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DEGREE PROJECT IN ENGINEERING MECHANICS,
SECOND CYCLE, 30 CREDITS

STOCKHOLM , SWEDEN 2016
Towards the Measurement of Two

Independent Viscoelastic
Functions Using Spherical
Indentation
HASSAN MOHAMMED
KTH ROYAL INSTITUTE OF TECHNOLOGY

SCHOOL OF ENGINEERING SCIENCES
Contents
List of Figures iv
List of Tables vii
List of Symbols viii
List of Abbreviations ix
Abstract x
Acknowledgement xi
1 Introduction 1
2 Literature Review 5
2.1 Indentation of Viscoelastic Materials . . . . . . . . . . . . . . . . 5
2.1.1 Indentation Creep/Relaxation with Constant Poisson’s Ra-
tio . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5
2.1.2 Lee and Radok’s Functional Integrals . . . . . . . . . . . 7
2.1.3 Other Methods . . . . . . . . . . . . . . . . . . . . . . . . 9
2.2 Indentation of Bitumen and Bitumen-based Materials . . . . . . 10
2.2.1 Indentation Creep/Relaxation with Constant Poisson’s Ra-
tio . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 10
2.2.2 Lee and Radok’s Functional Integrals . . . . . . . . . . . 11
2.2.3 Other Methods . . . . . . . . . . . . . . . . . . . . . . . . 12
3 Analytical Solutions 15
3.1 The Linear elastic solution . . . . . . . . . . . . . . . . . . . . . . 15
3.2 Relaxation indentation test . . . . . . . . . . . . . . . . . . . . . 17
3.3 Ramp test . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 17
ii
4 Validation of Analytical Solutions Using Simulations 19
4.1 Models Overview . . . . . . . . . . . . . . . . . . . . . . . . . . . 19
4.1.1 Indentation Relaxation Test . . . . . . . . . . . . . . . . . 21
4.1.2 Indentation Ramped Load Test . . . . . . . . . . . . . . . 22
4.2 Back-Calculation of the Viscoelastic Functions from Model Data 22
4.2.1 Indentation Relaxation Test . . . . . . . . . . . . . . . . . 22
4.2.2 Indentation Ramped Load Test . . . . . . . . . . . . . . . 27
4.3 Effect of Finite Specimen Dimensions . . . . . . . . . . . . . . . . 32
4.4 Effect of Errors in Strain Measurement . . . . . . . . . . . . . . . 32
5 Experimental Tests 34
5.1 Tensile Test on POM Samples . . . . . . . . . . . . . . . . . . . . 34
5.1.1 The Experimental Setup . . . . . . . . . . . . . . . . . . . 35
5.1.2 Mathematical Formulation . . . . . . . . . . . . . . . . . 36
5.1.3 Experimental Results . . . . . . . . . . . . . . . . . . . . 37
5.2 Indentation Tests on POM Samples . . . . . . . . . . . . . . . . . 41
5.2.1 The Experimental Setup . . . . . . . . . . . . . . . . . . . 41
5.2.2 Machine Compliance . . . . . . . . . . . . . . . . . . . . . 43
5.2.3 Relaxation Indentation Tests Results . . . . . . . . . . . . 43
5.2.4 Ramped Indentation Tests Results . . . . . . . . . . . . . 49
6 Discussion 53
6.1 Analytical Solutions . . . . . . . . . . . . . . . . . . . . . . . . . 53
6.2 The Tensile Test . . . . . . . . . . . . . . . . . . . . . . . . . . . 54
6.3 The Indentation Relaxation Test . . . . . . . . . . . . . . . . . . 54
6.4 The Indentation Ramped Test . . . . . . . . . . . . . . . . . . . . 55
7 Conclusion 56
Appendices 61
A Linear Elastic Equations 62

A.1 Load–Depth Equation . . . . . . . . . . . . . . . . . . . . . . . . 62
A.2 Circumferential Strain Relation . . . . . . . . . . . . . . . . . . . 63
B Experimental Results 64
B.1 Uniaxial Tensile Tests . . . . . . . . . . . . . . . . . . . . . . . . 64
B.2 Indentation Relaxation Tests . . . . . . . . . . . . . . . . . . . . 66
B.3 Indentation Ramped Tests . . . . . . . . . . . . . . . . . . . . . . 69
iii
List of Figures
1 ZHU zwickiLine a commercial indenter for universal hardness

testing . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2
2 Schematic of multi-scale modeling of bitumen, mastic and asphalt
by Jäger, Lackner, and Stangl (2007) . . . . . . . . . . . . . . . . 3
3 Predicted and experimental results for Polyurethane (left) and

