Polymer
Testing
2
nd
Edition
Wolfgang Grellmann
Sabine Seidler
Grellmann, Seidler
Polymer Testing
Wolfgang Grellmann
Sabine Seidler (Eds.)
Hanser Publishers, Munich Hanser Publications, Cincinnati
2
nd
Edition
Polymer
Testing
With contribution by
Volker Altstädt, Monika Bauer, Christian Bierögel, Gert Busse,
Klaus Friedrich, Henrik Höninger, Thomas Lüpke, Bernd Michel,
Hans-Joachim Radusch, Falko Ramsteiner, Andreas Schönhals,
Jörg Trempler
e Editors:
Prof. Dr. rer. nat. habil. Wolfgang Grellmann,
Martin-Luther-University Halle-Wittenberg, Centre of Engineering Science, D-06099 Halle and
Polymer Service GmbH Merseburg, D-06217 Merseburg, Germany
Prof. Dr.-Ing. habil. Sabine Seidler
Vienna University of Technology, Institute of Materials Science and Technology
Favoritenstraße 9, A-1040 Vienna, Austria
Distributed in North and South America by:
Hanser Publications
6915 Valley Avenue, Cincinnati, Ohio 45244-3029, USA
Fax: (513) 527-8801
Phone: (513) 527-8977
www.hanserpublications.com
Distributed in all other countries by
Carl Hanser Verlag
Postfach 86 04 20, 81631 München, Germany
Fax: +49 (89) 98 48 09
www.hanser-fachbuch.de
e use of general descriptive names, trademarks, etc., in this publication, even if the former are not especially
identied, is not to be taken as a sign that such names, as understood by the Trade Marks and Merchandise Marks
Act, may accordingly be used freely by anyone. While the advice and information in this book are believed to be
true and accurate at the date of going to press, neither the author nor the editors nor the publisher can accept any
legal responsibility for any errors or omissions that may be made. e publisher makes no warranty, express or
implied, with respect to the material contained herein.
Library of Congress Cataloging-in-Publication Data
Grellmann, Wolfgang, 1949-
[Kunststopruefung. English]
Polymer testing / Wolfgang Grellmann, Sabine Seidler. -- 2nd edition.
pages cm
Includes bibliographical references and index.
ISBN 978-1-56990-548-7 (hardcover) -- ISBN 978-1-56990-549-4 (e-book) 1. Polymers--Testing. I. Seidler,
Sabine, 1961- II. Title.
TA455.P58G7413 2013
620.1’920287--dc23
2013026084
Bibliograsche Information Der Deutschen Bibliothek
Die Deutsche Bibliothek verzeichnet diese Publikation in der Deutschen Nationalbibliograe;
detaillierte bibliograsche Daten sind im Internet über <http://dnb.d-nb.de> abruar.
ISBN 978-1-56990-548-7
E-Book ISBN 978-1-56990-549-4
All rights reserved. No part of this book may be reproduced or transmitted in any form or by any means, electronic
or mechanical, including photocopying or by any information storage and retrieval system, without permission
in writing from the publisher.
© Carl Hanser Verlag, Munich 2013
Production Management: Steen Jörg
Coverconcept: Marc Müller-Bremer, www.rebranding.de, München
Coverdesign: Stephan Rönigk
Printed and bound by Kösel, Krugzell
Printed in Germany
Preface to the Second Edition
The textbook „Polymer Testing“ is mainly intended for the education of university
students and students of universities of applied sciences. This textbook was deemed
to be necessary because the testing of polymers has become established as a separate
scientific discipline within polymer sciences in recent years. The textbook was first
published in German in 2005. An improved English version was published in 2007,
and a Russian edition appeared in 2010 with special consideration given to the spe-
cific GOST standards.
The positive reviews from our colleagues demonstrate that the concept „Method –
Parameters – Examples“ meets students` needs and is also accepted in practice.
Although there have been no significant changes to basic testing methods since the
first edition appeared, there have been considerable advances in the evaluation of
structure-property correlations and standardisation. It has become increasingly nec-
essary to provide material-scientific parameters to quantify the relationship between
microstructure and macroscopic properties. Therefore, it seemed necessary to pub-
lish a second edition. The previous edition has been comprehensively revised, and the
new edition covers all the latest developments in the field, including all amendments
to the most important polymer test standards up to May 2013.
Using the same concept and methodical structure in the presentation of polymer test
procedures, the parameters obtained by the latter and the selected examples, the new
edition provides university students and students of universities of applied sciences
with a good and fast source of information. This is why the textbook has been widely
adopted by universities and universities of applied sciences for the teaching of „Poly-
mer Testing“.
In order to provide support the lecturers, a PowerPoint presentation has been created
for all pictures and tables. It can be downloaded from www.hanserpublications.com.
In this regard, we would like to thank Prof. Dr.-Ing. Christian Bierögel, in particular,
for his valuable advice in the preparation of this edition and especially for the new
publication of the pictures, which are now in colour, and his extensive work on pro-
ducing the PowerPoint presentation of all pictures.
VI Preface to the Second Edition
A Wiki dictionary, „Plastics Testing and Diagnostics“, has been produced on the sci-
entific basis of the book and of publications from the Merseburg scientific school, and
it often provides more detail than the book. The dictionary is available at
www.polymerservice-merseburg.de/wiki-lexikon-kunststoffpruefung and can be
used for practical work. An extensive compilation of fracture mechanics test speci-
mens and approximation equations to calculate parameters in fracture mechanics are
just two examples of what the dictionary offers.
