Characterization Techniques for Polymer Nanocomposites -- Contents -- Preface -- List of Contributors -- 1: Characterization of Nanocomposite Materials: An Overview -- 1.1 Introduction -- 1.2 Characterization of Morphology and Properties -- 1.3 Examples of Characterization Techniques -- References -- 2: Thermal Characterization of Fillers and Polymer Nanocomposites -- 2.1 Introduction -- 2.2 TGA of Fillers -- 2.2.1 Quantification of the Extent of Surface Modification -- 2.2.2 Cleanliness of the Filler Surface -- 2.2.3 Comparing the Stability of Different Fillers -- 2.2.4 Dynamic TGA Analysis of the Fillers -- 2.2.5 Characterization of the Surface Reactions -- 2.2.6 Different Measurement Environments -- 2.2.7 Correlation of Organic Matter with Basal Spacing -- 2.3 TGA of Polymer Nanocomposites -- 2.3.1 Effect of Filler Concentration -- 2.3.2 Effect of Compatibilizer -- 2.4 DSC of Fillers -- 2.4.1 Thermal Transitions in the Modified Fillers -- 2.5 DSC of Composites -- 2.5.1 Transitions in Composites -- 2.5.2 Optimization of Curing Conditions -- References -- 3: Flame-Retardancy Characterization of Polymer Nanocomposites -- 3.1 Introduction -- 3.2 Types of Flame-Retardant Nanoadditives -- 3.2.1 One-Dimensional Nanomaterials -- 3.2.1.1 Montmorillonite Clay -- 3.2.1.2 Nanographene Platelets -- 3.2.2 Two-Dimensional Nanomaterials -- 3.2.2.1 Carbon Nanofibers -- 3.2.2.2 Carbon Nanotubes -- 3.2.2.3 Halloysite Nanotubes -- 3.2.3 Three-Dimensional Nanomaterials -- 3.2.3.1 Nanosilica -- 3.2.3.2 Nanoalumina -- 3.2.3.3 Nanomagnesium Hydroxide -- 3.2.3.4 Polyhedral Oligomeric Silsequioxanes -- 3.3 Thermal, Flammability, and Smoke Characterization Techniques -- 3.3.1 Introduction to Test Methods -- 3.3.2 Thermogravimetric Analysis (TGA) -- 3.3.3 The UL 94 Vertical Flame Test -- 3.3.4 Oxygen Index (Limiting Oxygen Index) (ASTM D2863-97).

3.3.5 Cone Calorimeter (ASTM E 1354) -- 3.3.6 Microscale Combustion Calorimeter (ASTM D 7309) -- 3.3.7 Steiner Tunnel Test (ASTM E 84) -- 3.4 Thermal and Flame Retardancy of Polymer Nanocomposites -- 3.4.1 One-Dimensional Nanomaterial-Based Nanocomposites -- 3.4.1.1 Polymer-Clay Nanocomposites -- 3.4.1.2 Polymer-Graphene Nanocomposites -- 3.4.2 Two-Dimensional Nanomaterial-Based Nanocomposites -- 3.4.2.1 Polymer Carbon Nanofiber Nanocomposites -- 3.4.2.2 Polymer Carbon Nanotube Nanocomposites -- 3.4.2.3 Polymer Halloysite Nanotube Nanocomposites -- 3.4.3 Three-Dimensional Nanomaterial-Based Nanocomposites -- 3.4.3.1 Polymer Nanosilica Nanocomposites -- 3.4.3.2 Polymer Nanoalumina Nanocomposites -- 3.4.3.3 Polymer Nanomagnesium Hydroxide Nanocomposites -- 3.4.3.4 Polymer POSS Nanocomposites -- 3.4.4 Multicomponent FR Systems: Polymer Nanocomposites Combined with Additional Materials -- 3.4.4.1 Polymer-Clay with Conventional FR Additive Nanocomposites -- 3.4.4.2 Polymer-Carbon Nanotubes with Conventional FR Additive Nanocomposites -- 3.4.4.3 Polymer-Clay and -Carbon Nanotubes with Conventional FR Additive Nanocomposites -- 3.5 Flame Retardant Mechanisms of Polymer Nanocomposites -- 3.6 Concluding Remarks and Trends of Polymer Nanocomposites -- Acknowledgments -- References -- 4: PVT Characterization of Polymeric Nanocomposites -- 4.1 Introduction -- 4.2 Components of Polymeric Nanocomposites -- 4.2.1 Size, Size Distribution, and Shape of the Clay Platelets -- 4.2.2 Chemical Composition of Clays -- 4.2.3 Impurities -- 4.3 Pressure-Volume-Temperature (PVT) Measurements -- 4.3.1 Transitions -- 4.3.2 Determination of PVT -- 4.3.3 Effects of Clay, Intercalant, and Compatibilizer -- 4.4 Derivatives, Compressibility, and Thermal Expansion Coefficient -- 4.4.1 Interpolating the Data.