PL-1 (right), Oyen (2006) . . . . . . . . . . . . . . . . . . . . . . 9
4 non-linear dash-pot model, Jäger, Lackner, and Stangl (2007) . . 11
5 Validation of nano-indentation results, Jäger, Lackner, and Stangl
(2007) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 12
6 Validation of nano-indentation results, Veytskin, Bobko, and Ca-
storena (2014) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 13
7 A schematic of the indentation showing relevant parameters . . . 16
8 The geometry and boundary conditions used in the analysis, ge-

ometry to half-space scale is changed for illustration purposes . . 20
9 The zoomed-in view of the mesh and the different zones used . . 21
10 A plot showing the indented geometry with 26 elements in contact 21
11 Relaxation load . . . . . . . . . . . . . . . . . . . . . . . . . . . . 23
12 Relaxation circumferential strain . . . . . . . . . . . . . . . . . . 24
13 The shear viscoelastic function (relaxation test) . . . . . . . . . . 24
14 The bulk viscoelastic function (relaxation test) . . . . . . . . . . 25
15 The time dependent Poisson’s ratio (relaxation test) . . . . . . . 25
16 The error in the viscoelastic functions (relaxation test) . . . . . . 26
17 The error in the viscoelastic bulk function (relaxation test) . . . 26
18 The ramped load . . . . . . . . . . . . . . . . . . . . . . . . . . . 27
19 Slope of square–root of cubed depth . . . . . . . . . . . . . . . . 28
20 Slope of circumferential strain . . . . . . . . . . . . . . . . . . . . 28
21 The shear viscoelastic function (ramp test) . . . . . . . . . . . . 29
22 The bulk viscoelastic function (ramp test) . . . . . . . . . . . . . 29
iv
23 The time dependent Poisson’s ratio (ramp test) . . . . . . . . . . 30
24 The error in the viscoelastic functions (ramp test) . . . . . . . . 30
25 The error in the viscoelastic bulk function (ramp test) . . . . . . 31
26 The errors obtained in the calculation of the viscoelastic functions
vs. the quotient of the contact radius to the distance from the
center of contact to the sample edges . . . . . . . . . . . . . . . . 32
27 The errors in the obtained viscoelastic functions due to errors in
strain measurement . . . . . . . . . . . . . . . . . . . . . . . . . . 33
28 The uniaxial creep test sample . . . . . . . . . . . . . . . . . . . 34

29 The uniaxial creep test experimental setup . . . . . . . . . . . . . 35
30 The strain gauge on the uniaxial creep sample . . . . . . . . . . . 35
31 The axial stress for sample 3 at 15 M P a load level . . . . . . . . 37
32 The axial strain for sample 3 at 15 M P a load level . . . . . . . . 38
33 The axial strain for sample 3 at 20 M P a load level . . . . . . . . 38
34 The creep compliance for sample 3 at 15 M P a load level . . . . . 39
35 The relaxation function for POM . . . . . . . . . . . . . . . . . . 40
36 The Poisson’s ratio for POM . . . . . . . . . . . . . . . . . . . . 40
37 The indentation tests setup . . . . . . . . . . . . . . . . . . . . . 42
38 The strain gauges glued to the POM specimen . . . . . . . . . . 42
39 Load displacement curve for the testing machine . . . . . . . . . 43
40 Load change in time during the relaxation indentation test . . . 44
41 Indentation depth change in time during the relaxation indenta-
tion test . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 44
42 Strain change in time during the relaxation indentation test . . . 45
43 Shear relaxation modulus obtained at different depths for the
indentation relaxation test . . . . . . . . . . . . . . . . . . . . . . 46
44 Averaged shear relaxation modulus for the indentation relaxation
test with 95% confidence interval . . . . . . . . . . . . . . . . . . 46
45 Averaged shear relaxation modulus from indentation relaxation
compared to uniaxial creep test . . . . . . . . . . . . . . . . . . . 47
46 Difference error between shear relaxation modulus from indenta-
tion relaxation and the uniaxial creep test . . . . . . . . . . . . . 48
47 Load change in time during the ramped indentation test . . . . . 49
48 Indentation depth change in time during the ramped indentation
test . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 50
49 Averaged shear relaxation modulus from indentation ramped test
compared to the indentation relaxation and uniaxial creep tests . 50
50 Averaged shear relaxation modulus for the indentation ramped
test with 95% confidence interval . . . . . . . . . . . . . . . . . . 51
v
51 Difference error between shear relaxation modulus from indenta-
tion ramped test and the uniaxial creep test . . . . . . . . . . . . 52
52 E(t) for the tensile tests on Specimen 1 . . . . . . . . . . . . . . 64

55 G(t) for the relaxation indentation test at 40 µm depth . . . . . 66
59 G(t) for the ramped indentation test at depths 20 µm initial and
50 µm final . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 69
60 G(t) for the ramped indentation test at depths 30 µm initial and
60 µm final . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 70
vi
List of Tables
1 Flat punch indentation validation error, Larsson and Carlsson

(1998) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6
2 Maximum validation errors for different materials, VanLanding-
ham et al. (2005) . . . . . . . . . . . . . . . . . . . . . . . . . . . 7
3 Maximum validation errors for different materials and different
indenters, Lu et al. (2003) . . . . . . . . . . . . . . . . . . . . . . 7
4 Shear and bulk viscoelastic functions validation errors, Huang
and Lu (2006) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8
5 Smallest diameter du for each uniaxial test sample . . . . . . . . 35