We would like to thank Carl Hanser Verlag, especially Ms. Dr. N. Warkotsch, Ms. Dr.
C. Strohm, Ms. Dipl.-Ing. (FH) U. Wittmann and Mr. S. Jörg, for their much-
appreciated and reliable assistance.
June 2013 The Editors
Preface to the First Edition
This book is based on the editors’ extensive experience in research, development and
education in the field of materials science and especially polymer testing, polymer
diagnostics and failure analysis. The results of their work were published in several
reference books about deformation and fracture behavior of polymers, in numerous
single publications in peer-reviewed scientific journals and in proceedings. Given the
fact that the field of science undergoes a rapid and dynamic development it seemed
prudent to present these results in a textbook for students.
The following factors convinced us that a comprehensive representation of the state
of knowledge was needed:
• The ever-increasing importance of this materials group for continued technical
progress led to an increasing share of polymers and compounds in various
applications.
• The increased safety awareness led to the development of hybrid methods of
polymer diagnostics, which enable a complex view of the connection between
loading and material behavior under actual loading conditions and ambient
influences
• As a result of the development of fiber-reinforced thermoplastic and
thermosetting composite materials, new challenges to polymer testing methods
emerged.
• The increasing use of polymers and elastomers in medical technology for various
applications requires the development of technological testing methods for
viability, serviceability, operating safety and /or service life.
• As a consequence of the trend to miniaturization components (microsystems),
more suitable testing methods are necessary for the evaluation of various
thermomechanical loadings of materials properties, e.g., in highly integrated
electronic components.
In addition, a number of new standards and regulatory codes for polymer testing
have been introduced over the past years, further emphasizing the need for a
redesigned textbook for this discipline of science. The book presents a comprehensive
representation of knowledge provided by respected colleagues from universities,
universities of applied sciences and the polymer industry. A list of co-authors as well
VIII Preface to the First Edition
as acknowledgements for numerous colleagues and co-workers follow on separate
pages.
The editors and co-authors tried hard to overcome the limits of classic polymer
testing using ASTM and ISO standards in order to make the importance of polymer
testing for the development and application of new polymers, composite materials
and materials compounds, as well as the introduction of new technologies, more
recognizable.
This book is primarily designed for students of bachelor, diploma and master courses
of material science, material technology, plastic technology, mechanical engineering,
process engineering and chemical engineering. It can be used by students, teachers of
universities and colleges for supplementary studies in the disciplines of chemistry and
industrial engineering. The methods of polymer testing are also essential to the
development and application of biomedical or nanostructured materials.
With the publication of this book we hope that it will not only serve the important
task of training of young scientists in physical and material oriented disciplines, but
will also make a contribution to further education of professional polymer testers,
design engineers, and technologists.
We thank Carl Hanser Publishers for publishing this book, entitled “Polymer
Testing”, especially we are grateful to Dr. Christine Strohm who thoroughly revised
the complete text for this edition. We also thank Dr. Paul I. Anderson for the
translation of several chapters. The main idea of this book was based on the 1992s
book by Dr. Heinz Schmiedel “Handbook of Polymer Testing”, written in German
language. We kept the physical-methodical approach and also, the comprehensive
chapter “Fracture Toughness Measurements in Engineering Plastics” based on our
research work in this field for many years. For example it is pointed out on the
extensive collection of fracture mechanics specimen and the evaluation equations for
determination of fracture mechanics parameters.
We want to thank sincerely all co-workers from the Center of Engineering Science
and the Institute of Polymer Materials e.V. of the Martin-Luther-University of Halle-
Wittenberg and all collaborators from the Institute of Materials Science and
Technology of the Vienna University of Technology who, with their commitment and
their willing cooperation, made the publication of this book possible in the first place.
Sabine Seidler, Vienna Wolfgang Grellmann, Halle
May 2007
Listing of Co-authors
Prof. Dr. Volker Altstädt
University of Bayreuth, Germany
(Chapter 10)
Prof. Dr. Monika Bauer
Fraunhofer-Einrichtung für Polymermaterialien und Composite PYCO, Teltow,
Germany
Technical University of Brandenburg (BTU), Cottbus, Germany
(Part 11.2)
Prof. Dr. Christian Bierögel
Martin Luther University Halle-Wittenberg and Polymer Service GmbH Merseburg,
Institute of Martin Luther University Halle-Wittenberg, Germany
(Chapter 2, Part 4.3 and Chapter 9)
Prof. Dr. Gert Busse
University of Stuttgart, Germany
(Chapter 8)
Prof. Dr. Dr. Klaus Friedrich
Institute for Composite Materials (IVW), Technical University of Kaiserslautern,
Germany
(Part 4.8)
Dr. Henrik Höninger
IMA Materialforschung und Anwendungstechnik Dresden, Germany (formerly)
(Parts 4.5, 4.6 and 11.3)
Dr. Thomas Lüpke
Kunststoff-Zentrum (KUZ) Leipzig, Germany
(Parts 4.1 and 4.2)
Prof. Dr. Bernd Michel
FhG Institute for Reliability and Microintegration (IZM) Berlin, Germany
(Chapter 12)
X Co-authors
Prof. Dr. Hans-Joachim Radusch
Martin Luther University Halle-Wittenberg, Germany
(Chapter 3)
Dr. Falko Ramsteiner
BASF Group Ludwigshafen, Germany (formerly)
(Chapter 7)
Prof. Dr. Andreas Schönhals
Federal Institute for Materials Research and Testing (BAM) Berlin, Germany
(Part 6.3)
Dr. Jörg Trempler
Martin Luther University Halle-Wittenberg, Germany (formerly)
(Part 6.2)
The chapters and sections not listed above were written by the editors.
