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Polymer Melt
Fracture
Polymer Melt
Fracture
Rudy Koopmans
Jaap den Doelder
Jaap Molenaar

Boca Raton London New York

CRC Press is an imprint of the

Taylor & Francis Group, an informa business
CRC Press
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Version Date: 20140514

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To our families and friends
 There is nothing stable in this world; uproar’s your only music.

John Keats
English poet (1795–1821)

Remember that there is nothing stable in human affairs; therefore

avoid undue elation in prosperity, or undue depression in adversity.

Socrates
Greek philosopher in Athens (469 BC–399 BC)
Contents
Foreword .................................................................................................................. xv
Preface....................................................................................................................xvii
Authors ....................................................................................................................xxi

Chapter 1 Polymer Melt Fracture Pictures............................................................ 1

1.1 Optical Microscopy ...................................................................2
1.2 Scanning Electron Microscopy ............................................... 10
Reference ............................................................................................20

Chapter 2 Polymer Characteristics ..................................................................... 21

2.1 Polymers .................................................................................. 22
2.1.1 Polymer Architecture .................................................24
2.1.2 Molar Mass Distribution ............................................28
2.1.3 Polymerization Processes ........................................... 32
2.2 Polymer Characterization ........................................................ 35
2.2.1 Polymer Architecture ................................................. 35
2.2.1.1 Spectrometry: Ultraviolet,
Visible, Infrared, and Raman ..................... 36
2.2.1.2 Nuclear Magnetic Resonance
Spectrometry............................................... 36
2.2.1.3 Density ........................................................ 39
2.2.1.4 Thermal Analysis ....................................... 39
2.2.2 Molar Mass, Molar Mass Distribution .......................40
2.2.2.1 Dilute Solution Viscosity ............................ 41
2.2.2.2 Light Scattering .......................................... 43
2.2.2.3 Colligative Property Measurement
Techniques ..................................................44
2.2.2.4 Gel Permeation Chromatography ............... 45
2.2.2.5 Fractionation ...............................................46
2.2.2.6 Rheology ..................................................... 47
2.3 General Observation ................................................................ 49
References .......................................................................................... 50

Chapter 3 Polymer Rheology .............................................................................. 53

3.1 Continuum Mechanics ............................................................. 53
3.2 Scalars, Vectors, and Tensors .................................................. 54
3.3 Stress Tensor ............................................................................ 58

ix
x Contents

3.4 Strain Tensors .......................................................................... 59

3.4.1 Finger Tensor .............................................................. 59
3.4.2 Rate of Deformation and Vorticity Tensor ................. 63
3.4.3 Relation between Finger Tensor B and Rate of
Deformation Tensor D ................................................ 65
3.5 Equations of Motion ................................................................ 65
3.5.1 Transport Theorem .....................................................66
3.5.2 Mass Balance.............................................................. 67
3.5.3 Momentum Balance ................................................... 68
3.6 Constitutive Equations ............................................................. 71
3.6.1 Elastic Behavior.......................................................... 71
3.6.2 Viscous Behavior........................................................ 72
3.6.3 Viscoelastic Behavior ................................................. 75
3.6.4 Linear Viscoelasticity................................................. 78
3.6.5 Compliance Function .................................................80
3.7 General Observation ................................................................84
References ..........................................................................................84

Chapter 4 Polymer Processing ............................................................................ 87

4.1 Extrusion ................................................................................. 87
4.1.1 Granulation ................................................................. 88
4.1.2 Film Blowing .............................................................. 88
4.1.3 Film and Sheet Casting .............................................. 93
4.1.4 Extrusion Blow Molding ............................................ 95
4.1.5 Wire Coating ..............................................................97
4.1.6 Pipe and Profile .......................................................... 98
4.1.7 Fiber Spinning ............................................................ 98
4.1.8 Co-Extrusion ............................................................ 101
4.2 Injection Molding .................................................................. 102
4.3 Rotational Molding ................................................................ 103
4.4 Calendering ........................................................................... 103
4.5 General Observation .............................................................. 104
References ........................................................................................ 105

Chapter 5 Melt Fracture Experiments............................................................... 109

5.1 Constant-Pressure and Constant-Rate Experiments .............. 110
5.1.1 Discontinuous Flow Curves ..................................... 114
5.1.2 Continuous Flow Curves .......................................... 120
5.2 Flow Visualization................................................................. 122
5.2.1 Particle Tracking ...................................................... 124
5.2.2 Flow Birefringence ................................................... 126
5.2.3 Stacked Colors .......................................................... 130
5.3 Critical Numbers ................................................................... 131
5.3.1 Reynolds Number ..................................................... 132
5.3.2 Weissenberg and Deborah Number .......................... 132
Contents xi

