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Particulate-Filled Polymer Composites, 2nd Edition by ed. Roger N. Rothon

This text provides a comprehensive guide to the main types of particulate-filled polymers. It covers their characteristics, the rules governing their use, methods of incorporation and the effects of surface treatment.

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This is the second edition of this book. This book brings together many scientific and technical disciplines, including mineralogy, crystallography, precipitation, powder technology, materials science and many more. All the chapters have been updated for this book and there is the addition of an extra one on Composites using Nanofillers. This book is a fundamental guide to the subject and will be of interest to filler producers, machinery manufacturers, polymer compounders and suppliers of processing aids and surface modifiers.

Contents

Preface

Contributors

1 General Principles Guiding Selection and Use of Particulate Materials

1.1 Introduction

1.2 Basic Characteristics of Particulate Fillers

1.2.1 Cost

1.2.2 Chemistry, Composition and Impurities

1.2.3 Density or Specific Gravity

1.2.4 Hardness

1.2.5 Abrasiveness

1.2.6 Optical Properties

1.2.7 Thermal Properties

1.2.8 Particle Shape and Size

1.2.9 Shape

1.2.10 Particle Size

1.3 Surface Modification

1.3.1 Stearic Acid and Stearates

1.3.2 Coupling Agents

1.3.3 Polymer Modifications

1.3.4 Direct Bonding

1.4 Particle Packing and the Maximum Packing Fraction

1.4.1 Introduction

1.4.2 Determination of Maximum Packing Fraction (Pf) by Oil Absorption Procedures

1.4.3 Particle Packing Theory

1.4.4 Applications of Packing Principles to Particulate Filled Composites

1.5 Interparticle Spacing

1.6 Particle Effects on the Structure of Polymers.

1.6.1 Introduction

1.6.2 Molecular Weight Reduction During Processing

1.6.3 Molecular Weight and Crosslinking Changes due to Cure Modifications

1.6.4 Preferential Adsorption of Polar Species

1.6.5 Formation of an Interphase of Immobilised Polymer

1.6.6 Effects on Polymer Conformation due to the Presence of Particle Surfaces and Interparticle Spacing

1.6.7 Effects on Crystallinity

References

2 Principal Types of Particulate Fillers

2.1 Introduction

2.2 Particulate Fillers from Natural Origins (Mineral Fillers)

2.2.1 Introduction

2.2.2 Minerals and Rocks

2.2.3 Rocks

2.2.4 Calcium Carbonate Minerals

2.2.5 Dolomite

2.2.6 China Clay or Kaolin

2.2.7 Calcined Clay

2.2.8 Mica

2.2.9 Talc

2.2.10 Montmorillonite (AlMg)8(Si4O10)3-(OH)10.12H2O

2.2.11 Barite (BaSO4).

2.2.12 Calcium Sulfate Products

2.2.13 Wollastonite (CaSiO3)

2.2.14 Crystalline Silicas

2.3 Synthetic Particulate Fillers

2.3.1 Carbon Black

2.3.2 Synthetic Silicas

2.3.3 Hydroxides and Basic Carbonates

2.3.4 Precipitated Calcium Carbonate (PCC).

Acknowledgements

References

3 Analytical Techniques for Characterising Filler Surfaces

3.1 Introduction

3.2 Acid-Base Theory

3.2.1 Introduction

3.2.2 Gutmann Approach

3.2.3 Drago Approach

3.2.4 Use in Characterising Fillers

3.3 Analytical Techniques

3.4 Reactive Techniques

3.4.1 Flow Microcalorimetry

3.4.2 Inverse Gas Chromatography

3.5 Spectroscopic Techniques

3.5.1 Introduction

3.5.2 X-Ray Photoelectron Spectroscopy

3.5.3 Secondary Ion Mass Spectrometry

3.5.4 Diffuse Reflectance Fourier Transform Infrared Spectroscopy

3.6 Methods for Examining Structural Order in Filler Coatings