We owe particular gratitude for their assistance with the development and compila-
tion of the manuscript to:
Ms. Dipl.-Ing. Yvonne Chowdhury, InnoMat GmbH, Teltow, Germany
(Part 11.2),
Ms. Dipl.-Ing. Ivonne Pegel, ESW GmbH, Wedel, Germany (Chapter 10) and
Mr. Dr. Hans Walter, FhG Institute for Reliability and Microintegration (IZM)
Berlin, Germany (Chapter 12).
In particular we would like to thank co-author Prof. Dr. Christian Bierögel not only
for his contributions to the book, but moreover for his comprehensive assistance and
critical advice during the composition of the manuscript.
We thank Prof. Dr. Peter Grau for the professional revision of the parts on micro-
hardness testing.
For the critical revision of single chapters we thank our longtime co-workers Ao. Prof.
Dr. mont. Vasiliki-Maria Archodoulaki, Dr. Thomas Koch, Prof. Dr. Ines Kotter,
Dr. Ralf Lach, Prof. Dr. Beate Langer and finally Dr. Katrin Reincke.
We thank Ms. Dagmar Fischer for the technical editing of figures and images that we
provided in various graphical file formats and their transformation into the format
required for printing by Carl Hanser Publishers.
Table of Contents
Nomenclature (Selection) XXI
Terminology XXIX
Symbols and Abbreviated Terms XXXIII
1 Introduction 1
1.1 The Genesis of Polymer Testing as a Science 1
1.2 Factors Influencing Data Acquisition 4
1.3 Classification of Polymer Testing Methods 5
1.4 Standards and Regulatory Codes for Polymer Testing 7
1.5 Compilation of Standards 10
1.6 References by Area of Specialization 11
2 Preparation of Specimens 15
2.1 Introduction 15
2.2 Testing Molding Materials 17
2.3 Specimen Preparation 18
2.3.1 General Remarks 18
2.3.2 Specimen Preparation by Direct Shaping 19
2.3.2.1 Production of Specimens from Thermoplastic
Molding Materials 19
2.3.2.2 Production of Specimens from Thermosetting
Molding Materials 26
2.3.2.3 Production of Specimens from Elastomeric Materials 28
2.3.3 Specimen Preparation by Indirect Shaping 29
2.3.4 Characterization of Specimen State 31
2.4 Specimen Preparation and Conditioning 33
2.5 Compilation of Standards 36
2.6 References 38
3 Determining Process-Related Properties 39
3.1 Molding Materials 39
XII Table of Contents
3.2 Determining Bulk Material Properties 40
3.2.1 Bulk Density, Compacted Apparent Density, Fill Factor 40
3.2.2 Pourability, Angle of Repose, Slide Angle 41
3.3 Determining the Properties of Fluids 42
3.3.1 Rheological Fundamentals 42
3.3.1.1 Viscosity of Newtonian and non-Newtonian Fluids 42
3.3.1.2 Temperature and Pressure Dependence of Viscosity 46
3.3.1.3 Molecular Mass Influence on Viscosity 46
3.3.1.4 Volume Properties 47
3.3.2 Measuring Rheological Properties 48
3.3.2.1 Rheometry/Viscometry 48
3.3.2.2 Rotational Rheometers 49
3.3.2.3 Capillary Rheometers 55
3.3.2.4 Extensional Rheometers 66
3.3.3 Selecting Measurement Methods for Characterizing
Polymer Materials 68
3.4 Compilation of Standards 69
3.5 References 70
4 Mechanical Properties of Polymers 73
4.1 Fundamental Principles of Mechanical Behavior 73
4.1.1 Mechanical Loading Parameters 73
4.1.1.1 Stress 73
4.1.1.2 Strain 76
4.1.2 Material Behavior and Constitutive Equations 77
4.1.2.1 Elastic Behavior 77
4.1.2.2 Viscous Behavior 80
4.1.2.3 Viscoelastic Behavior 82
4.1.2.4 Plastic Behavior 88
4.2 Mechanical Spectroscopy 90
4.2.1 Experimental Determination of Time Dependent
Mechanical Properties 90
4.2.1.1 Static Testing Methods 91
4.2.1.2 Dynamic–Mechanical Analysis (DMA) 92
4.2.2 Time and Temperature Dependence of Viscoelastic Properties 99
4.2.3 Structural Factors Influencing Viscoelastic Properties 102
4.3 Quasi-Static Test Methods 104
4.3.1 Deformation Behavior of Polymers 104
Table of Contents XIII
4.3.2 Tensile Tests on Polymers 110
4.3.2.1 Theoretical Basis of the Tensile Test 110
4.3.2.2 Conventional Tensile Tests 113
4.3.2.3 Enhanced Information of Tensile Tests 122
4.3.3 Tear Test 128
4.3.4 Compression Test on Polymers 130
4.3.4.1 Theoretical Basis of the Compression Test 130
4.3.4.2 Performance and Evaluation of Compression Tests 133
4.3.5 Bend Tests on Polymers 138
4.3.5.1 Theoretical Basis of the Bend Test 138
4.3.5.2 The Standardized Bend Test 144
4.4 Impact Loading 149
4.4.1 Introduction 149
4.4.2 Charpy Impact Test and Charpy Notched Impact Test 150
4.4.3 Tensile-Impact and Notched Tensile-Impact Tests 155
4.4.4 Free-falling Dart Test and Puncture Impact Test 158
4.5 Fatigue Behavior 161
4.5.1 Fundamentals 161
4.5.2 Experimental Determination of Fatigue Behavior 163
4.5.3 Planning and Evaluating Fatigue Tests 167
4.5.4 Factors Influencing the Fatigue Behavior and
Service-Life Prediction of Service Life for Polymers 169
4.6 Long-Term Static Behavior 171