4.4.2 Computation of the Thermal Expansion and Compressibility Coefficients, α and κ -- 4.4.3 Polymer α and κ from PVT -- 4.4.4 Effect of Clay on α and κ in PS-Based PNC -- 4.4.5 Effect of Clay on α and κ in PA-6 Based PNC -- 4.5 Thermodynamic Theories -- 4.5.1 Simha-Somcynsky Cell-Hole Theory -- 4.5.2 Simha-Somcynsky eos for Multicomponent Systems -- 4.5.3 The Vitreous Region -- 4.5.4 Equation of State for Semicrystalline PNC -- 4.6 Thermodynamic Interaction Coefficients -- 4.7 Theoretical Predictions -- 4.8 Summary and Conclusions -- 4.8.1 Characterization of Clays -- 4.8.2 PVT Measurements -- 4.8.3 Derivative Properties -- 4.8.4 Thermodynamic Theories -- 4.8.5 Interaction Parameters -- 4.8.6 Theoretical Predictions -- References -- 5: Following the Nanocomposites Synthesis by Raman Spectroscopy and X-Ray Photoelectron Spectroscopy (XPS) -- 5.1 Nanocomposites Based on POSS and Polymer Matrix -- 5.1.1 Introduction -- 5.1.2 Raman Spectroscopy Applied for Following the Synthesis of Nanocomposites Based on Polymer Matrix and POSS -- 5.1.3 XPS Applied for Characterization of Polymer-POSS Nanocomposites -- 5.1.3.1 Analysis of Functionalized POSS Molecules -- 5.1.3.2 Characterization of Nanocomposite Materials -- 5.1.4 Conclusions -- 5.2 Raman and XPS Applied in Synthesis of Nanocomposites Based on Carbon Nanotubes and Polymers -- 5.2.1 Introduction -- 5.2.2 X-Ray Photoelectron Spectroscopy (XPS) Used to Monitorize the Synthesis of Polymer-CNT-Based Nanocomposites -- 5.2.2.1 CNT Functionalization with Carboxylic Groups -- 5.2.2.2 CNT Functionalization with Amines -- 5.2.2.3 CNT Functionalization with Bioconjugated Systems Based on Dendritic Polymers and Antitumoral Drug -- 5.2.3 Polymer-CNT-Based Nanocomposites Synthesis Followed by Raman Spectroscopy -- 5.2.4 Conclusions -- Acknowledgments -- References.

