Electron Paramagnetic Resonance in Modern Carbon-Based Nanomaterials E-Book

• Herausgeber: Bentham Science Publishers
• Kategorie: Wissenschaft und neue Technologien
• Serie: Frontiers in Magnetic Resonance
• Sprache: Englisch

Seitenzahl: 510

Veröffentlichungsjahr: 2018

Beschreibung

This volume presents information about several topics in the field of electron paramagnetic resonance EPR study of carbon-containing nanomaterials. It introduces the reader to an array of experimental and theoretical approaches for the analysis of param

Leseprobe

Table of Contents

Welcome

Table of Contents

Title

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FOREWORD

PREFACE

List of Contributors

Fundamentals of Electron Paramagnetic Resonance in Modern Carbon-based Materials

Abstract

ELECTRON ZEEMAN EFFECT: EPR RESONANCE CONDITION

HYPERFINE SPLITTING

EPR LINE SHAPES

SPIN HAMILTONIAN

SIMULATION OF EPR SPECTRA

Simulation of Single-crystal Spectrum

Transition Probability

Lineshape function F(Bri, Bk)

Simulation of a Polycrystalline Spectrum

Calculation of First-derivative EPR Spectrum

PULSE EPR

Nuclear Modulation Effects Leading to ENDOR and ESEEM

CW ENDOR: Theory

ENDOR Instrumentation

Mims and Davies Pulsed ENDOR Sequences

Davies ENDOR

Mims ENDOR

Electron Spin Echo Envelope Modulation (ESEEM) and Hyperfine Sublevel Correlation Spectroscopy (HYSCORE)

CW EPR SPECTROMETERS

Continuous Wave EPR

Typical X-band, Low- and High-frequency CW Spectrometers

X-band EPR Spectrometer Design ([10])

Design of Low-frequency Spectrometers

Design of High-frequency (hf) Spectrometers

EPR IN CARBON-BASED MATERIALS

CONCLUSION

Consent for Publication

CONFLICT OF INTEREST

ACKNOWLEDGEMENT

REFERENCES

Resolution of EPR Signals in Graphene-based Materials from Few Layers to Nanographites

Abstract

INTRODUCTION

Bulk Material, Edges and Defects

Conduction Electrons

Edges and Edge States

Defects and Molecular States

Oxygen

CONTINUOUS WAVE EPR SPECTRA

Lineshape

Temperature Variation of the Spectra and Separation of the Components

g-Values

PULSE EPR SPECTRA

FT- and ED-EPR

Hyperfine Spectroscopies

CONCLUSION

Consent for Publication

CONFLICT OF INTEREST

ACKNOWLEDGEMENT

REFERENCES

Study of Electron Spin Lifetime of Conducting Carbon Nanomaterials

Abstract

INTRODUCTION

Spin Dynamics and Electron Spin Resonance for Spintronics

Coherent Control of the Quantum State of Electron Spin

ESR AND SPIN DYNAMICS OF SYNTHETIC GRAPHENE

ESR AND SPIN DYNAMICS OF CONDUCTING CARBON NANOSPHERES

PERSPECTIVES & OUTLOOK

Consent for Publication

CONFLICT OF INTEREST

ACKNOWLEDGEMENT

REFERENCES

EPR Spectroscopy on Double-Walled and Multi-Walled Carbon Nanotube Polymer Composites

Abstract

INTRODUCTION

DOUBLE-WALL CARBON NANOTUBES

Materials and Methods

Electron Paramagnetic Resonance

MULTIWALL CARBON NANOTUBE POLY(ETHER-ESTER) NANOCOMPOSITES

Materials and Methods

Static Magnetization

Electron Paramagnetic Resonance

CONCLUDING REMARKS

Consent for Publication

CONFLICT OF INTEREST

ACKNOWLEDGEMENT

REFERENCES

Impact of Point Defects on Graphene Oxide and Carbon Nanotubes: Study of Electron Paramagnetic Resonance Spectroscopy