4.6.1 Fundamentals 171
4.6.2 Tensile Creep Test 173
4.6.3 Flexural Creep Test 180
4.6.4 Creep Compression Test 181
4.7 Hardness Test Methods 183
4.7.1 Principles of Hardness Testing 183
4.7.2 Conventional Hardness Testing Methods 185
4.7.2.1 Test Methods for Determining Hardness Values
after Unloading 185
4.7.2.2 Test Methods for Determining Hardness Values
under Load 187
4.7.2.3 Special Testing Methods 191
4.7.2.4 Comparability of Hardness Values 191
4.7.3 Instrumented Hardness Test 193
4.7.3.1 Fundamentals of Measurement Methodology 193
XIV Table of Contents
4.7.3.2 Material Parameters Derived from Instrumented
Hardness Tests 195
4.7.3.3 Examples of Applications 198
4.7.4 Correlating Microhardness with Yield Stress and
Fracture Toughness 200
4.8 Friction and Wear 203
4.8.1 Introduction 203
4.8.2 Fundamentals of Friction and Wear 205
4.8.2.1 Frictional Forces 205
4.8.2.2 Temperature Increase Resulting from Friction 206
4.8.2.3 Wear as a System Characteristic 207
4.8.2.4 Wear Mechanisms and Formation of Transfer Film 207
4.8.3 Wear Tests and Wear Characteristics 208
4.8.3.1 Selected Model Wear Tests 209
4.8.3.2 Wear Parameters and Their Determination 211
4.8.3.3 Wear Parameters and Their Presentation 212
4.8.4 Selected Experimental Results 213
4.8.4.1 Counterbody Influence 213
4.8.4.2 Influencing of Fillers 214
4.8.4.3 Influence of Loading Parameters 216
4.8.4.4 Predicting Properties Via Artificial Neural Networks 217
4.8.5 Summary 219
4.9 Compilation of Standards 219
4.10 References 225
5 Fracture Toughness Measurements in Engineering Plastics 233
5.1 Introduction 233
5.2 Current State and Development Trends 234
5.3 Fundamental Concepts of Fracture Mechanics 235
5.3.1 Linear-Elastic Fracture Mechanics (LEFM) 235
5.3.2 Crack-Tip-Opening Displacement (CTOD) Concept 240
5.3.3 J-Integral Concept 243
5.3.4 Crack Resistance (R-) Curve Concept 245
5.4 Experimental Determination of Fracture Mechanical Parameters 247
5.4.1 Quasi-static Loading 247
5.4.2 Instrumented Charpy Impact Test 251
5.4.2.1 Test Configuration 251
5.4.2.2 Maintenance of Experimental Conditions 252
Table of Contents XV
5.4.2.3 Types of Load–Deflection Diagrams – Optimization
of Diagram Shape 253
5.4.2.4 Special Approximation Methods for
Estimating J Values 256
5.4.2.5 Requirements for Specimen Geometry 258
5.4.3 Instrumented Free-Falling Dart Test 261
5.5 Applications for Material Development 263
5.5.1 Fracture Mechanical Toughness Evaluation on
Modified Polymers 263
5.5.1.1 Particle Filled Thermoplastics 263
5.5.1.2 Fiber-Reinforced Thermoplastics 267
5.5.1.3 Blends and Copolymers 271
5.5.2 Instrumented Tensile-Impact Testing for Product Evaluation 277
5.5.3 Consideration of Fracture Behavior for Material Selection and
Dimensioning 280
5.6 Compilation of Standards 282
5.7 References 284
6 Testing of Physical Properties 287
6.1 Thermal Properties 287
6.1.1 Introduction 287
6.1.2 Determining Heat Conductivity 289
6.1.3. Differential Scanning Calorimetry (DSC) 293
6.1.4 Thermogravimetric Analysis (TGA) 298
6.1.5 Thermomechanical Analysis (TMA) 300
6.2 Optical Properties 304
6.2.1 Introduction 304
6.2.2 Reflection and Diffraction 304
6.2.2.1 Directed and Diffuse Reflection 304
6.2.2.2 Refractive Index Determination 305
6.2.3 Dispersion 309
6.2.4 Polarization 310
6.2.4.1 Optical Activity 310
6.2.4.2 Polarization of Optical Components 311
6.2.4.3 Polarization-Optical Testing Methods 312
6.2.5 Transmission, Absorption and Reflection 319
6.2.6 Gloss, Intrinsic Diffuse Reflectance and Haze 321
6.2.7 Color 325
XVI Table of Contents
6.2.8 Transparency and Translucency 328
6.2.9 Infrared Spectroscopy 332
6.2.10 Laser Technology 334
6.2.11 Testing the Stability of Optical Values 335
6.3 Electrical and Dielectrical Properties 337
6.3.1 Introduction 337
6.3.2 Physical Fundamentals 339
6.3.3 Electrical Conductivity and Resistance 342
6.3.3.1 Volume Resistivity 343
6.3.3.2 Surface Resistivity 345
6.3.3.3 Insulation Resistance 347
6.3.3.4 Measuring Procedures 347
6.3.3.5 Contacting and Specimen Preparation 350
6.3.4 Dielectrical Properties and Dielectrical Spectroscopy 351
6.3.4.1 Relaxation Processes 352
6.3.4.2 Alternating Current Conductivity (AC Conductivity) 360
6.3.4.3 Broadband Dielectric Measurement Techniques 360
6.3.5 Special Technical Testing Methods 368
6.3.5.1 Electrostatic Charge 368
6.3.5.2 Electric Strength 370
6.3.5.3 Creep Resistance and Arc Resistance 374
6.4 Compilation of Standards 376
6.5 References 380
7 Evaluating Environmental Stress Cracking Resistance 385
7.1 General Remarks on the Failure of Polymers in Aggressive Fluids 385
7.2 Testing Environmental Stress Cracking Resistance 389