6 Depths used in the indentation relaxation test . . . . . . . . . . . 41
7 Depths used in the indentation ramped test . . . . . . . . . . . . 42
vii
List of Symbols
A Contact area of indentation
a Contact radius
A0 Constant contact area during relaxation indentation
Au Smallest area in the uniaxial test
D Indenter diameter
ei Prony series parameter for relaxation viscoelastic function
˜θ Laplace transform of circumferential strain–time curve
θ Circumferential strain
x Uniaxial strain
G Relaxation modulus or relaxation viscoelastic function
G0 Instantaneous shear modulus
G̃ Laplace transform of the shear viscoelastic function
gi Prony series parameter for shear relaxation function
h Indentation depth
h0 Constant indenation depth applied during indentation relaxation
hi Prescribed initial indentation depth
hr Prescribed final ramp depth
ji Prony series parameter for creep viscoelastic function
J Compliance or compliance viscoelasic function
J0 Instantaneous creep compliance
J˜ Laplace transform of the compliance viscoelastic function
K Bulk modulus or bulk viscoelastic function
K0 Instantaneous bulk modulus
K̃ Laplace transform of the bulk viscoelastic function
ki Prony series parameter for bulk viscoelastic function
ν Poisson’s ratio
P Indentation load
P0 Constant load applied during indentation creep
P̃ Laplace transform of load–time curve
r Strain gauge distance from the center of indentation
R Indenter radius
s Laplace variable
σx Uniaxial stress
t Time
τ and ξ Dummy variables for the time integral
τi Relaxation time of a Prony series branch
ūz Surface displacement
viii
List of Abbreviations
AFM Atomic Force Microscopy
BBR Bending Beam Rheometer
DSR Dynamic Shear Rheometer
DTT Direct Tension Tester
FEM Finite Element Method
LLDP Linear Low-Density Polyethylene
PC Polycarbonate
PDMS Polydimethylsiloxane
PMMA Poly(methyl methacrylate)
POM Polyoxymethylene
PVAc Polyvinyl Acetate
ix
Abstract
Instrumented indentation is a promising testing technique for obtaining the time

dependent viscoelastic properties of bitumen and bitumen-based mastics. It of-
fers several advantages: controlling the length scale of measurement and thus
could be used in multi-scale modelling of asphalt, the possibility of in-situ tests
and the minimal requirements of sample preparation. The measured viscoelastic
properties are of high importance to the established models of asphalt defor-
mation and fracture degradation with a direct effect on the cost and service
life of roads. Most of the viscoelastic indentation experiments and solutions
in the published literature assume a constant and known Poisson’s ratio and
use the relaxation indentation method, a method that applies a Heaviside step
function of indentation depth, this method introduces difficulties for low stiff-
ness materials with high relaxation rates such as bitumen. The goal of this
report is to develop a testing method capable of measuring two independent
viscoelastic functions while using a loading scheme, ramped load/depth, that
would alleviate the problems that plague the viscoelastic indentation of low
stiffness materials and specifically bitumen. The method of functional integrals
is used on the Hertz solution of the contact problem to obtain two indepen-
dent equations, the equations requires measurement of the load, indentation
depth and circumferential strain during indentation. non-linear regression is
performed on the two equations simultaneously to obtain the viscoelastic pa-
rameters. Numerical simulations are used to validate the obtained analytical
solutions and the effects of finite specimen size and strain measurement errors
are investigated. Polyoxymethylene (POM) is used as a model material to test
the developed technique. Indentation relaxation tests and indentation ramped
tests are performed on the material and the results are validated by uniaxial
tensile creep tests. The ramped indentation test results proved successful in
measuring the viscoelastic shear relaxation function, but with higher error at
the beginning of the test. The difficulties encountered during the tests are pre-
sented and analysed and their effects are projected and discussed upon using
the developed method on bitumen and bitumen–based mastics.
x
Acknowledgement
I would like to start by expressing my deepest gratitude to my supervisors,

associate professor Denis Jelagin and professor Per-Lennart Larsson for their
continuous, and detailed, guidance and feedback on every stage and aspect of
this master thesis. I would also thank them for their continuous motivation and
patience.
My sincere gratitude to Martin Öberg and Irene Linares Arregui for their
tremendous help in setting up and performing the experiments, for without their
help and experience achieving all of this would have been difficult.
My heartfelt thanks to my family, friends and colleagues who throughout
the period of the master program continued to support and encourage during
the happy and sad times.
Last but not least, I wholeheartedly express my sincere gratitude to the
Swedish Institute Scholarship for offering me this rare opportunity to undertake
a master programme in such a prestigious university and the chance to explore
a different environment and culture with all the necessary self–exploration and
self–development.
xi
Chapter 1
Introduction
Indentation tests are used extensively in characterizing materials in the scientific

