X-ray and synchrotron investigations of heterogeneous systems based on multiwalled carbon nanotubes

Сивков, В. Н.; Ob”edkov, A. M.; Петрова, О. В.; Nekipelov, S. V.; Kremlev, K. V.; Kaverin, B. S.; Semenov, N. M.; Gusev, S. A.

doi:10.1134/s1063783415010291

Cited by 10 publications

(7 citation statements)

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“…The MWCNTs and WC 1-x /MWCNT nanocomposites were studied using NEXAFS spectroscopy method in TEY mode. The background radiation contributions in the incident beam and in the TEY signal was determined using the method detailed in [42,65,66].…”

Section: Nexafs Spectroscopy Research Of the Nanocomposites And Initial Mwcntsmentioning

confidence: 99%

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

et al. 2020

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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 WC1-x nanoscale particles layer; (iii) a 3.3 nm thick non-stoichiometric tungsten oxide WO3-x layer on the WC1-x/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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Section: Nexafs Spectroscopy Research Of the Nanocomposites And Initial Mwcntsmentioning

confidence: 99%

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

et al. 2020

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“…The preparation of a hybrid material based on MWCNTs coated with pyrolytic Cr and Fe thin layers is an actual task in view of such hybrids' widespread possible application. Despite the intensive investigation of Fe/MWCNT and Cr/MWCNT composites [19][20][21], to date there are many open questions associated with both the heterocomposites synthesis technology and their physicochemical properties diagnostics. In particular, it is important to obtain detailed information about the characteristics of the composite surface and the interaction between the MWCNT outer surface and the metal coating nanolayer.…”

Section: Introductionmentioning

confidence: 99%

The Structure and Chemical Composition of the Cr and Fe Pyrolytic Coatings on the MWCNTs’ Surface According to NEXAFS and XPS Spectroscopy

et al. 2020

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The paper is devoted to the structure and properties of the composite material based on multi-walled carbon nanotubes (MWCNTs) covered with pyrolytic iron and chromium. Fe/MWCNTs and Cr/MWCNTs nanocomposites have been prepared by the metal organic chemical vapor deposition (MOCVD) growth technique using iron pentacarbonyl and bis(arene)chromium compounds, respectively. Composites structures and morphologies preliminary study were performed using X-ray diffraction, scanning and transmission electron microscopy and Raman scattering. The atomic and chemical composition of the MWCNTs’ surface, Fe-coating and Cr-coating and interface—(MWCNTs surface)/(metal coating) were studied by total electron yield method in the region of near-edge X-ray absorption fine structure (NEXAFS) C1s, Fe2p and Cr2p absorption edges using synchrotron radiation of the Russian-German dipole beamline (RGBL) at BESSY-II and the X-ray photoelectron spectroscopy (XPS) method using the ESCALAB 250 Xi spectrometer and charge compensation system. The absorption cross sections in the NEXAFS C1s edge of the nanocomposites and MWCNTs were measured using the developed approach of suppressing and estimating the contributions of the non-monochromatic background and multiple reflection orders radiation from the diffraction grating. The efficiency of the method was demonstrated by the example of the Cr/MWCNT nanocomposite, since its Cr2p NEXAFS spectra contain additional C1s NEXAFS in the second diffraction order. The study has shown that the MWCNTs’ top layers in composite have no significant destruction; the MWCNTs’ metal coatings are continuous and consist of Fe3O4 and Cr2O3. It is shown that the interface between the MWCNTs and pyrolytic Fe and Cr coatings has a multilayer structure: a layer in which carbon atoms along with epoxy –C–O–C– bonds form bonds with oxygen and metal atoms from the coating layer is formed on the outer surface of the MWCNT, a monolayer of metal carbide above it and an oxide layer on top. The iron oxide and chromium oxide adhesion is provided by single, double and epoxy chemical binding formation between carbon atoms of the MWCNT top layer and the oxygen atoms of the coating, as well as the formation of bonds with metal atoms.