7.2.1 Test Methods for Determining Environmental
Stress Crack Formation 389
7.2.2 Examples for Evaluating Environmental Stress Cracking
Resistance with Standardized Test Methods 392
7.2.3 Fracture Mechanics Test Methods 397
7.3 Modeling Plastics Failure in Fluids Caused by Stress Cracking 401
7.4 Factors Influencing Stress Cracking Behavior 404
7.4.1 Crosslinking 404
7.4.2 Molecular Weight and Molecular Weight Distribution 405
7.4.3 Branching 407
7.4.4 Crystalline Regions 408
Table of Contents XVII
7.4.5 Molecular Orientation 409
7.4.6 Physical-Chemical Interaction Processes 412
7.4.7 Viscosity of the Immersion Fluid 418
7.4.8 Influence of Test Specimen Thickness 423
7.4.9 Temperature Influence 424
7.5 Compilation of Standards 427
7.6 References 428
8 Non-Destructive Polymer Testing 431
8.1 Introduction 431
8.2 Non-Destructive Testing by Electromagnetic Waves 433
8.2.1 X-Ray Radiation 433
8.2.1.1 Projection Methods by Means of Absorption 434
8.2.1.2 Compton Backscatter 436
8.2.1.3 X-Ray Refractometry 437
8.2.2 Spectral Range of Visible Light 439
8.2.2.1 Measuring Thickness of Transparent Components 440
8.2.2.2 Photoelastic Imaging of Transparent Components 440
8.2.2.3 Confocal Laser Scan Microscopes 441
8.2.2.4 Line Projection for Detecting Contour 442
8.2.2.5 Interferometric Methods 443
8.2.3 Thermography 449
8.2.4 Microwaves 449
8.2.5 Dielectric Spectroscopy 453
8.2.6 Eddy Current 455
8.3 Non-Destructive Testing with Elastic Waves 456
8.3.1 Elastic Waves under Linear Material Behavior 457
8.3.1.1 Ultrasound 457
8.3.1.2 Mechanical Vibrometry 467
8.3.2 Elastic Waves with Non-linear Material Behavior 472
8.3.2.1 Fundamentals on Elastic Waves in
Non-Linear Materials 472
8.3.2.2 Non-Linear Air-Ultrasound 472
8.3.2.3 Non-Linear Vibrometry 475
8.4 Non-Destructive Testing by Dynamic Heat Transport 478
8.4.1 External Excitation 478
8.4.1.1 Heat-Flux Thermography by Non-Periodical
Heat Transport 478
XVIII Table of Contents
8.4.1.2 Thermography with Periodical Heat Transport 481
8.4.2 Internal Excitation 484
8.4.2.1 Thermography with Excitation by Elastic Waves 484
8.4.2.2 Thermography with Other Types of Internal Excitation 489
8.5 Outlook 489
8.6 References 491
9 Hybrid Methods of Polymer Diagnostics 497
9.1 Objectives 497
9.2 Tensile Test, Acoustic Emission Test and Video Thermography 499
9.3 Tensile Test and Laser Extensometry 501
9.4 Fracture Mechanics and Non-Destructive Testing 506
9.5 References 510
10 Testing of Composite Materials 513
10.1 Introduction 513
10.2 Theoretical Background 514
10.2.1 Anisotropy 514
10.2.2 Elastic Properties of Laminates 516
10.2.3 Influence from Moisture and Temperature 516
10.2.4 Laminate Theory and St. Venant’s Principle 517
10.2.5 Applying Fracture Mechanical Concepts to Fiber Composites 518
10.3. Specimen Preparation 520
10.3.1 Manufacture of Laminates 520
10.3.2 Preparing Specimens for Unidirectional Loading 522
10.4 Determining Fiber Volume Content 524
10.5 Mechanical Test Methods 525
10.5.1 Tensile Tests 525
10.5.2 Compression Tests 528
10.5.3 Flexural Tests 532
10.5.4 Interlaminar Shear Strength 534
10.5.5 Shear Tests 536
10.5.5.1 r 45° Off-Axis Tensile Test 536
10.5.5.2 10° Off-Axis Tensile Test 538
10.5.5.3 Two- and Three-Rail Shear Test 538
10.5.5.4 Iosipescu Shear Test 540
10.5.5.5 Plate-Twist Shear Test 541
10.5.5.6 Torsional Loading on Thin-Walled Tubes 542
Table of Contents XIX
10.6 Fracture Mechanical Test Methods 543
10.6.1 Experimental Tests on Fiber Composite Materials 543
10.6.2 Special Specimen Configuration 544
10.6.2.1 Specimens for Mode I Loading 544
10.6.2.2 Specimen for Mode II Loading 546
10.6.2.3 Mixed-Mode Specimens 549
10.6.3 Fracture Mechanical Values of Fiber Composite Materials 551
10.7 Dedicated Test Methods 553
10.7.1 Edge Delamination Test (EDT) 553
10.7.2 Boeing Open-Hole Compression Test 554
10.8 Peel Strength of Flexible Laminates 554
10.9 Impact Loading and Damage Tolerance 556
10.10 Compilation of Standards and Guidelines 560
10.11 References 562
11 Technological Testing Methods 565
11.1 Heat Distortion Resistance 565
11.1.1 Fundamentals and Definitions 565
11.1.2 Determining Heat Distortion Resistance Temperature HDT
and Vicat Softening Temperature 566
11.1.3 Practical Examples for the Informational Value of the Vicat
and HDT Test 569
11.2 Fire Behavior 573
11.2.1 Introduction 573
11.2.2 Stages of a Fire and Fire-Determining Parameters 575
11.2.3 Fire Tests 577
11.2.3.1 Smoldering Fire 578
11.2.3.2 Ignitability 579
11.2.3.3 Flame Spread 584
11.2.3.4 Heat Release 586
11.2.3.5 Fire Resistance 588
11.2.3.6 Ease of Extinguishment 588
11.2.4 Utilization of a Cone Calorimeter to Characterize Fire Behavior 590
11.3 Component Testing 596