and engineering applications due to their relatively experimental simplicity; ease
of sample preparation as well as the ability to perform multiple tests on the
same sample without destroying it. The recent technological advancements
opened up the possibility of using the indentation test to be valid for a wide
range of materials as described by Gouldstone et al. (2007), such as biological
materials, nano-materials and other materials with low stiffness such as bitumen
and mastics. These technological advancements enabled the recording of a wide
range of forces in the order of pico-Newtons and kilo-Newtons, and a wide range
of displacements.
Different shapes of indenters can be used for different applications, sharp
indenters i.e. Vickers and Berkovich are reliable for obtaining plastic material
properties and fracture toughness due to the high stress concentration under the
tip. Spherical and sphero-conical on the other hand can be used for obtaining
plastic or elastic material properties since they minimize the stress under the
indenter. The flat punch is also another kind of indenter that is used due to
the simplicity of the analytical formulation as a results of a constant and known
contact area, but the alignment of the indenter on the specimen remains one of
its biggest challenges together with the stress concentration at the boundaries
of contact. Figure 1 shows a photo of a commercial instrumented indentation
machine that is used for hardness testing.
Instrumented indentation, where the load and the indentation depth are con-
tinuously monitored, is a useful tool that can be used to extract the properties
of time dependent materials. But on the other hand, the interpretation of the
results of the test is a challenging task. This thesis aims to develop a method
to characterize two independent viscoelastic functions for the viscoelastic ma-
terials using spherical indentation. The thesis serves as a first step towards the
1
Figure 1: ZHU zwickiLine a commercial indenter for universal hardness testing
multi-scale characterization of bitumen and bitumen based materials.

The bitumen binder at high temperatures is generally considered a viscous
liquid, and at low temperatures it is mainly considered a viscoelastic mate-
rial and sometimes a viscoplastic material as described by Wang (2010). The
bitumen–based mastics are the mixtures of the bitumen and fillers, and they are
generally modeled with the same models as the bitumen binder, characterized
using the same tests Wang (2010).
The conventional methods of testing bituminous binders assumes the sample
to be a homogeneous linear viscoelastic material, although recent advances have
shown it to be an inhomogeneous material. Allen et al. (2013) have identified
three different phases within the binder. The widely used conventional methods
to characterize bitumen and bitumen–based mastics are the Dynamic Shear
Rheometer (DSR) and the Bending Beam Rheometer (BBR). In both the DSR
and BBR tests bitumen or mastic is assumed to be incompressible.
In the DSR test a sample from the binder or mastic is placed between a fixed
base plate and an oscillating plate. There are two types of DSR tests: controlled
stress and controlled strain. In the controlled stress tests a fixed applied torque
is applied to the oscillating plate while in the controlled strain test a fixed
oscillating frequency is applied and the resulting torque is measured, Wang
(2010). The DSR test can characterize both the viscous and elastic properties
of the specimens in the form of the complex shear modulus (G∗ ), and there
are established methods to transform it to the shear viscoelastic function in the
time domain.
In the BBR test a three-point bending specimen is created from the bitumen
2
or mastic sample and mounted on the BBR apparatus. The BBR apparatus is
used to measure the how much deflection or creeping the sample sustains at
a certain temperature. The beam theory is used to calculate the compliance
viscoelastic function, Wang (2010). An alternative to the BBR is the Direct
Tension Tester (DTT) which is basically a uniaxial tensile test for the sample.
The developed test would be able to measure the bitumen and bitumen–
based mastics viscoelastic properties across different length scales and temper-
ature with minimal changes on the experimental setup. The measuring across
different size scale will allow the advancement of the multi-scale modeling of bi-
tumen, mastic and asphalt as illustrated by Jäger, Lackner, and Stangl (2007)
in figure 2. The developed test has the ability to measure local and in situ of bi-
tumen viscoelastic properties, an advantage that the conventional bitumen and
mastics tests lack. An important benefit of this test is that the bitumen and
mastics properties measured can be incorporated into the asphalt deformation
and fracture degradation models that have a direct effect on the cost and service
life of designed roads.
Figure 2: Schematic of multi-scale modeling of bitumen, mastic and asphalt by

Jäger, Lackner, and Stangl (2007)
This thesis will start by exploring the state of the art published research,
in chapter 2, on the indentation of viscoelastic materials in general and then
narrows the focus on the bitumen and bitumen based materials indentation re-
search. In chapter 3 the formulas for two testing cases will be derived: controlled
depth test and ramp load test, that should be used in order to extract two in-
dependent viscoelastic functions form the test data. In chapter 4 numerical
simulations will be performed using finite element software, in order to mimic
the laboratory indentation test and re-calculate the independent viscoelastic
function using the solution methods derived in chapter 3. In addition, in chap-
ter 4 the effect of finite sample size and circumferential strain measurement
3
uncertainties will be explored.
In chapter 5 the results will be presented and described of the experimental
work performed on Polyoxymethylene (POM) samples. POM is used as a model
viscoelastic material to explore the possibility of applying the test on bitumen
and bitumen–based mastics samples. The reason for that is to bypass the re-
quirement of cooling and controlling the temperature of bitumen samples, that
would introduce additional uncertainties into the measurements. Performing the
experiments on POM would act as a verification of the developed method and
one step ahead in indentation testing of bitumen and bitumen–based mastics.
In chapter 6 the results obtained from the experiments will be thoroughly
discussed and their implications explored. The conclusions obtained form the
tests and their impact on bitumen and bitumen-based mastics are presented in
chapter 7.
4
Chapter 2
Literature Review
Indentation testing is a well-established method for measuring the elastic prop-

erties of linear–elastic isotropic materials. Recently, advances has been made
to extend its use to creeping and viscoelastic materials. The literature review
focuses on the most recent advances in the use of indentation techniques in the
mechanical characterization of viscoelastic materials in general and bitumen and
bitumen based materials in particular. The scope of the literature review is to
identify and group the published research according to the analytical formula-
tion of the indentation and subcategorize them according to the indenter type,
while noting if there are independent validation tests performed and their degree
of agreement with the performed test.
2.1 Indentation of Viscoelastic Materials