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“…Deposition of pyrolytic chromium coatings on the MWCNT surface was also performed by the MOCVD method using as a precursor the "Barkhos" chromium-organic liquid, consisting of a mixture of bis-arene chromium compounds. The details of the preparation technique of the studied samples are described in the following works [1,3,4].…”

Section: Methodsmentioning

confidence: 99%

“…The most common methods of composite synthesis are the electrochemical reduction of metallic salts using the sol-gel method, metal organic chemical vapor deposition (MOCVD), and physical deposition (electron-beam sputtering, thermal spraying, etc.). In our earlier studies, it was shown that MOCVD, due to its technological characteristics, is the most appropriate method for the synthesis of MWCNT composites with a metal containing coating [1][2][3][4].…”

Section: Introductionmentioning

confidence: 99%

NEXAFS- и XPS-исследования композитов Cr/МУНТ

Nekipelov

Мингалева

Петрова

et al. 2020

kcmf

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Проведены исследования нанокомпозитов, полученных путем осаждения методом MOCVD с использованием хроморганической жидкости «Бархос» слоев разной толщины пиролитического хрома на внешнюю поверхность многостенных углеродных нанотрубок (МУНТ). Данные покрытия из пиролитического Cr имеют высокую микротвердость, термостойкость, гидрофобность и химическую стойкость по отношению к соляной и серной кислотам и расплаву щелочей.Уникальные физические свойства хромовых покрытий, а также химическая стойкость в широком диапазоне температур и большая внешняя поверхность МУНТ открывают широкие перспективы возможных приложений исследуемых нанокомпозитов. Важной проблемой в этом случае является выяснение механизмов адгезии хрома на химически инертную поверхность МУНТ.Перспективным методом изучения интерфейса поверхность МУНТ – покрывающий слой является ультрамягкая рентгеновская спектроскопия в области NEXAFS 1s – порога ионизации углерода. Однако такие исследования для соединений хрома практически отсутствуют в литературе по причине наложения структуры NEXAFS Cr2p-спектров поглощения на область NEXAFS C1s – порога ионизации. В настоящей работе исследования нанокомпозитов были проведены методом полного выхода электронов с использованием оригинальной методики подавления и измерениявклада кратных порядков в области C1s – края поглощения. Проведенные методами NEXAFS и XPS-спектроскопии исследования нанокомпозита (пиролитический Cr) / МУНТ показали: (i) в спектре композита сохраняются особенности, характерные для чистой МУНТ; (ii) отсутствиесущественной деструкции внешних слоев МУНТ; (iii) интерфейс между МУНТ и покрытием пиролитического хрома представляет собой многослойную структуру. Эта структура включает внешнюю поверхность МУНТ, атомы которой образуют С–О и С–Cr связи с покрытием пиролитического хрома, монослой карбида хрома и покрывающий слой оксида хрома (Cr2O3). Для исследованных образцов определены эффективные толщины покрывающих слоев оксидаи карбида хрома 1.5 и 0.3 нм соответственно. ЛИТЕРАТУРА Ob’edkov A. M., Kaverin B. S., Gusev S. A., Ezerskii A. B., Semenov N. M., Zaytsev A. A., Egorov V. A., Domrachev G. A. MOCVD modifi cation of the surface of multiwalled carbon nanotubes to impart to them necessary physicochemical properties. Journal of Surface Investigation. 