11.3.1 Introduction 596
11.3.2 Basic Testing Methods 597
11.3.2.1 General Remarks 597
11.3.2.2 Testing Visible Features 597
XX Table of Contents
11.3.2.3 Testing Materials Properties 599
11.3.2.4 Testing Serviceability 601
11.3.3 Testing Plastic Piping 603
11.3.3.1 Quality Assurance for Plastic Piping 603
11.3.3.2 Testing Hydrostatic Rupture Strength for Plastic Pipes 604
11.3.4 Testing Plastics Components for Application in Vehicle Design 607
11.3.4.1 Test Requirements 607
11.3.4.2 Mechanical Tests 607
11.3.4.3 Permeation and Emission Tests 609
11.3.5 Testing Plastics Components for Application in
Building Construction 612
11.3.5.1 Introduction 612
11.3.5.2 Testing Sandwich Panels 613
11.3.5.3 Testing Plastic Casing Pipes 616
11.4 Implant Testing 621
11.4.1 Introduction 621
11.4.2 Push-out Tests for Implants 623
11.4.3 Testing the Application Behavior of Pharyngotracheal
Voice Prostheses 626
11.4.4 Determining the Mechanical Properties of Human Cartilage 629
11.5 Compilation of Standards 631
11.6 References 634
12 Testing of Microcomponents 637
12.1 Introduction 637
12.2 Microspecimen Testing 640
12.2.1 Micro-Tensile Tests 640
12.2.2 Fracture Mechanics Investigations Using Mini
Compact Tension (CT) Specimens 645
12.3 Nanoindentation Testing 647
12.4 Testing Methods on Their Way to the Nanoworld 649
12.4.1 Non-Contacting Displacement Field Analysis Using
Digital Image Correlation (Gray-Value Correlation Analysis) 649
12.4.2 In-Situ Deformation Measurement with
Atomic Force Microscopy (AFM) 651
12.5 References 655
Subject Index 659
Nomenclature (Selection)
a (mm)
initial crack length (i.e. machined notch plus razor-sharpened tip),
the physical crack size at the start of testing
a
BS
(mm)
physical crack length augmented to account for crack tip plastic
deformation (fracture mirror length)
a
cN
(kJ m
-2
) Charpy impact strength of notched specimen according to ISO 179
a
cU
(kJ m
-2
)
Charpy impact strength of unnotched specimen according to
ISO 179
a
eff
(mm) effective crack length
a/W ratio of initial crack length to specimen width
a (O) absorption degree
A (μm) average interparticle distance
A
0
(mm
2
) cross-section
A
el
(N mm) elastic part of A
G
A
G
(N mm)
total deformation energy of test specimen computed from the area
under the load–deflection diagram up to F
max
A
H
(N mm) nominal impact energy of pendulum hammer
A
k
(N mm)
complementary deformation energy, used in the J-integral evalua-
tion method of Merkle and Corten
A
n
n
th
amplitude considered for the calculation of the logarithmic
decrement
A
pl
(N mm) plastic part of A
G
A
R
(N mm) crack propagation energy
A
S
(mm
2
) damage area
b (mm) specimen width according to ISO 179
b
N
(mm)
remaining width at the notch base of the test specimen according to
ISO 179-1
B (mm) specimen thickness
C (mm N
-1
) compliance
C
i
constants of the power law for describing J
R
-curves
d (mm) effective way of light through the specimen
D (μm) average particle diameter
XXII Nomenclature (Selection)
D
1,2
geometrical functions in the J-integral evaluation method of Merkle
and Corten (MC)
E (MPa) Young’s modulus (modulus of elasticity)
E (kJ m
-2
) tensile-impact strength according to ISO 8256
E
50
(J) energy at 50 % failure according to ISO 6603-1
E
c
(J) corrected impact energy according to ISO 179-1
E
d
(MPa) dynamic flexural modulus
E
f
(MPa) flexural modulus according to ISO 178
E
n
(kJ m
-2
) tensile-impact strength (notched specimen) according to ISO 8256
E
t
(MPa) modulus of elasticity according to ISO 527
F (mm) deflection
f
gy
(mm)
deflection at the transition from elastic to elastic–plastic material
behavior
f
K
(mm) maximum deflection f
max
excluding the component f
B
f
max
(mm) deflection at maximum load F
max
F (N) load (force)
F
1
(N)
inertial load, which arises from the inertia of the part of the test
specimen accelerated after the first contact with the striker
F
gy
(N)
characteristic load value corresponding to the transition from
elastic to elastic–plastic material behavior
F
max
(N) maximum load
F
P
(N) maximum load (force) according to ISO 6603-2
g gloss degree
G gloss
G (MPa) shear modulus
G (N mm
-1
) energy release rate
G
12
(MPa) interlaminar shear modulus
G
I
(N mm
-1
) energy release rate in mode I
G
Ic
(N mm
-1
)
energy release rate, critical value at the point of unstable crack
growth; static loading, geometry-independent
G
IIc
(N mm
-1
)
energy release rate in mode II, critical value at the point of unstable
crack growth; static loading, geometry-independent
Gc (MPa) dynamic modulus (storage modulus)
Gcc (MPa) dynamic modulus (loss modulus)
GD basic dispersion
h gloss height
H heterogeneity
Nomenclature (Selection) XXIII
HB (N mm
