
Egor S. Zakharchenko
Mikhail V. Voronin
Natalia A. Drozhzhina
author_facet Anna V. Spivak
Ninel Yu. Sharapova
Tatiana V. Setkova
Andrey V. Bobrov
Vitaliy I. Korepanov
Anastasia V. Iskrina
Egor S. Zakharchenko
Mikhail V. Voronin
Natalia A. Drozhzhina
author_sort Anna V. Spivak
collection DOAJ
description High-pressure high-temperature (HPHT) crystalline monosulfide solid solution (Mss) phases (Fe<sub>x</sub>Ni<sub>1−x</sub>S, x = 0.90, 0.75, 0.50, 0.25), troilite (FeS I), and α-NiS of the Fe-Ni-S system were synthesized at 7 GPa and 900–1550 °C. The structural parameters of the obtained phases were refined by XRD using the Rietveld method. Factor group analysis revealed the number of active Raman modes for FeS I and α-NiS. Raman spectra of troilite, α-NiS, and Mss phases were obtained. It was shown that the Raman spectra of Mss phases and α-NiS have a similar topology. The Raman spectra of the experimental phases in the Fe-Ni-S system were analyzed with non-negative matrix factorization, which provided a meaningful concentration dependence of the spectral patterns. The spectral components were assigned to the FeS I and α-NiS structures. The structural and spectroscopic studies show linear dependencies of unit cell parameters and spectral components on composition and confirm the existence of a series of monosulfide solid solution Fe<sub>x</sub>Ni<sub>1−x</sub>S.
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series Crystals
spelling doaj-art-2d20ef57a03f4e5db7f85fcff6e7fdc02024-11-26T17:58:40ZengMDPI AGCrystals2073-43522024-11-01141196710.3390/cryst14110967High-Pressure Monosulfide Solid Solution Fe<sub>x</sub>Ni<sub>1−x</sub>S Phases: X-Ray Diffraction Analysis and Raman SpectroscopyAnna V. Spivak0Ninel Yu. Sharapova1Tatiana V. Setkova2Andrey V. Bobrov3Vitaliy I. Korepanov4Anastasia V. Iskrina5Egor S. Zakharchenko6Mikhail V. Voronin7Natalia A. Drozhzhina8Korzhinskii Institute of Experimental Mineralogy of Russian Academy of Sciences (IEM RAS), Chernogolovka 142342, RussiaKorzhinskii Institute of Experimental Mineralogy of Russian Academy of Sciences (IEM RAS), Chernogolovka 142342, RussiaKorzhinskii Institute of Experimental Mineralogy of Russian Academy of Sciences (IEM RAS), Chernogolovka 142342, RussiaKorzhinskii Institute of Experimental Mineralogy of Russian Academy of Sciences (IEM RAS), Chernogolovka 142342, RussiaInstitute of Microelectronics Technology and High Purity Materials of Russian Academy of Sciences (IMT RAS), Chernogolovka 142342, RussiaKorzhinskii Institute of Experimental Mineralogy of Russian Academy of Sciences (IEM RAS), Chernogolovka 142342, RussiaKorzhinskii Institute of Experimental Mineralogy of Russian Academy of Sciences (IEM RAS), Chernogolovka 142342, RussiaKorzhinskii Institute of Experimental Mineralogy of Russian Academy of Sciences (IEM RAS), Chernogolovka 142342, RussiaKorzhinskii Institute of Experimental Mineralogy of Russian Academy of Sciences (IEM RAS), Chernogolovka 142342, RussiaHigh-pressure high-temperature (HPHT) crystalline monosulfide solid solution (Mss) phases (Fe<sub>x</sub>Ni<sub>1−x</sub>S, x = 0.90, 0.75, 0.50, 0.25), troilite (FeS I), and α-NiS of the Fe-Ni-S system were synthesized at 7 GPa and 900–1550 °C. The structural parameters of the obtained phases were refined by XRD using the Rietveld method. Factor group analysis revealed the number of active Raman modes for FeS I and α-NiS. Raman spectra of troilite, α-NiS, and Mss phases were obtained. It was shown that the Raman spectra of Mss phases and α-NiS have a similar topology. The Raman spectra of the experimental phases in the Fe-Ni-S system were analyzed with non-negative matrix factorization, which provided a meaningful concentration dependence of the spectral patterns. The spectral components were assigned to the FeS I and α-NiS structures. The structural and spectroscopic studies show linear dependencies of unit cell parameters and spectral components on composition and confirm the existence of a series of monosulfide solid solution Fe<sub>x</sub>Ni<sub>1−x</sub>S.https://www.mdpi.com/2073-4352/14/11/967crystal structuresolid solutionsrecrystallizationRamanX-ray diffractionminerals
spellingShingle Anna V. Spivak
Ninel Yu. Sharapova
Tatiana V. Setkova
Andrey V. Bobrov
Vitaliy I. Korepanov
Anastasia V. Iskrina
Egor S. Zakharchenko
Mikhail V. Voronin
Natalia A. Drozhzhina
High-Pressure Monosulfide Solid Solution Fe<sub>x</sub>Ni<sub>1−x</sub>S Phases: X-Ray Diffraction Analysis and Raman Spectroscopy
Crystals
crystal structure
solid solutions
recrystallization
Raman
X-ray diffraction
minerals
title High-Pressure Monosulfide Solid Solution Fe<sub>x</sub>Ni<sub>1−x</sub>S Phases: X-Ray Diffraction Analysis and Raman Spectroscopy
title_full High-Pressure Monosulfide Solid Solution Fe<sub>x</sub>Ni<sub>1−x</sub>S Phases: X-Ray Diffraction Analysis and Raman Spectroscopy
title_fullStr High-Pressure Monosulfide Solid Solution Fe<sub>x</sub>Ni<sub>1−x</sub>S Phases: X-Ray Diffraction Analysis and Raman Spectroscopy
title_full_unstemmed High-Pressure Monosulfide Solid Solution Fe<sub>x</sub>Ni<sub>1−x</sub>S Phases: X-Ray Diffraction Analysis and Raman Spectroscopy
title_short High-Pressure Monosulfide Solid Solution Fe<sub>x</sub>Ni<sub>1−x</sub>S Phases: X-Ray Diffraction Analysis and Raman Spectroscopy
title_sort high pressure monosulfide solid solution fe sub x sub ni sub 1 x sub s phases x ray diffraction analysis and raman spectroscopy
topic crystal structure
solid solutions
recrystallization
Raman
X-ray diffraction
minerals
url https://www.mdpi.com/2073-4352/14/11/967
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