Abstract

INTRODUCTION

EPR INVESTIGATIONS OF FUNCTIONALIZED GRAPHENE AND CARBON NANOTUBES

MATERIALS AND METHODS

Synthesis

EPR EXPERIMENTS

Spin-counting Procedure

RESULTS AND DISCUSSIONS

Elimination of Mn2+ Impurities Within GO and O-CNT Samples

EPR investigation of Graphene and CNT with Different Functional Groups

Comparison of EPR Signals of TrGO and CNT-SH

Dependence of EPR Signals of O-CNT and TrGO on Temperatures

CONCLUSIONS ON THE EPR BEHAVIORS OF FUNCTIONALIZED MWCNTS AND GRAPHENE

INVESTIGATION OF CHARGE TRANSFER WITHIN QUANTUM DOTS – GRAPHENE HYBRID MATERIALS USING EPR QUENCHING EXPERIMENTS

Charge Transfer Within CdSe QD-TrGO Hybrid Materials

Charge Transfer Within GO-ZnO and TrGO-ZnO Hybrid Materials

CONCLUSION

Consent for Publication

CONFLICT OF INTEREST

ACKNOWLEDGEMENT

REFERENCES

Electron Spin Resonance Spectroscopy of Single-Walled Carbon-Nanotube Thin-Films and their Transistors

Abstract

INTRODUCTION

EXPERIMENTAL

SW-CNT Thin Film and Transistor Fabrication

ESR and Transfer Characteristic Measurements

RESULTS AND DISCUSSION

Gate Voltage Dependence of ESR of SW-CNT Transistors

Electrically Induced Ambipolar Spin Vanishment in SW-CNTs

No ESR Observation in Tomonaga-Luttinger Liquid

Microscopic Investigation into Atomic Vacancies in SW-CNTs

Anisotropic Spin-orbital Interaction in SW-CNTs

CONCLUSIONS

Consent for Publication

CONFLICT OF INTEREST

ACKNOWLEDGEMENT

REFERENCES

Characterizing the Nature of Surface Radicals in Carbon-Based Materials, Using Gas-Flow EPR Spectroscopy

Abstract

INTRODUCTION

EXPERIMENTAL METHODS

Experimental Setup: In Situ Gas Flow EPR Experiments on Carbon-based Materials

General Characteristics of EPR Spectra of Radicals in Carbon-based Materials

EPR ON COAL SAMPLES

Coal Samples

Oxidation Processes Occurring at 95 °C on a Timescale of Weeks

EPR Experiments

g-values

Line-width

Radical Concentrations

Comparison with Previous Results

Summary of EPR Spectroscopy Results

Nuclear Magnetic Resonance (NMR) Studies

Summary and Conclusions

IN-SITU OXIDATION MEASUREMENTS AT ROOM TEMPERATURE (RT) ON A TIMESCALE OF MINUTES

EPR Experiments

Comparison with Prior Results

EPR ON GRAPHENE OXIDE-BASED MATERIALS

EPR Spectroscopy of Graphene Oxide Reduced at Different Temperatures

In-situ Oxidation Measurements at RT for Graphene Oxide Materials

OUTLOOK

Consent for Publication

CONFLICT OF INTEREST

ACKNOWLEDGEMENT

REFERENCES

Application of the Two-Temperature EPR Measurement Method to Carbonaceous Solids

Abstract

INTRODUCTION

THE TWO-TEMPERATURE MEASUREMENT METHOD

CARBONACEOUS SOLIDS WITH PAULI PARAMAGNETISM

Carbon Black

Pyrolytic carbon

Multi-walled Carbon Nanotubes (MWCNTs)

COAL MACERALS WITH THERMALLY EXCITED TRIPLET STATES

CONCLUSION

Consent for Publication

CONFLICT OF INTEREST

ACKNOWLEDGEMENT

REFERENCES

Paramagnetic Defects and Impurities in Nanodiamonds as Studied by Multi-frequency CW and Pulse EPR Methods