2.1.1 Indentation Creep/Relaxation with Constant Pois-
son’s Ratio
Explicit analytical expressions of the viscoelastic indentation problem can be
obtained by assuming the constancy of Poisson’s ratio while performing inden-
tation relaxation or indentation creep test. This is the approach used by Larsson
and Carlsson (1998) and VanLandingham et al. (2005).
Equations for this type of modelling as shown in the paper VanLandingham
et al. (2005) are shown in equations 1 and 2.
• Indentation creep: p
8h(t) A(t)
J(t) = √ (1)
3 π(1 − ν) × P0
5
• Indentation relaxation:
√
3 π(1 − ν)P (t)
G(t) = √ (2)
8h0 × A0
Larsson and Carlsson (1998) looked into the possibility of using the indentation
test to measure the viscoelastic functions of polymers. Analytical and experi-
mental analysis were performed for the flat-punch and spherical indenters on two
different kinds of polymers; an epoxy resin and PMMA. The authors indented
the test materials rapidly and kept the indentation depth constant to mimic a
relaxation test, while measuring the evolution of force in time and measuring
the residual imprint at the end of the test. They showed using FEM simulations
that the residual imprint can be measured well after the test before it recovers
fully. In addition the authors suggested using a strain gauge to measure the
evolution of the circumferential strain in order to measure two independent vis-
coelastic functions, they used this method on the flat punch indentation. The
authors used uniaxial relaxation tests to validate the indenation tests, the re-
ported errors for the flat punch indentation are shown in table 1. While the
error is 3.5% in the instantaneous shear modulus (G0 ) for ball indentation of
PMMA.
Table 1: Flat punch indentation validation error, Larsson and Carlsson (1998)
Material/Property G0 error (%) ν error (-)

Epoxy Resin 3.09 2.86
PMMA 1.72 2.27
VanLandingham et al. (2005) used rounded conical and Berkovich indenters

on epoxy, PMMA, filled and unfilled PDMS, the results are qualitatively similar
to validation tests performed using tensile rheometry techniques, but the values
for the time dependent shear modulus differed considerably from the validation
tests as shown in table 2. The authors attributed the large difference to several
reasons:
• Post-yield behaviour due to the concentrated stresses under the sharp

indenters.
• The dynamic model used to determine the indentation area did not take
damping into consideration.
• Difficulty of indenter-tip contact detection especially for PDMS.
• Tip–sample adhesion.
6
Table 2: Maximum validation errors for different materials, VanLandingham
et al. (2005)
Material/Property G(t) error (%)

Epoxy 70-80
PMMA 80
Filled PDMS 65-70
Unfilled PDMS 85-95
2.1.2 Lee and Radok’s Functional Integrals

The paper published by Lee and Radok (1960) is the seminal work that ex-
panded the Hertzian elastic solution of the contact problem into the viscoelastic
solution. The changing contact area boundary condition makes the correspon-
dence principle unsuitable to be used in this class of problems, but by using the
functional integrals a solution can be obtained. The functional integrals can
utilize any type of loading as long as the contact area does not decrease. The
method of functional integrals is used by Lu et al. (2003), Huang and Lu (2006),
and Oyen (2006). Equation 15 is a general equation for any kind of loading and
any model for the viscoelastic relaxation functions G(t) and K(t).
Lu et al. (2003) used two different types of indenters; namely Berkovich and
spherical indenters. The formulas used the functional integrals method while
assuming a constant Poisson’s ratio to simplify the calculations. Two polymers
were used for the research, PMMA and PC, and two loading schemes were used;
ramp loading and suddenly applied load that is kept constant for a period of time
(creep indentation). The paper also suggested monitoring the residual imprint
over a period of time and whether the imprint disappears or not decides whether
linearity has been achieved or not. For validation the authors used conventional
tension and shear tests on the polymers, the maximum reported errors in the
creep compliance are shown in table 3.
Table 3: Maximum validation errors for different materials and different

indenters, Lu et al. (2003)
Berkovich error (%) Spherical error (%)

Ramp load Step load Ramp load Step load
PMMA 3.9 5.4 0.9 7.8
PC 2.8 7.0 1.7 4.0
Huang and Lu (2006) used the functional integrals method in order to mea-
sure two independent viscoelastic functions; by using two different types of
indenters, one axis-symmetric while the other is not, to obtain two indepen-
dent equations solved simultaneously in a non-linear mean square minimization
7
for the all experimental points to obtain the independent viscoelastic functions.
The loading type used was ramp loading. The method of functional integrals
was used to obtain the analytical solutions for the viscoelastic indentation prob-
lem. For validation the authors used conventional tests results referenced from
other published literature, table 4 shows the average error difference between the
conventional tests and performed indentation tests for bulk and shear functions.
Table 4: Shear and bulk viscoelastic functions validation errors, Huang and Lu
(2006)
Material/Property G0 error (%) K0 error (%)