-2
) ball indentation hardness according to DIN EN ISO 2039-1
HDT (°C) heat distortion temperature according to ISO 75
HK (N mm
-2
) Knoop hardness
HM (N mm
-2
) Martens hardness
HR (N mm
-2
) Rockwell hardness
HV (N mm
-2
) Vickers hardness
I intensity
I
p
(A) photometer current intensity at a bearing specimen
I
po
(A)
photometer current intensity at a bearing specimen at perpendicu-
lar light direction
I
sw
(A) photometer current intensity at a bearing matt white standard
I
swo
(A)
photometer current intensity at a bearing matt white standard at
perpendicular light direction
J (N mm
-1
)
J-integral; a mathematical expression, a line or surface integral that
encloses the crack front from one surface to the other, used to
characterize the local stress–strain field around the crack front;
fracture mechanics parameters are calculated using methods of
evaluation of this integral
J
I
(N mm
-1
)
J value in mode I (the index I is only used in the case of geometry
independence)
J
Id
(N mm
-1
)
critical J value at the point of unstable crack growth; dynamic load-
ing, geometry-independent
J
Id
MC
(N mm
-1
)
critical J value at the point of unstable crack growth, for dynamic
loading, in the geometry-independent J-integral evaluation method
of Merkle and Corten
J
Id
ST
(N mm
-1
)
critical J value at the point of unstable crack growth, for dynamic
loading, in the geometry-independent J-integral evaluation method
of Sumpter and Turner
J
0,2
(N mm
-1
)
technical crack initiation value for an amount of crack growth of
'a = 0.2 mm
J
i
(N mm
-1
)
physical crack initiation value determined from intersection of
stretch zone width and J–R curve
JT
J
(N mm
-1
) energy absorption capacity of a material during stable crack growth
k
Boltzmann number (k = 1,38 10
-23
J K
-1
)
k
number of colour order of an isochromatic line series
K (MPa) compression modulus
K (MPa mm
1/2
) stress intensity factor
K
I
(MPa mm
1/2
)
stress intensity factor in mode I (the index I is only used in the case
of geometry independence)
XXIV Nomenclature (Selection)
K
Ic
(MPa mm
1/2
)
fracture toughness, critical value at the point of unstable crack
growth; static loading, geometry-independent
K
Id
(MPa mm
1/2
)
fracture toughness, critical value at the point of unstable crack
growth; dynamic loading, geometry-independent
CTOD
Id;Ic
K (MPa mm
1/2
) K
Ic
and K
Id
, calculated from CTOD
l (mm) specimen length
L (mm) clamping length; initial distance between grips
L (mm) support span according to ISO 179-1
L
0
(mm) initial gauge length
m (g) mass
m constraint factor in relation between J and G concepts
m
P
(kg) weight of pendulum hammer
M
c
molecular weight of a chain network
M
W
(g mol
-1
) molecular weight, weight average
MFR (g (10 min)
-1
) melt mass-flow rate according to ISO 1133
MVR (cm
3
(10 min)
-1
) melt volume-flow rate according to ISO 1133
n rotational factor
n refraction, refraction index
n
C
refraction at wavelength C (656 nm) of the Fraunhofer line
n
D
refraction at wavelength D (589 nm) of the Fraunhofer line
n
f
refraction of immersion oil at temperature in contrast minimum
n
F
refraction at wavelength F (486 nm) of the Fraunhofer line
n
x
refraction of immersion oil at room temperature
N crosslink density
p (O) spectral reflexion degree
p (MPa) pressure
Q (J) quantity of heat
r
N
(μm) notch base radius according to ISO 179-1
R universal gas constant (R = 8,314 J mol
-1
K
-1
)
R
s
reflectance of a layer above a black ground
R
f
reflectance of an optical dense layer
s (mm) support span
S dispersion coefficient
t (s) time
t
b
(ms) time to brittle fracture
t
B
(ms) time to fracture
Nomenclature (Selection) XXV
t
p
(ms) time to maximum load according to ISO 6603-2
tan G mechanical loss factor
T total transmission
T (°C) temperature
T
D
translucency
T
g
(°C) glass transition temperature
T
g
haze dimension
T
J
tearing modulus
T
J
0,2
tearing modulus determined from J–'a curve at 'a = 0.2 mm
T
m
(°C) melting temperature
T
p
transparency
T
s
transmittance of the scattered light
T
S
(N mm
-1
) tear strength
T
G
0,2
tearing modulus determined from G-'a curve at 'a = 0,2 mm
U (N mm) deformation energy
v (mm) crack-mouth-opening displacement
v
I
(m s
-1
) impact velocity according to ISO 13802
v
L
(mm) load-line displacement
v
T
(mm min
-1
);
(m s
-1
)
cross-head speed
V mm
3
volume
VST (°C) Vicat softening temperature
W (mm) specimen width
W
S
(mm
3
(Nm)
-1
) specific wear rate
x standardized colour data
X intensity of the colour red
y standardized colour data
Y intensity of the colour green
z (mm) distance of knife-edge from specimen surface
Z intensity of the colour blue
D (K
-1
) linear thermal expansion
