Polymer Microscopy. Second edition LINDA C. SAWYER. and. DAVID T. GRUBB Cornell University Ithaca, NY USA. Hoechst Celanese Corporation Summit, NJ USA

Transcription

1 Polymer Microscopy Second edition LINDA C. SAWYER Hoechst Celanese Corporation Summit, NJ USA and DAVID T. GRUBB Cornell University Ithaca, NY USA CHAPMAN & HALL London Glasgow Weinheim New York Tokyo Melbourne Madras

2 Color plates appear between pages 274 and 275 Preface to the second edition Acknowledgements xi xiii 1 Introduction to polymer morphology Polymer materials Introduction Definitions Polymer morphology Amorphous polymers Semicrystalline polymers Liquid crystalline polymers Polymer processes Extrusion of fibers and films Extrusion and molding Polymer characterization General techniques Microscopy techniques Specimen preparation methods Applications of microscopy to polymers New microscopy techniques 14 2 Fundamentals of microscopy Introduction Lens-imaging microscopes Scanning-imaging microscopes Optical microscopy (OM) Introduction, Objective lenses :;. *> Imaging modes, 22

3 vi Contents Measurement of refractive index Polarized light Scanning electron microscopy (SEM) Introduction Imaging signals SEM optimization Special SEM types Transmission electron microscopy (TEM) Imaging in the TEM Diffraction techniques Phase contrast and lattice imaging Scanning probe microscopy (SPM) Microscopy of radiation sensitive materials SEM operation Low dose TEM operation Analytical microscopy X-ray microanalysis X-ray analysis in the SEM vs. AEM Elemental mapping Quantitative microscopy Stereology and image analysis Calibration Image processing Dynamic microscopy Stages for dynamic microscopy 43 3 Imaging theory Imaging with lenses., Basic optics Resolution Electron diffraction Contrast mechanisms Illumination systems Imaging by scanning electron beam Scanning optics Beam - specimen interactions Image formation Imaging by scanning a solid probe Polarizing microscopy Polarized light Anisotropic materials Polarizing microscopy Radiation effects Effect of radiation on polymers Radiation doses and specimen heating Effects of radiation damage on the image 74

4 vii Noise limited resolution Image processing 78 4 Specimen preparation methods Simple preparation methods Optical preparations SEM preparations TEM preparations SPM preparations Polishing Polishing artifacts Polishing specimen surfaces Microtomy Peelback of fibers/films for SEM Sections for OM Sections for SEM Ultrathin sectioning Ultrathin cryosectioning Staining * Introduction Osmium tetroxide Ebonite Chlorosulfonic acid Phosphotungstic acid Ruthenium tetroxide Silver sulfide Mercuric trifluoroacetate Iodine Summary Etching Introduction Plasma and ion etching Solvent and chemical etching Acid etching Summary Replication Simple replicas Replication for TEM Conductive coatings Coating devices Coatings for TEM Coatings for SEM and STM Artifacts Gold decoration Yielding and fracture Fractography 147

5 viii Contents Fracture: standard physical testing In situ deformation Crazing Freezing and drying methods Simple freezing methods Freeze drying Critical point drying Freeze fracture-etching Polymer applications Fibers Introduction Textile fibers Problem solving applications Industrial fibers Films and membranes Introduction Model studies Industrial films Hat film membranes Hollow fiber membranes Engineering resins and plastics Introduction Extrudates and molded parts Multiphase polymers Failure analysis Composites ; Introduction Composite characterization Fiber composites Particle filled composites Carbon black filled rubber Emulsions and adhesives Introduction Latexes Wettability Adhesives and adhesion Liquid crystalline polymers Introduction Optical textures Solid state structures High modulus fibers Structure-property relations in LCPs 293

6 ix 6 New techniques in polymer microscopy Introduction Optical microscopy Confocal scanning microscopy Near field optical microscopy Scanning electron microscopy (SEM) Low voltage SEM High resolution SEM High pressure (environmental) SEM Transmission electron microscopy (TEM) High resolution TEM Structure determination by electron diffraction Scanning tunneling microscopy (STM) Principles of STM Instrumentation and operation of the STM STM of insulators Adsorbed organic molecules Other polymer applications Scanning "force microscopy (SFM) Principles of atomic force microscopy (AFM) Atomic resolution in the AFM Metrology using scanning probe microscopy Frictional force microscopy Problem solving summary Where to start Problem solving protocol Polymer structures \ Instrumental techniques Comparison of techniques Optical techniques SEM techniques TEM techniques SPM techniques Technique selection Interpretation Artifacts Summary Supporting characterizations X-ray diffraction Thermal analysis Spectroscopy Small angle scattering Summary 375

7 Appendices 379 Appendix I Abbreviations of polymer names 379 Appendix II List of acronyms - techniques 380 Appendix III Manmade polymer fibres 381 Appendix IV Common commercial polymers and tradenames for plastics, films and engineering resins 382 Appendix V General suppliers of microscopy accessories 384 Appendix VI Suppliers of optical and electron microscopes 385 Appendix VII Suppliers of x-ray microanalysis equipment 385 Appendix VIII Suppliers of scanning probe microscopes 386 Index 387