3.6.1 Wide Angle X-Ray Diffraction

3.6.2 Differential Scanning Calorimetry

3.7 Summary

References

4 Surface Modification and Surface Modifiers

4.1 Introduction

4.2 Reasons for Using Surface Modifiers

4.3 General Principles of Surface Modification

4.4 Methods of Using Surface Modifiers

4.5 Choice of Coating Level

4.6 Techniques for Determining the Amount of Coating Present, and Assessing the Amount Needed for Mono-layer Coverage

4.6.1 Determination of Amount of Additive and it’s Distribution

4.6.2 The Monolayer and it’s Determination

4.6.3 Effects of Processing on the Coating Structure

4.7 Surface Modifier Types

4.7.1 Monomeric Organic Acids and their Salts

4.7.2 Stearic Acid (CH3(CH2)16COOH

4.7.3 Other Saturated Fatty Acids and Related Substances

4.7.4 Effects of Stearic Acid Coating in Composites

4.7.5 Fatty Acid Salts

4.7.6 Unsaturated and other Functional Organic Acids in Composites

4.7.7 Polymeric Acids and Anhydrides

4.7.8 Organo-silicon Compounds

4.7.9 Examples of Silane Coupling Agent Effects in

Filled Polymers

4.7.10 Organo-Titanates and Zirconates

4.7.11 Aluminates and Zircoaluminates

4.7.12 Phosphates and Borates

4.7.13 Organic Amines and Amino-acids

4.8 Conclusions

References

5 Compound Preparation, Mixture Characterisation and Process Enhancement of Particulate-Filled Polymer Compounds

5.1 Introduction

5.2 Functional Characteristics of Compounding Machinery

5.2.1 Transport of Feedstock

5.2.2 Melting and Shear Heating

5.2.3 Mixing

5.2.4 Melt Devolatilisation

5.2.5 Melt Pumping and Pressurisation

5.3 Constructional Design of Compounding Plant

5.3.1 Low and Medium Intensity Premixing Procedures

5.3.2 High-Intensity Compounding Machinery

5.4 Characterisation of Filled Compounds

5.4.1 Introduction

5.4.2 Residence Time Distribution

5.4.3 Specific Energy Input

5.4.4 Screen Pack Analysis

5.4.5 Rheological Analysis

5.4.6 Ultrasonic Measurement

5.4.7 Microstructural Analysis.

5.4.8 Miscellaneous Methods of Analysis

5.5 Process Enhancement of Particulate Polymer Composites

5.5.1 Addition of Rigid Particulate Fillers

5.5.2 Effects on Polymer Molecular Weight

5.5.3 Short Fibre-Reinforced Thermoplastics Composites

5.6 Woodflour and Natural Fibre-Filled Thermoplastics

5.7 Supercritical Fluid Assisted Processing of Filled Compounds

5.8 Processing of Thermoset Recyclate Waste Materials

5.9 Preparation of Silicate Layer Polymer Nanocomposites

5.10 Conclusions

References

6 Effects of Particulate Fillers on Flame Retardant Properties of Composites

6.1 Introduction

6.2 General Effects of Fillers on Polymer Flammability

6.3 Fire Retardant Testing.

6.3.1 Oxygen Index Test (ASTM D2863-87)

6.3.2 Underwriters Laboratory Vertical Burn Test (UL94 -1980)

6.3.3 Horizontal Burn Test (ASTM D635-88)

6.3.4 Ignitability Test (ISO5657 1986)

6.3.5 Cone Calorimeter (ASTM E1354, ISO 5660)

6.3.6 Smoke and Corrosive Gas Tests

6.4 Fire Retardant Fillers that Rely on Endothermic Decomposition

6.4.1 Historical Background

6.4.2 Potential Endothermic Flame Retardant Fillers

6.4.3 Performance of Endothermic Flame Retardant Fillers

6.4.4 Smoke and Corrosive and Toxic Gases

6.5 Nano-Clays

6.6 Ammonium Polyphosphate (APP)

6.7 Fillers for Use in Conjunction with Halogens

References

7 Particulate Fillers in Elastomers

7.1 Introduction

7.2 Uses of Elastomers

7.3 Elasticity of Rubber

7.4 Formulation of Elastomers

7.4.1 General

