Studies of Buried Layers and Interfaces of Tungsten Carbide Coatings on the MWCNT Surface by XPS and NEXAFS Spectroscopy

Currently, X-ray photoelectron spectroscopy (XPS) is widely used to characterize the nanostructured material surface. The ability to determine the atom distribution and chemical state with depth without the sample destruction is important for studying the internal structure of the coating layer seve...

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Main Authors: Danil Sivkov, Sergey Nekipelov, Olga Petrova, Alexander Vinogradov, Alena Mingaleva, Sergey Isaenko, Pavel Makarov, Anatoly Ob’edkov, Boris Kaverin, Sergey Gusev, Ilya Vilkov, Artemiy Aborkin, Viktor Sivkov
Format: Article
Language:English
Published: MDPI AG 2020-07-01
Series:Applied Sciences
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Online Access:https://www.mdpi.com/2076-3417/10/14/4736
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author Danil Sivkov
Sergey Nekipelov
Olga Petrova
Alexander Vinogradov
Alena Mingaleva
Sergey Isaenko
Pavel Makarov
Anatoly Ob’edkov
Boris Kaverin
Sergey Gusev
Ilya Vilkov
Artemiy Aborkin
Viktor Sivkov
author_facet Danil Sivkov
Sergey Nekipelov
Olga Petrova
Alexander Vinogradov
Alena Mingaleva
Sergey Isaenko
Pavel Makarov
Anatoly Ob’edkov
Boris Kaverin
Sergey Gusev
Ilya Vilkov
Artemiy Aborkin
Viktor Sivkov
author_sort Danil Sivkov
collection DOAJ
description Currently, X-ray photoelectron spectroscopy (XPS) is widely used to characterize the nanostructured material surface. The ability to determine the atom distribution and chemical state with depth without the sample destruction is important for studying the internal structure of the coating layer several nanometers thick, and makes XPS the preferable tool for the non-destructive testing of nanostructured systems. In this work, ultra-soft X-ray spectroscopy methods are used to study hidden layers and interfaces of pyrolytic tungsten carbide nanoscale coatings on the multi-walled carbon nanotube (MWCNT) surfaces. XPS measurements were performed using laboratory spectrometers with sample charge compensation, and Near Edge X-ray Absorption Fine Structure (NEXAFS) studies using the Russian–German dipole beamline (RGBL) synchrotron radiation at BESSY-II. The studied samples were tested by scanning and transmission electron microscopy, X-ray diffractometry, Raman scattering and NEXAFS spectroscopy. It was shown that the interface between MWCNT and the pyrolytic coating of tungsten carbide has a three-layer structure: (i) an interface layer consisting of the outer graphene layer carbon atoms, forming bonds with oxygen atoms from the oxides adsorbed on the MWCNT surface, and tungsten atoms from the coating layer; (ii) a non-stoichiometric tungsten carbide WC<sub>1-x</sub> nanoscale particles layer; (iii) a 3.3 nm thick non-stoichiometric tungsten oxide WO<sub>3-x</sub> layer on the WC<sub>1-x</sub>/MWCNT nanocomposite outer surface, formed in air. The tungsten carbide nanosized particle’s adhesion to the nanotube outer surface is ensured by the formation of a chemical bond between the carbon atoms from the MWCNT upper layer and the tungsten atoms from the coating layer.
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spelling doaj.art-e587abc8ada74154a4bf25263619fecc2023-11-20T06:20:56ZengMDPI AGApplied Sciences2076-34172020-07-011014473610.3390/app10144736Studies of Buried Layers and Interfaces of Tungsten Carbide Coatings on the MWCNT Surface by XPS and NEXAFS SpectroscopyDanil Sivkov0Sergey Nekipelov1Olga Petrova2Alexander Vinogradov3Alena Mingaleva4Sergey Isaenko5Pavel Makarov6Anatoly Ob’edkov7Boris Kaverin8Sergey Gusev9Ilya Vilkov10Artemiy Aborkin11Viktor Sivkov12Faculty of Physics, Federal State Budgetary Educational Institution of Higher Education “Saint-Petersburg State University”, 199034 St. Petersburg, RussiaInstitute of Physics and Mathematics, Komi Science Center Ural Division of the Russian Academy of Sciences, 167982 Syktyvkar, RussiaInstitute of Physics and Mathematics, Komi Science Center Ural Division of the Russian Academy of Sciences, 167982 Syktyvkar, RussiaFaculty of Physics, Federal State Budgetary Educational Institution of Higher Education “Saint-Petersburg State University”, 199034 St. Petersburg, RussiaInstitute of Physics and Mathematics, Komi Science Center Ural Division of the Russian Academy of