Abstract

INTRODUCTION

STUDY OF NITROGEN CENTRES IN NANODIAMONDS

NV CENTERS IN DIAMONDS CREATED BY SINTERING PROCEDURE OF DETONATION NANODIAMONDS

CONCLUSIONS AND OUTLOOK

Consent for Publication

CONFLICT OF INTEREST

ACKNOWLEDGEMENT

REFERENCES

EPR and FMR of SiCN Ceramics and SiCN Magnetic Derivatives

Abstract

INTRODUCTION

SYNTHESIS AND STRUCTURE

SiCN/Fe Ceramics

SiCN/Mn Ceramics

PURE SiCN: EPR OF CARBON RELATED DANGLING BONDS

Temperature Variation of the EPR Linewidth and Estimation of Exchange Interaction

EPR STUDY OF SiCN/Fe AND THE TRANSFORMATIONS AT VARIOUS PYROLYSIS TEMPERATURES

EPR/FMR Spectra of SiCN/Fe Ceramics

Temperature Dependence of Fe3+ EPR Lines

EPR/FMR STUDY OF SiCN/Mn CERAMICS

FMR lines

EPR Lines

CONCLUDING REMARKS AND DISCUSSION

Consent for Publication

CONFLICT OF INTEREST

ACKNOWLEDGEMENTS

REFERENCES

CW and Pulse EPR Study of Paramagnetic Centers in Silicon Carbide Nanomaterials

Abstract

INTRODUCTION

SAMPLE CHARACTERIZATION AND EXPERIMENTAL TECHNIQUE

EXPERIMENTAL RESULTS

CW and Pulsed EPR Study of the SiC Nanoparticles

ENDOR and HYSCORE Study of SHF Structure of VC in the β-SiC Crystalline Phase

CONCLUSION

Consent for Publication

CONFLICT OF INTEREST

ACKNOWLEDGEMENT

REFERENCES

Size-dependent Effects in Silicon Carbide and Diamond Nanomaterials as Studied by CW and Pulse EPR Methods

Abstract

INTRODUCTION

SAMPLE CHARACTERIZATION AND EXPERIMENTAL TECHNIQUE

SIZE EFFECT IN ED EPR SPECTRA OF SIC NANOPARTICLES

SIZE EFFECT IN EPR SPECTRA OF NANODIAMONDS

SIZE EFFECT IN ENDOR SPECTRA OF SIC NANOPARTICLES

CONCLUSION

Consent for Publication

CONFLICT OF INTEREST

ACKNOWLEDGEMENT

REFERENCES

Paramagnetic Defects in Amorphous Hydrogenated Silicon Carbide and Silicon Carbonitride Films

Abstract

INTRODUCTION

SAMPLE CHARACTERIZATION AND EXPERIMENTAL TECHNIQUE

PARAMAGNETIC DEFECTS IN a-Si1-xCx:H FILMS

EPR Spectra in the Initial a-Si1-xCx:H Films

The Impact of Thermal Treatment on the EPR Spectra of the a-Si1-xCx:H Films

The Temperature Dependence of g-tensor Anisotropy of the CRD Signal in a-Si1-xCx:H Films Annealed at High Temperatures

Evaluation of the sp2/sp3 Carbon Ratio in the Initial a-Si1-xCx:H Films

MAGNETIC PROPERTIES OF THE HIGH TEMPERATURE ANNEALED a-Si1-xCx:H FILMS

Magnetization Effect in High Temperature Annealed a-Si1-xCx:H Films

Temperature Dependence of Q-band EPR Spectra in a-Si1-xCx:H Films

Magnetic Ordering in CRD and SiDB Clusters in a-Si1-xCx:H Film

PARAMAGNETIC DEFECTS IN a-SiCxNy FILMS AND THEIR MAGNETIC PROPERTIES

CW and Pulsed EPR Spectra in a-SiCxNy Films

Identification of the Paramagnetic Defects in a-SiCxNy Films with Different N Content

Magnetic Properties of the Carbon dangling Bonds in a-SiCxNy Films with High Nitrogen Content

CONCLUSIONS

Consent for Publication

CONFLICT OF INTEREST

ACKNOWLEDGEMENT

REFERENCES

Frontiers in Magnetic Resonance

(Volume 1)