7.4.2 Selection of Polymer

7.4.3 The Curing System

7.4.4 Antioxidants and Antiozonants

7.4.5 Coupling Agents

7.4.6 Process Oils and Plasticisers

7.4.7 Fillers

7.4.8 Specialty Additives

7.5 The Performance of the Polymer

7.5.1 Specification of the Polymer

7.5.2 Processing Considerations

7.5.3 Strength Characteristics of Polymers

7.5.4 Compounding Considerations

7.6 The Performance of Fillers

7.6.1 Reinforcement of Rubber by Fillers

7.6.2 Processing Considerations

7.6.3 Compounding Considerations

7.7 Filler Types

7.7.1 Specification of Fillers for Elastomers

7.7.2 Carbon Black

7.7.3 Synthetic Silicas and Silicates

7.7.4 Clay Minerals

7.7.5 Calcium Carbonates

7.7.6 Alumina Trihydrate

7.7.7 Talcs

7.7.8 Natural Silicas

7.7.9 Barytes and Blanc Fixe

7.7.10 Miscellaneous

Acknowledgements

References

8 Filled Thermoplastics

8.1 Introduction

8.1.1 Thermoplastics and Typical Applications

8.1.2 Thermoplastic Composites

8.2 Bulk and Process Related Properties

8.2.1 Specific Gravity or Relative Density

8.2.2 Acoustic Properties

8.2.3 Melt Viscosity (MFI)

8.2.4 Compounding and Extrusion

8.2.5 Thermal Conductivity and Specific Heat Capacity

8.2.6 Thermal Expansion.

8.2.7 Electrical Properties

8.2.8 Barrier Properties

8.3 Mechanical Properties

8.3.1 Introduction

8.3.2 Modulus – Tensile and Flexural

8.3.3 Heat Deflection Temperature (HDT)

8.3.4 Yield Strength

8.3.5 Impact Strength (Toughness)

8.4 Effects of Filler on the Polymer Phase

8.4.1 Introduction

8.4.2 Nucleation

8.4.3 Transcrystallinity

8.4.4 Interphase

8.5 Surface Science Aspects

8.5.1 Introduction

8.5.2 Surface Energy and Surface Tension

8.5.3 Wetting and Spreading

8.5.4 Adhesion

8.5.5 Dispersion and Agglomeration

8.5.6 Surface Treatments – Dispersants and Coupling Agents

8.6 Aesthetics

8.6.1 Introduction

8.6.2 Colour/Pigmentation.

8.6.3 Surface Finish and Gloss

8.6.4 Scratch and Abrasion Resistance

8.7 Stabilisation and Recycleability

8.7.1 Introduction

8.7.2 The Effect of Filler Chemistry and Impurities on Stability

8.7.3 The Effect of Antioxidant Adsorption on Stability

8.7.4 Recycleability

8.8 Uses of Filled Thermoplastics

8.8.1 Uses of Fillers

8.8.2 Fillers in PVC

8.8.2 Uses of Fillers in Unplasticised PVC

8.8.3 Uses of Fillers in Polypropylene

8.8.4 Uses of Fillers in Polyethylene

8.8.5 The Use of Fillers in Polyamides

8.8.6 Polybutylene Terephthalate

8.8.7 Polyethylene Terephthalate

8.9 Conclusions

Acknowledgements

References

9 Filled Thermosets

9.1 Introduction

9.2 Brief Chemistry of Thermoset Polymers

9.2.1 Free-Radical Chain-Growth Curing Resins

9.2.2 Step Addition Curing Resins

9.2.3 Condensation Resins.

9.3 Mechanical Properties

9.3.1 Modulus

9.3.2 Fracture Toughness and Fracture Energy

9.3.3 Failure Stress

9.3.4 Fatigue

9.4 Applications

9.4.1 Cost Reduction

9.4.2 Modified Mechanical Properties

9.4.3 Exotherm Control.

9.4.4 Shrinkage Control.

9.4.5 Processing Aids

9.4.6 Flame Retardants

9.4.7 Metal Fillers

9.4.8 Structural Adhesives

Acknowledgements

References

10 Composites Using Nano-Fillers

10.1 Introduction

10.2 Scope

10.3 General Comments

10.4 Nano-Filler Forms

10.4.1 Regular Shapes

10.4.2 Rods, Fibres, etc.

10.4.3 Platy Nano-Fillers (Nano-Clays and Related Materials)

10.5 Summary and Future Perspectives

Acknowledgements

References

Abbreviations and Acronyms

Author Index

Index

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