PMMA 2.64 9.54
PVAc 5.90 4.80
Oyen (2006) on the other hand derived an analytical solution for a com-
bination of ramp-creep test by controlling the load for both spherical and
Berkovich pyramidal indenters. The author used three different polymer ma-
terials: Polyurethane, PL-1 and PMMA. The validation utilized the material
properties of one of the loading conditions using spherical indenter to predict the
load–depth data of another loading condition of the Berokovich indenter, and
the error is the difference between the analytically predicted load–depth data
and the obtained data experimentally. Figure 3 shows the difference between the
predicted data, and the data obtained from the experiment for Polyurethane and
PL-1. The material parameters used in the predicted data are obtained using
spherical indentation, and the experimental data are obtained using Berkovich
indentation. The author attributes the large difference in the figure due to the
effects of plasticity introduced by the sharp tip of Berkovich indenter, which
should be explicitly included in the derivation of the analytical formulation of
the viscoelastic indentation problem. Another potential cause for the deviation
is the large strains induced by the sharp indenter.
8
Figure 3: Predicted and experimental results for Polyurethane (left) and PL-1
(right), Oyen (2006)
2.1.3 Other Methods

Some other authors like Giannakopoulos (2006) focused on the obtaining com-
putational expressions for pyramid indenters in the elastic case and managed
to extend the solution to the viscoelastic materials (utilizing a standard linear
solid with a single relaxation mechanism) under relaxation, creep and single step
recovery loads that simplified the viscoelastic solution and made the expressions
explicit. The author used a published experimental research on Vickers micro-
indentation of linear low-density polyethylene (LLDP). The author used two
times for comparison: the unrelaxed elastic modulus MU = E(t → 0) and the
relaxed elastic modulus MR = E(t → ∞). MU differed by 64.57% and MR
differed by 13.92%.
A research with the aim of including the finite specimen thickness to the
spherical indentation solution was performed by Qiang et al. (2011). The re-
search used two viscoelastic materials with various degrees of viscoelasticity and
used the relaxation test equation and combined it with a numerical expression
that accounts for the finite thickness. The authors concluded that the formula
proposed can only be used as an estimate for viscoelastic materials.
Another novel method is the dynamic indentation technique, that determines
the complex modulus (E ∗ ) components the storage (E 0 ) and loss (E 00 ) moduli.
The analytical treatment links the dynamic problem to the Hertzian contact
problem through two assumptions: the correspondence principle is applicable
and the sample damping is negligible compared to the loading frame. Some of
the published work about the viscoelastic dynamic indentation are performed
by Odegard, Gates, and Herring (2005) and Herbert, Oliver, and Pharr (2008),
in which Odegard, Gates, and Herring (2005) used Berkovich indenter tip and
reported a 30% error difference between the storage and loss moduli obtained
9
through nano–indentation and the conventional Dynamic Mechanical Analysis
(DMA). Herbert, Oliver, and Pharr (2008) on the other hand, used a flat punch
nano indenter and reported a 15% error between the nano–indentation and the
conventional DMA test.
2.2 Indentation of Bitumen and Bitumen-based

Materials
2.2.1 Indentation Creep/Relaxation with Constant Pois-
son’s Ratio
Several authors explored the simplified indentation problem with the assumption
of constant Poisson’s ratio and a constant load (indentation creep) or a constant
depth (indentation relaxation). Zofka and Nener-Plante (2011) and Jelagin and
Larsson (2013) are two researches that explored this method.
Zofka and Nener-Plante (2011) used flat punch indentation technique on as-
phalt binder specimens. The authors assumed a constant Poisson’s ratio. The
analytical method used is an explicit relation obtained by using indentation
creep. The authors started by performing FEM simulations that have resulted
in two conclusions; the friction effects are negligible, and the analytical solution
can capture the viscoelastic properties accurately. For validation BBR mea-
surements were compared to the creep indentation results, the best agreement
between the results happened at -9◦ C with an error of approximately 40%, at
-12◦ C and -6◦ C the errors registered were 70% and 100% respectively.
Jelagin and Larsson (2013), on the other hand, applied the spherical in-
dentation test on a bitumen specimen and assumed the bitumen material as
incompressible. The test was performed at 0◦ C in iced water. The type of
loading used is constant displacement after reaching a certain depth rapidly
(indentation relaxation). The indenter was painted and the indentation area
was measured after the test. Due to the constant contact area the viscoelas-
tic correspondence principle can be used directly. The results were validated
with measurements from DSR results. the error in G0 ranged from 3% to 41%
depending on the indenter size and the loading rate, the error at G(t → 50s)
ranged from 8% to 75%. The differences have been attributed to the assumption
on the Poisson’s ratio. A particular difficulty that has been emphasized in this
research, is that the high relaxation rate of the bitumen made the consideration
of machine compliance more difficult; for as the material relaxes the machine
then acts as a spring to push the indenter into the sample.
10
2.2.2 Lee and Radok’s Functional Integrals
Jäger, Lackner, and Eberhardsteiner (2007), Jäger, Lackner, and Stangl (2007),
and Veytskin, Bobko, and Castorena (2014) have utilized the functional integrals
in their bitumen and bitumen based mastics evaluations.
Jäger, Lackner, and Eberhardsteiner (2007) used the method of functional
integrals to transform the elastic solution into the viscoelastic one while taking
the real deforming geometry of the indenter into account. The authors used
different spring-damper models to represent the elastic and viscous behaviours
of the viscoelastic materials and by relating these parameters (shear modulus
and viscosity) to the force and indentation depth an analytical formula can be
obtained. By fitting the model parameters to the experimental data and per-
forming least square minimization the viscoelastic parameters can be obtained
numerically. The authors used bitumen type (B50/70) in Berkovich indenta-
tion test. Grid nano–indentation technique was used to get the morphology of
the bitumen in the micro–meter range as well as the ability to use statistical
methods to interpret the nano–indentation results. In addition, the authors also
explored the effect of loading rate and maximum load on the obtained param-
eters; concluding that the loading rate has no significant effect on the results
in contrast to the maximum load, where the authors have noted that the ob-
tained model parameters keep decreasing until they reach a limiting value. The
authors have not used an independent viscoelastic test results obtained using a
different methods to validate the obtained material properties. In their next pa-
per Jäger, Lackner, and Stangl (2007) further extended the research by utilizing
the grid indentation technique to identify the properties of the different phases
in the bitumen. The nano-indentation tests were performed at different loading
rates, maximum loads and temperature in order to investigate their effects. The
non-linear dash-pot model is used to describe the viscoelastic functions. Fig-
ure 4 and equations 3 and 4 show the model used by the authors; where F (t)
is a function that depends on the geometric properties, Ȳ is the viscoelastic
function, Ja and k are the model parameters.
Figure 4: non-linear dash-pot model, Jäger, Lackner, and Stangl (2007)
11
Z t
dP (τ )
F (t) = Ȳ (t − τ ) (3)
0 dτ
k !
1 t
Ȳ (t) = Ja (4)
4 τ̄
Depending on the temperature range, the authors used DSR and BBR to
validate the results. At approximately 0◦ C the error difference in Ja is about
40% as shown in figure 5.
Figure 5: Validation of nano-indentation results, Jäger, Lackner, and Stangl