Electron Paramagnetic Resonance in Modern

Carbon-Based Nanomaterials

Edited by

Dariya Savchenko

Department of Analysis of Functional Materials, Division of Optics,

Institute of Physics CAS, Prague, Czech Republic

Department of Physics and Solid State Physics,

National Technical University of Ukraine,

“Igor Sikorsky Kyiv Polytechnic Ins titute”, Kyiv,

Ukraine

Abdel Hadi Kassiba

Institute of Molecules and Materials, UMR-CNRS,

&

Le Mans University, Le Mans,

France

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FOREWORD

Carbon based materials include nanographites, conducting carbon nanomaterials, carbon nanotubes, graphene oxides, nanodiamonds, hybrids like carbon nanotubes embedded into polymer composites or functionalized molecular groups. These compounds are being implemented in multiple architectures with versatile chemical bonding, organization and morphologies leading to the unique physical properties such as exceptional electrical, thermal, structural dependent dimensionalities, mechanical and tribological performances. For instance, pure diamond is an excellent electrical insulator while some graphite based materials are more or less good electrical conductors, depending on their composition and pre-treatment. Carbon and graphite foams are very good thermal insulators, even at very high temperatures. On the other hand, diamond is used for the heat sink in electronics due to its very high thermal conductivity. Mechanical properties of carbon materials also differ considerably, depending on the type of the material. Since carbon allotropes and hybrids materials may contain different chemical bonding, multi-functional compounds can be tailored for various applications in nanoelectronics, integrated optoelectronics, energy storage and conversion, sensors, biomedicine, etc., being both already implemented in working devices and currently under development.

Intrinsic electronic features originating from doping or structural defects critically contribute to physical properties of carbon-based materials. These features may be exhaustively characterized by various electron magnetic resonance techniques including continuous wave (CW) or pulse electron paramagnetic resonance (EPR), electron nuclear double resonance (ENDOR) and other advanced electron magnetic resonance methods. Using a variety of complementary EPR techniques provides detailed insight into the local environment and the electronic peculiarity of defect structures in carbon-based systems. Moreover, extraordinary sensitivity of EPR techniques to the relaxation times (both spin-lattice and spin-spin) of paramagnetic species as well as the capability of selective control and detection of defects paves the way for the understanding of spin dynamics, which is extremely important in quantum computation or implementations of non-volatile memory devices. Thus, EPR techniques, based on different instrumental functionalities and methodologies, due to their specific window of time scales allow probing structural and electronic features of intrinsic and engineered spin systems in carbon based materials with the aim to open new challenges toward advanced and emerging technologies.

Dr. Alexander I. Shames Laboratory of Magnetic Resonance, Department of Physics Faculty of Natural Sciences Ben-Gurion University of the Negev Be’er-Sheva

PREFACE

The Volume 1 of Frontiers in Magnetic Resonance comprises 13 chapters on topics of high importance in the field of electron paramagnetic resonance study of carbon-containing nanomaterials. The topics and authors were selected from recently published papers in highly cited journals (Nat. Commun., Sci. Rep., J. Mater. Chem. C, Phys. Chem. Chem. Phys., Phys. Rev. B, Appl. Phys. Lett., J. Appl. Phys., Chem. Phys. Lett., Phys. Status Solidi B, Appl. Magn. Reson., etc.).