Sciences, 167982 Syktyvkar, RussiaInstitute of Physics and Mathematics, Komi Science Center Ural Division of the Russian Academy of Sciences, 167982 Syktyvkar, RussiaInstitute of Physics and Mathematics, Komi Science Center Ural Division of the Russian Academy of Sciences, 167982 Syktyvkar, RussiaHybrid Nanomaterials Laboratory, G.A.Razuvaev Institute of Organometallic Chemistry of the Russian Academy of Sciences, 603950 Nizhny Novgorod, RussiaHybrid Nanomaterials Laboratory, G.A.Razuvaev Institute of Organometallic Chemistry of the Russian Academy of Sciences, 603950 Nizhny Novgorod, RussiaDepartment of Magnetic Nanostructures, Institute for Physics of Microstructures of the Russian Academy of Sciences, 603950 Nizhny Novgorod, RussiaHybrid Nanomaterials Laboratory, G.A.Razuvaev Institute of Organometallic Chemistry of the Russian Academy of Sciences, 603950 Nizhny Novgorod, RussiaInstitute of Engineering, Vladimir State University Named after Alexander and Nikolay Stoletovs, Gorky Str. 87, 600000 Vladimir, RussiaInstitute of Physics and Mathematics, Komi Science Center Ural Division of the Russian Academy of Sciences, 167982 Syktyvkar, RussiaCurrently, X-ray photoelectron spectroscopy (XPS) is widely used to characterize the nanostructured material surface. The ability to determine the atom distribution and chemical state with depth without the sample destruction is important for studying the internal structure of the coating layer several nanometers thick, and makes XPS the preferable tool for the non-destructive testing of nanostructured systems. In this work, ultra-soft X-ray spectroscopy methods are used to study hidden layers and interfaces of pyrolytic tungsten carbide nanoscale coatings on the multi-walled carbon nanotube (MWCNT) surfaces. XPS measurements were performed using laboratory spectrometers with sample charge compensation, and Near Edge X-ray Absorption Fine Structure (NEXAFS) studies using the Russian–German dipole beamline (RGBL) synchrotron radiation at BESSY-II. The studied samples were tested by scanning and transmission electron microscopy, X-ray diffractometry, Raman scattering and NEXAFS spectroscopy. It was shown that the interface between MWCNT and the pyrolytic coating of tungsten carbide has a three-layer structure: (i) an interface layer consisting of the outer graphene layer carbon atoms, forming bonds with oxygen atoms from the oxides adsorbed on the MWCNT surface, and tungsten atoms from the coating layer; (ii) a non-stoichiometric tungsten carbide WC<sub>1-x</sub> nanoscale particles layer; (iii) a 3.3 nm thick non-stoichiometric tungsten oxide WO<sub>3-x</sub> layer on the WC<sub>1-x</sub>/MWCNT nanocomposite outer surface, formed in air. The tungsten carbide nanosized particle’s adhesion to the nanotube outer surface is ensured by the formation of a chemical bond between the carbon atoms from the MWCNT upper layer and the tungsten atoms from the coating layer.https://www.mdpi.com/2076-3417/10/14/4736XPSNEXAFSTEYMWCNTWC<sub>1-x</sub>/MWCNTsMOCVD
spellingShingle Danil Sivkov
Sergey Nekipelov
Olga Petrova
Alexander Vinogradov
Alena Mingaleva
Sergey Isaenko
Pavel Makarov
Anatoly Ob’edkov
Boris Kaverin
Sergey Gusev
Ilya Vilkov
Artemiy Aborkin
Viktor Sivkov
Studies of Buried Layers and Interfaces of Tungsten Carbide Coatings on the MWCNT Surface by XPS and NEXAFS Spectroscopy
Applied Sciences
XPS
NEXAFS
TEY
MWCNT
WC<sub>1-x</sub>/MWCNTs
MOCVD
title Studies of Buried Layers and Interfaces of Tungsten Carbide Coatings on the MWCNT Surface by XPS and NEXAFS Spectroscopy
title_full Studies of Buried Layers and Interfaces of Tungsten Carbide Coatings on the MWCNT Surface by XPS and NEXAFS Spectroscopy
title_fullStr Studies of Buried Layers and Interfaces of Tungsten Carbide Coatings on the MWCNT Surface by XPS and NEXAFS Spectroscopy
title_full_unstemmed Studies of Buried Layers and Interfaces of Tungsten Carbide Coatings on the MWCNT Surface by XPS and NEXAFS Spectroscopy
title_short Studies of Buried Layers and Interfaces of Tungsten Carbide Coatings on the MWCNT Surface by XPS and NEXAFS Spectroscopy
title_sort studies of buried layers and interfaces of tungsten carbide coatings on the mwcnt surface by xps and nexafs spectroscopy
topic XPS
NEXAFS
TEY
MWCNT
WC<sub>1-x</sub>/MWCNTs
MOCVD
url https://www.mdpi.com/2076-3417/10/14/4736
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