(2007)
Veytskin, Bobko, and Castorena (2014) explored the nano-indentation tech-

nique using a sphero-conical indenter on two asphalt binders and one mastic at
room temperature. The Poisson’s ratio was assumed as constant. The func-
tional integrals were used to obtain the analytical solution, and the material
is assumed to follow the generalized power law. A large number of tests were
performed and test results of each material were averaged, the properties were
acquired and compared to relaxation moduli obtained from the DSR tests, the
comparison between the nanoindention results and DSR are shown in in figure 6.
2.2.3 Other Methods

Ossa, Deshpande, and Cebon (2005) expanded the power law creep from uni-
axial problems to their multi-axial counterparts in order to use in the viscoelastic
spherical–half space contact problem. In their analytical analysis the authors
separated the power law creep constitutive relation into two components, a vis-
cous part and a recovery part. The solution was simplified into an equivalent
rigid flat punch indentation into a non-linear elastic solid based on the observa-
12
Figure 6: Validation of nano-indentation results, Veytskin, Bobko, and
Castorena (2014)
tion that the stress and strain fields under the indenter are self-similar. Different
types of loading were used. The comparison between the analytical solution and
the experiments showed close agreement at the beginning of the test but they
started to diverge in the later parts of the time domain, the maximum error
between the measured and predicted force is 12.5% to 13.5% in the considered
time frame. No independent validation test was used. Ossa and Collop (2007)
further expanded the application of the formulas to asphalt mixtures to good
agreement between the experiments and the predicted analytical solution. The
downside to this analysis is the requirement to assume the bitumen as a power
law creeping solid with no flexibility to test other models.
Hamzaoui, Guessasma, and Bennabi (2013) did not use analytical solutions
to calculate the viscoelastic functions from indentation readings, but instead
the authors have used FEM simulations with varying model parameters in or-
der to fit the results with the experiments. Prony series parameters with one
summation term were used as a model for the functions with Poisson’s ratio
assumed as a constant. the authors used flat punch indentation technique on
asphalt binder specimens. The authors observed non-linear effects for the higher
loads and higher temperatures, while low loads have also resulted in incorrect
measured quantities; the authors attributed that due to the contact conditions,
friction forces or low resolution measurement error. There were no independent
validation tests performed on the bitumen. A severe limitation of this method
is the computational cost required to fit the parameters especially if more Prony
series summation parameters were used.
Allen et al. (2013) used the atomic force microscopy (AFM) technique to
13
obtain semi-quantitative values of the asphalt binder properties. The authors
identified three phases within the bitumen, for each one the phases the relaxation
modulus was calculated. The authors used the composite theory to calculate
the lower and upper bounds of the bulk binder material properties.
14
Chapter 3
Analytical Solutions
From reviewing the current literature, the bitumen and bitumen-based inden-
tation testing have two proposed loading schemes:
1. Relaxation indentation test: the machine will be used in displacement

control. The indenter will be pressed into the material rapidly until it
reaches a prescribed depth whence it will be held constant.
2. Ramped test: the machine will be operated in either load control or

displacement control where the load or displacement will be increased
linearly to prescribed value respectively.
The analytical manipulation required for each type of loading varies sig-
nificantly; for the relaxation indentation test the viscoelastic functions can be
obtained directly from the correspondence principle, while the ramp loading
scheme requires the use of the more convoluted method of functional integrals
developed by Lee and Radok (1960).
The experiments will use a spherical indenter to alleviate the difficulties en-
countered on other indenter types; sharp indenters will always introduce plas-
ticity and flat indenters introduce singular stress field leading to plastic defor-
mations at higher loads.
3.1 The Linear elastic solution