The first chapter by Prof. S.K. Misra will give the reader the fundamentals of EPR spectroscopy in regards to its application to the carbon-containing materials. The focus of chapter 2 by Dr. A. Barbon et al. is set to the resolution of the EPR signals attributable to different species, or structures, that are present in graphite and graphene-like materials. Chapter 3 by Prof. L. Forró et al., presents the ESR characterization of spin dynamics of conducting carbon nanomaterials. In chapter 4, by Dr. V. Likodimos et al., the EPR spectroscopy is exploited to investigate spin dynamics of DWCNTs and composites of oxidized MWCNTs embedded in an elastomeric poly(ether-ester) block copolymer. Chapter 5 by Dr. rer. nat. E. Erdem et al., focuses on discussing EPR investigations on graphene oxide, reduced graphene oxide, and carbon nanotubes with different chemical functionalities. In Chapter 6, Dr. K. Marumoto reviews the ESR spectroscopy of semiconducting single-walled CNT thin films and their transistors. Chapter 7 by Dr. S. Ruthstein et al. describes the findings on the oxygenation processes of coal and graphene materials using in-situ EPR experiments at various atmospheric environments. In Chapter 8, Prof. A.B. Więckowski et al. describe the application of the two-temperature EPR measurement method to carbonaceous solids. In Chapter 9, Prof. P. Baranov et al. review the characterization of impurities in nanodiamonds by means of multifrequency CW and pulse EPR techniques. Chapter 10 by Dr.Sc. S. Andronenko et al. shows the application of multifrequency EPR to the study of SiCN nanoceramics. In Chapter 11, Prof. A. Kassiba et al. discuss the study of paramagnetic centers in SiC nanomaterials by means of CW and pulse EPR techniques. In Chapter 12, Dr. D. Savchenko reviews the size effects observed in EPR and ENDOR spectra of SiC nanoparticles and nanodiamonds. Finally, in Chapter 13, DrSc. E. Kalabukhova et al. review the EPR study of paramagnetic defects in amorphous a-Si1-xCx:H and a-SiCxNy thin films.

We would like to express our gratitude to all the authors for their excellent contributions. We would also like to thank the entire team of Bentham Science Publishers, particularly Mr. Shehzad Naqvi (Senior Manager Publication) and Dr. Faryal Sami (Assistant Manager Publications), for their excellent efforts. We are confident that this volume will receive wide appreciation from students and researchers.

Dr. Dariya Savchenko Department of Analysis of Functional Materials, Division of Optics, Institute of Physics CAS, Prague Czech Republic Department of Physics and Solid State Physics, National Technical University of Ukraine “Igor Sikorsky Kyiv Polytechnic Institute”, Kyiv UkraineProf. Abdel Hadi Kassiba Institute of Molecules and Materials, UMR-CNRS, Le Mans University, Le Mans France