2009; 3(4): 554–558. DOI: https://doi.org/10.1134/S1027451009040120 Кириллов А. И., Объедков А. М., Егоров В. А., Домрачев Г. А., Каверин Б. С., Семенов Н. М., Лопатина Т. И., Гусев С. А., Мансфельд А. Д. Создание с помощью MOCVD-технологии наноструктурированных композиционных материалов на основе многостенных углеродных нанотрубок. Нанотехника. 2011; 1(25): 72–78. Sivkov V. N., Ob’edkov A. M., Petrova O. V., Nekipelov S. V., Kremlev K.V ., Kaverin B. S., Semenov N. M., Gusev S. A. X-ray and synchrotron investigations of heterogeneous systems based on multiwalled carbon nanotubes. Physics of the Solid State. 2015;57(1): 197–204. DOI: https://doi.org/10.1134/S1063783415010291 Petrova O. V., Nekipelov S. V., Mingaleva A. E., Sivkov V. N., Obiedkov A. M., Kaverin B. S., Kremlev K. V., Ketkov S. Yu., Gusev S. A., Vyalikh D. V., Molodtsov S. L. Study of composite MWCNT/pyrolytic Cr interface by NEXAFS spectroscopy. Journal of Physics: Conference Series. 2016;741(1): 012038. DOI: https://doi.org/10.1088/1742-6596/741/1/012038 Fedoseenko S. I., Iossifov I. F., Gorovikov S. A., Schmidt J., Follath R., Molodtsov S. L., Adamchuk V. K., Kaindl G. Development and present status of the Russian-German soft X-ray beamline at BESSY II. Nucl. Instr. and Meth. A. 2001;470: 84-88. DOI: https://doi.org/10.1016/S0168-9002(01)01032-4 Kummer K., Sivkov V. N., Vyalikh D. V., Maslyuk V. V., Bluher A., Nekipelov S. V., Bredow T., Mertig I., Mertig M., Molodtsov S. L. Oscillator strength of the peptide bond p*-resonances at all relevant x-ray absorption edges. Physical Review B. 2009;80: 155433–155438. DOI: https://doi.org/10.1103/PhysRevB.80.155433 Jeong H.-K., Noh H.-J., Kim J.-Y., Jin M.H., Park C. Y., and Lee Y. H. X-ray absorption spectroscopy of graphite oxide. Europhysics Letters. 2008;82: 67004-1–5. DOI: https://doi.org/10.1209/0295-5075/82/67004 Madix R. J., Solomon J. L., and Stцhr J. The orientation of the carbonate anion on Ag(110). Surf. Sci. 1988;197: L253–L259. DOI: https://doi.org/10.1016/0039-6028(88)90624-3 Chen J. G. NEXAFS investigations of transition metal oxides, nitrides, carbides, sulfi des and otherinterstitial compounds. Surface Science Report. 1997;30: 1–152. DOI: https://doi.org/10.1016/S0167-5729(97)00011-3 Ruihua Cheng B. Xu., Borca C. N., Sokolov A., Yang C.-S., Yuan L., Liou S.-H., Doudin B., Dowben P. A. Characterization of the native Cr2O3 oxide surface of CrO2. Appl. Phys. Letters. 2001;79: 3122–3124. DOI: https://doi.org/10.1063/1.1416474 NIST Standard Reference Database 71. NIST Electron Inelastic-Mean-Free-Path Database: Version1.2. Режим доступа: www.nist.gov/srd/nist-standardreference-database-71 Teghil R., Santagata A., De Bonis A., Galasso A., Villani P. Chromium carbide thin fi lms deposited by ultra-short pulse laser deposition. Applied Surface Science. 2009; 255: 7729–7733. DOI: https://doi.org/10.1016/j.apsusc.2009.04.151 Zhao D., Jiang X., Wang Y., Duan W., Wang L. Microstructure evolution, wear and corrosion resistance of Cr-C nanocomposite coatings in seawater. Applied Surface Science. 2018;457: 914–924. DOI: https://doi.org/10.1016/j.apsusc.2018.06.248

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X-ray and synchrotron investigations of heterogeneous systems based on multiwalled carbon nanotubes

Cited by 10 publications

References 14 publications

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

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

The Structure and Chemical Composition of the Cr and Fe Pyrolytic Coatings on the MWCNTs’ Surface According to NEXAFS and XPS Spectroscopy

NEXAFS- и XPS-исследования композитов Cr/МУНТ

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