6: Tribological Characterization of Polymer Nanocomposites -- 6.1 Introduction -- 6.2 Tribological Fundamentals -- 6.2.1 Tribological System -- 6.2.2 Wear Mechanisms -- 6.2.3 Transfer Film Formation -- 6.2.4 Temperature Increase -- 6.3 Wear Experiments -- 6.3.1 Selected Wear Models -- 6.3.2 Characteristic Values of Tribological Systems -- 6.3.2.1 Wear Rate -- 6.4 Selection Criteria -- 6.5 Design of Polymer Nanocomposites and Multiscale Composites -- 6.6 Selected Experimental Results -- 6.6.1 Particulate Fillers -- 6.6.2 Short Fibers -- 6.6.3 Combination of Fillers -- 6.6.3.1 Internal Lubricants and Short Carbon Fibers -- 6.6.3.2 Short Carbon Fibers and Nanoparticles -- 6.6.4 Wear Mechanisms -- 6.6.4.1 Ball Bearing ("Rolling") Effect on a Submicro Scale -- 6.6.5 Summary -- References -- 7: Dielectric Relaxation Spectroscopy for Polymer Nanocomposites -- 7.1 Introduction -- 7.2 Theory of Dielectric Relaxation Spectroscopy -- 7.2.1 Dielectric Relaxations in Polymer Nanocomposites -- 7.2.2 Fitting to Experimental Data -- 7.2.3 Activation Energy of the Relaxation Process -- 7.2.4 Modulus Formalism -- 7.3 PVDF/Clay Nanocomposites -- 7.3.1 Frequency Dependence of Dielectric Permittivity -- 7.3.2 Vo-Shi Model Fitting to Dielectric Permittivity -- 7.3.3 Role of Interface -- 7.3.4 Frequency Dependence of Dielectric Relaxation Spectra -- 7.4 PVDF/BaTiO3 Nanocomposites -- 7.4.1 Frequency Dependence of Dielectric Relaxation Spectra -- 7.4.2 Electric Modulus Presentation of Dielectric Relaxation Spectra -- 7.4.3 Activation Energy of Crystalline and MWS Relaxation Processes -- 7.5 PVDF/Fe3O4 Nanocomposites -- 7.5.1 Low-Temperature Dielectric Relaxation Spectra -- 7.5.2 Activation Energy of Glass Transition Relaxation -- 7.5.3 Normalized Spectra of Dielectric Relaxation -- 7.6 Comparative Analysis of PVDF Nanocomposites -- 7.7 Conclusions -- Acknowledgment.

Nomenclature -- References -- 8: AFM Characterization of Polymer Nanocomposites -- 8.1 Atomic Force Microscope (AFM) -- 8.1.1 Principle of AFM -- 8.1.2 Principle of Tapping Mode AFM -- 8.1.3 Phase and Energy Dissipation -- 8.2 Elasticity Measured by AFM -- 8.2.1 Sample Deformation -- 8.2.2 Contact Mechanics -- 8.2.3 Sneddon's Elastic Contact -- 8.2.4 Nanopalpation Realized by AFM -- 8.2.5 Adhesive Contact -- 8.2.6 Nanomechanical Mapping -- 8.3 Example Studies -- 8.3.1 Carbon Nanotubes-Reinforced Elastomer Nanocomposites -- 8.3.2 Investigation of the Reactive Polymer-Polymer Interface -- 8.3.3 Nanomechanical Properties of Block Copolymers -- 8.4 Conclusion -- References -- 9: Electron Paramagnetic Resonance and Solid-State NMR Studies of the Surfactant Interphase in Polymer-Clay Nanocomposites -- 9.1 Introduction -- 9.2 NMR, EPR, and Spin Labeling Techniques -- 9.2.1 Solid-State NMR Spectroscopy -- 9.2.2 EPR Spectroscopy -- 9.2.3 Spin Label EPR -- 9.2.4 Spin Labeling of the Surfactant Interphase -- 9.3 Characterization of Organically Modified Layered Silicates -- 9.3.1 Heterogeneity of Organoclays -- 9.3.2 Heterogeneity and Position Dependence of Surfactant Dynamics -- 9.3.3 Further Features of Surfactant Dynamics -- 9.3.4 Structural Aspects of the Surfactant Layer -- 9.4 Characterization of Nanocomposites -- 9.4.1 Intercalated Nanocomposites and Nonintercalated Composites -- 9.4.2 Influence of the Polymer on Surfactant Dynamics -- 9.4.3 Influence of the Polymer on Surfactant Layer Structure -- 9.5: Conclusion -- Acknowledgments -- References -- 10: Characterization of Rheological Properties of Polymer Nanocomposites -- 10.1 Introduction -- 10.2 Fundamental Rheological Theory for Studying Polymer Nanocomposites -- 10.3 Characterization of Rheological Properties of Polymer Nanocomposites -- 10.4 Conclusions -- References.

11: Segmental Dynamics of Polymers in Polymer/Clay Nanocomposites Studied by Spin-Labeling ESR.