List of Contributors

Abdel Hadi KassibaInstitute of Molecules and Materials, UMR-CNRS, Le Mans University, 72085 Le Mans, FranceAndrzej B. WięckowskiInstitute of Physics, Faculty of Physics and Astronomy, University of Zielona Góra, Szafrana 4a, 65-516 Zielona Góra, Poland Institute of Molecular Physics of the Polish Academy of Sciences, Smoluchowskiego 17, 60-179 Poznań, PolandAndreas PöpplInstitute of Experimental Physics II, Faculty of Physics and Earth Sciences, Leipzig University, Leipzig, 04103, GermanyΑngeliki DiamantopoulouSection of Solid State Physics, Department of Physics, National and Kapodistrian University of Athens, Panepistimiopolis, 15 784, GreeceAnna SzymczykInstitute of Physics, West Pomeranian University of Technology, Al. Piastow 48, 70-311 Szczecin, PolandAntonio BarbonDepartment of Chemical Sciences, University of Padova, Padova, ItalyBálint NáfrádiLaboratory of Physics of Complex Matter (LPMC), Ecole Polytechnique Fédérale de Lausanne, CH-1015 Lausanne, SwitzerlandChuyen V. PhamLaboratory for MEMS Applications, Department of Microsystems Engineering - IMTEK, University of Freiburg, Georges-Koehler-Allee 103, D79110 Freiburg, GermanyDariya SavchenkoDepartment of Analysis of Functional Materials, Division of Optics, Institute of Physics of the Czech Academy of Sciences, Prague, 182 00, Czech Republic Department of Physics and Solid State Physics, National Technical University of Ukraine “Igor Sikorsky Kyiv Polytechnic Institute”, Kyiv, 03056, UkraineEmre ErdemInstitute of Physical Chemistry, University of Freiburg, Albertstr. 21, 79104 Freiburg, GermanyFrancesco TampieriDepartment of Chemical Sciences, , University of Padova, Padova, ItalyGeorge MaminDepartment of Quantum electronics and radiospectroscopy, Kazan Federal University, Kazan, 420000, Russian FederationGrzegorz P. SłowikInstitute of Physics, Faculty of Physics and Astronomy, University of Zielona Góra, Szafrana 4a, 65-516 Zielona Góra, PolandGrzegorz ZolnierkiewiczInstitute of Physics, West Pomeranian University of Technology, Al. Piastow 48, 70-311 Szczecin, PolandKazuhiro MarumotoDivision of Materials Science, University of Tsukuba, Tsukuba, Ibaraki 305-8573, Japan Tsukuba Research Center for Interdisciplinary Materials Science (TIMS), University of Tsukuba, Tsukuba, Ibaraki 305-8571, JapanMohammad ChoucairSchool of Chemistry, University of Sydney, Sydney, New South Wales 2006, AustraliaMichael KruegerCarl-von-Ossietzky University Oldenburg, Institute of Physics, Carl-von- Ossietzky Str. 9-11, D-26129 Oldenburg, GermanyNikolaos GuskosInstitute of Physics, West Pomeranian University of Technology, Al. Piastow 48, 70-311 Szczecin, PolandOrtal MarcianoBar-Ilan University, Faculty of Exact Sciences, Department of Chemistry, 5290002, Ramat Gan, IsraelPavel BaranovMicrowave Spectroscopy of Crystals Laboratory, Ioffe Institute, RAS, St Petersburg, 194021, Russian FederationSergey I. AndronenkoDepartment of Physics, Concordia University, Montreal, Canada, H3G 1M8 Institute of Physics, Kazan Federal University, Kazan, 420008, Russian FederationSergej ReppInstitute of Physical Chemistry, University of Freiburg, Albertstr. 21, 79104 Freiburg, GermanySergei OrlinskiiDepartment of Quantum electronics and radiospectroscopy, Kazan Federal University, Kazan, 420000, Russian FederationSharon RuthsteinBar-Ilan University, Faculty of Exact Sciences, Department of Chemistry, 5290002, Ramat Gan, IsraelSpyridon GlenisSection of Solid State Physics, Department of Physics, National and Kapodistrian University of Athens, Panepistimiopolis, 15 784, GreeceSushil K. MisraDepartment of Physics, Concordia University, Montreal, H3G 1M8, CanadaVlassis LikodimosSection of Solid State Physics, Department of Physics, National and Kapodistrian University of Athens, Panepistimiopolis, 15 784, GreeceViktor SoltamovMicrowave Spectroscopy of Crystals Laboratory, Ioffe Institute, RAS, St Petersburg, 194021, Russian Federation Department of Quantum electronics and radiospectroscopy, Kazan Federal University, Kazan, 420000, Russian Federation

Fundamentals of Electron Paramagnetic Resonance in Modern Carbon-based Materials

Sushil K. Misra*

Department of Physics, Concordia University, Montreal, H3G 1M8, Canada

Abstract

The advantages of using multifrequency Electron Paramagnetic Resonance (EPR) in studying carbon-based materials are discussed. The details of designing continuous-wave EPR spectrometers operating at different frequencies are presented. Designs of CW and pulse Electron Nuclear Double Resonance (ENDOR) spectrometers, which are very important techniques for studying precisely hyperfine interactions and local environment of paramagnetic ions in carbon-based materials are included. Analysis of EPR spectra, spin Hamiltonians, EPR lineshapes, evaluation of spin-Hamiltonian parameters, and simulation of single-crystal and powder spectra are also explained. A short review of carbon-based materials studied by EPR is given.

Keywords: Carbon-based materials, Continuous Wave EPR, Davies ENDOR, Electron spin echo (ESE), Electron Spin Echo Envelope Modulation (ESEEM), Evaluation of spin Hamiltonian parameters, Electron Nuclear Double Resonance (ENDOR), EPR, EPR lineshape, EPR spectrometer, High-frequency spectrometers, Hyperfine interaction, Hyperfine Sublevel Correlation Spectroscopy (HYSCORE), Mims ENDOR, Pulse EPR, Pulse ENDOR, Simulation of EPR spectrum, Spin Hamiltonian, Zeeman effect.

*Corresponding author Sushil K. Misra: Department of Physics, Concordia University, Montreal, H3G 1M8, Canada ; Tel: [phone]; E-mail: [email protected]