E proportionality constant of geometrical size criterion for LEFM
E (n °C
-1
) temperature coefficient of refraction
J shear strain
J
12
interlaminar shear strain
J
shear rate
XXVI Nomenclature (Selection)
G (mm)
crack-tip-opening displacement describing the local strain field in
front of the crack tip, calculated with the help of the plastic-hinge
model
G
I
(mm)
crack-tip-opening displacement in mode I (the index I is only used
in the case of geometry independence)
G
Ic
(mm)
critical
G value for unstable crack growth, quasi-static loading,
geometry-independent
G
Id
(mm)
critical
G value for unstable crack growth, dynamic loading,
geometry-independent
G
Idk
(mm)
critical
G value for unstable crack growth obtained by using
advanced plastic-hinge model, dynamic loading, geometry-
independent
G
0,2
(mm) technical crack-opening displacement calculated at 'a = 0.2 mm
G
i
(mm) crack-tip-opening displacement at physical crack initiation
'a (mm)
amount of stable crack growth, distance between original crack size
and crack front after loading
'a
max
(mm) upper validity limit of 'a
'a
min
(mm) lower validity limit of 'a
'l (mm) increase in specimen length
'L (mm) increase in clamping length
'L
0
(mm) increase in gauge length
'n birefringence
't (s) time difference
'v (m s
-1
) velocity change
H
proportionality constant of geometrical size criterion for J-integral
concept
H (%) strain
H (°) angle of incidence
Hc (°) angle of refraction
H
(s
-1
) strain rate
H
AE
(%) critical strain at acoustic onset
H
B
(%) tensile strain at break according to ISO 527
H
f
(%) normal flexural strain
H
l
(%) local strain
H
lmax
(%) maximum local strain
H
lmin
(%) minimum local strain
H
M
(%) normative strain at tensile strength according to ISO 527
H
q
(%) lateral (transverse) strain
Nomenclature (Selection) XXVII
H
t
(%) nominal tensile strain according to ISO 527
H
tB
(%) nominal tensile strain at break according to ISO 527
H
tM
(%) nominal strain at tensile strength according to ISO 527
H
W
(%) true strain
H
y
(%) yield strain according to ISO 527
K geometrical function
K dynamic viscosity
K
el; pl
geometrical functions for assessment of elastic (el) and plastic (pl)
parts of deformation energy used in the J-integral evaluation
method of Sumpter and Turner
O extension ratio
O (W (m K)
-1
) heat conductivity
O (nm) light wavelength
/ logarithmic decrement according to ISO 6721-1
P coefficient of friction, Poisson’s ratio
Q Poisson’s ratio
Q Abbe number
[ proportionality constant of geometrical size criterion for CTOD
U (kg m
-3
) density
V (MPa) stress
V
B
(MPa) tensile stress at break according to ISO 527
V
f
(MPa) flexural stress according to ISO 178
V
fc
(MPa) flexural strength at peripheral strain of 3.5 % according to ISO 178
V
fM
(MPa) flexural strength according to ISO 178
V
F
(MPa) yield stress: either V
y
or V
F
= 1/2(V
y
+V
M
)
V
l
(MPa) local stress
V
M
(MPa) tensile strength according to ISO 527
V
V
(MPa) comparative stress
V
W
(MPa) true stress
V
y
(MPa) yield stress (yield point) according to ISO 527
W (MPa) shear stress
W oscillation period
W
12
(MPa) interlaminar shear stress
W (O) spectral transmittance
M
V
filler or fiber content
) light beam that is bearing on a layer
XXVIII Nomenclature (Selection)
)
ds
KW
small angle light scattering
)
ds
WW
wide angle light scattering
)
dp
linear transmitted part of light
)
e
O
(W) hitting spectral radiant flux
(
)
e
O
)
a
(W) absorbed spectral radiant flux
(
)
e
O
)
p
(W) reflected spectral radiant flux
(
)
e
O
)
W
(W) transmitted spectral radiant flux
Terminology
AE acoustic emission analysis
AF aramid-fiber
AFM atomic force microscopy
ASTM American Society for Testing and Materials
ATR attenuated total reflection
BMI Bismaleinimide
BSS Boeing Specification Support Standard
BTT brittle-to-tough transition temperature
CA coupling agent
CF carbon-fiber
CFC carbon-fiber composite
CFRP carbon-fiber reinforced polymer
CFR Code of Federal Regulations
CT compact tension specimen
CTOD crack-tip-opening displacement
DCB double-cantilever beam specimen
DENT double-edge-notched tension specimen
DIN German Institute of Industrial Standards (D
eutsches Institut für
N
ormung)
DMTA dynamic–mechanical–thermal analysis
DOP Dioctylphthalat
DSC differential scanning calorimetry
DTG differential thermogravimetry
DVM German Association for Materials Testing (D
eutscher Verband für
M
aterialprüfung)
DVS German Association for Welding (D
eutscher Verband für Schweis-
sen und verwandte Verfahren)
EN European Norm
EPFM elastic–plastic fracture mechanics
ESIS European Structural Integrity Society
ESPI electronic speckle-pattern interferometry
FAR Federal Aviation Regulations
FEM finite element method