5.3.3 Recoverable Strain ................................................... 134

5.3.4 Critical Stress ........................................................... 135
5.4 Melt Fracture Observation ..................................................... 139
5.4.1 Microscopy ............................................................... 139
5.4.2 Profilometry.............................................................. 140
5.4.3 Indirect Methods ...................................................... 141
5.4.4 Melt Fracture Quantification .................................... 144
5.5 Change of Slope..................................................................... 147
5.6 Wall Slip ................................................................................ 148
5.6.1 The Mooney Method ................................................ 148
5.6.2 The Laun Method ..................................................... 151
5.6.3 Other Methods.......................................................... 153
5.7 Compressibility...................................................................... 154
5.8 General Observation .............................................................. 155
References ........................................................................................ 156

Chapter 6 Melt Fracture Variables .................................................................... 167

6.1 Polymer Architecture ............................................................ 167
6.2 Polymer-Processing Variables ............................................... 174
6.2.1 Length–Radius Ratio ............................................... 174
6.2.2 Die Entry and Exit Angle ......................................... 179
6.2.3 Die Construction Material........................................ 182
6.2.4 Die Surface Roughness ............................................ 184
6.2.5 Die Surface Modifier ................................................ 186
6.2.6 Temperature.............................................................. 187
6.3 General Observation .............................................................. 192
References ........................................................................................ 193

Chapter 7 Understanding Melt Fracture ........................................................... 201

7.1 Melt Fracture Mechanisms ....................................................202
7.1.1 Reynolds Turbulence ................................................202
7.1.2 Thermal Catastrophe ................................................202
7.1.3 Stress-Induced Fractionation ....................................202
7.1.4 Fracture ....................................................................202
7.1.5 Cavitation .................................................................205
7.1.6 Interfacial Slip ..........................................................205
7.1.6.1 Microscopic Mechanisms—Cohesive
Failure .......................................................207
7.1.6.2 Microscopic Mechanisms—Adhesive
Failure .......................................................209
7.2 The Constitutive Approach .................................................... 211
7.2.1 Phenomenology ........................................................ 211
7.2.2 Relaxation Oscillations ............................................ 212
7.2.3 Numerical Simulations ............................................. 214
7.2.4 Molecular Considerations......................................... 215
xii Contents

7.3 General Understanding .......................................................... 218

7.4 General Observation .............................................................. 225
References ........................................................................................ 226

Chapter 8 Advanced Polymer Rheology ........................................................... 233

8.1 Molar Mass, Zero-Shear Viscosity, and Recoverable
Compliance ............................................................................ 234
8.2 Continuous Models and Frame Invariance............................ 237
8.2.1 Upper-Convected Maxwell Model ........................... 239
8.2.2 Johnson–Segalman–(Oldroyd) Models .................... 241
8.2.2.1 Johnson–Segalman Model ........................ 241
8.2.2.2 Johnson–Segalman–Oldroyd Model ........244
8.2.3 Kaye–Bernstein–Kearsley–Zapas Model ................. 245
8.3 Microscopic Models ..............................................................248
8.3.1 Rouse Model............................................................. 250
8.3.2 Reptation Model ....................................................... 253
8.3.3 Branching ................................................................. 258
8.3.4 Pom-Pom Model ....................................................... 259
8.4 Molar Mass Distribution and Linear Viscoelasticity ............ 261
8.5 General Observation .............................................................. 263
References ........................................................................................ 263

Chapter 9 Modeling Melt Fracture ................................................................... 267

9.1 The Relaxation-Oscillation Model ........................................ 268
9.2 Coupling RO and Constitutive Equations.............................. 271
9.3 Slip-Boundary Conditions ..................................................... 275
9.4 A Rheological Model Including Wall Slip ............................280
9.5 Bulk and Interfacial Viscosity Balance for Different
Polymers ................................................................................284
9.6 Flow Curve and Melt Fracture Relation ................................ 287
9.6.1 “Spurt” Distortions................................................... 288
9.6.2 Surface Distortions ................................................... 288
9.6.3 Volume Distortions................................................... 290
9.7 General Observation ..............................................................290
References ........................................................................................ 291

Chapter 10 Preventing Melt Fracture .................................................................. 295

10.1 Additives ................................................................................ 295
10.1.1 Slip Agents ............................................................... 297
10.1.2 Polymer Blends......................................................... 298
10.1.3 Wax........................................................................... 299
10.1.4 Fillers........................................................................ 299
Contents xiii

10.2 Extruder and Processing Conditions .....................................300

10.3 Dealing with Melt Fracture ................................................... 303
10.3.1 Melt Fracture Checklist ............................................ 305
10.4 General Observation .............................................................. 305
References ........................................................................................306
Index ...................................................................................................................... 313
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