The analytical solutions for a sphere contact with a linear elastic half space have
been derived in detail in the classic book of contact mechanics, Johnson (1985).
The load–indentation depth and circumferential strain equations will be used
to obtain two independent viscoelastic functions. The derivations are shown in
Appendix A, and figure 7 shows a schematic of the indentation process with the
main variables involved in the analysis.
15
Figure 7: A schematic of the indentation showing relevant parameters
The independent equations are:
8 Ga3
P = (5)
3 (1 − ν) D
1 (2 ν − 1) P
θ (r) = (6)
4 πr2 G
Where: r
D
a= h (7)
2
and:
3K − 2G
ν= (8)
6K + 2G
By substituting equations 7 and 8 into 5 and 6, and utilizing D = 2R the
following final formulae are obtained:
8 √ 3KG + G2

P = R × h3/2 (9)
3 (3K + 4G)
3 P
θ (r) = − (10)
4 π r2 (3 K + G)
16
3.2 Relaxation indentation test
The relaxation indentation test is obtained by applying the correspondence prin-
ciple to 9 and 10, the Laplace transformed equations are:

8√ sG̃ 3K̃ + G̃ h
3/2
P̃ = R× × o (11)
3 3K̃ + 4G̃ s
3 P̃
˜θ (r) = − (12)
4 π r2 3 K̃ + G̃ × s
h3/2
While L(h3/2 ) = o
s has been utilized since h = ho is constant during the
test and the tilde (˜) symbol above the variables denotes the Laplace transform
of these parameters.
The steps required to obtain the relaxation functions are as follows:
• The recorded P and θ data are fitted into a four terms Prony series
• Laplace transform of P and θ into P̃ and ˜θ .
• The Laplace domain relaxation functions, G̃ and K̃, are obtained from
solving 11 and 12 simultaneously.
• The relaxation functions in the time domain are obtained by perform-

ing inverse Laplace transform of G̃ and K̃ numerically using the Talbot
algorithm.

L−1 G̃ = G

L−1 K̃ = K
3.3 Ramp test

Rearranging equations 11 and 12 respectively the following expressions are ob-
tained:
h i √ h i
3K̃ + 4G̃ s × P̃ = 8 R G̃ × s × K̃ s × h3/2
8√ h i (13)
+ R G̃ × s × G̃ s × h3/2
3
h i
−3G̃ s × P̃ = 4πr2 G̃ × s × G̃ [s × ˜θ ]
(14)
+12πr2 G̃ × s × K̃ [s × ˜θ ]
By recognizing that the inverse Laplace of the terms multiplied by the

Laplace variable s is the convolution integral:
17
h i R
t
L−1 B s × Ã = 0 B(t − τ ) dA
dτ dτ
Taking the inverse Laplace of 13 and 14 give respectively:

Z t Z t
dP (τ ) dP (τ )
3 K(t − τ ) dτ + 4 G(t − τ ) dτ
0 dτ 0 dτ
√ Z t
Z τ
dh3/2 (ξ)

d
=8 R G(t − τ ) K(τ − ξ) dξ dτ (15)
0 dτ 0 dξ
√ Z t Z τ 3/2

8 d dh (ξ)
+ R G(t − τ ) G(τ − ξ) dξ dτ
3 0 dτ 0 dξ
Z t
dP (τ )
−3 G(t − τ ) dτ
0 dτ
Z t Z τ
d dθ (ξ)
= 4πr2 G(t − τ ) G(τ − ξ) dξ dτ (16)
0 dτ 0 dξ
Z t Z τ
d dθ (ξ)
+12πr2 G(t − τ ) K(τ − ξ) dξ dτ
0 dτ 0 dξ
The steps required to obtain the relaxation functions are as follows:
• The recorded P , h3/2 and θ data are fitted into a polynomial function.
If P , h3/2 and θ cannot be fitted by a suitable polynomial the following
alternative way should be performed:
– Each part of P , h3/2 and θ is separated into equal time intervals

that are fitted individually into a polynomial.
– The slope of each section is found by differentiating the polynomial.
– The slope function is fitted back again into a Prony series form.
• The viscoelastic functions G and K are expressed in the Prony series

terms: !
n
X
−t/τi
G(t) = G0 × 1− gi × 1 − e (17)
i=1
n
!
X
−t/τi
K(t) = K0 × 1− ki × 1 − e (18)
i=1
• Equations 15 and 16 are obtained in a symbolic form, by substituting

dP (τ )
the polynomial forms for P , h3/2 and θ , or their slopes instead of dτ ,
3/2
dh (ξ) dθ (ξ)
dξ and dξ , and the Prony series forms of G and K to create the
two independent and time dependent constitutive relations.
• The two independent equations are solved for all data points in a non-
linear square fit to obtain the Prony series parameters that represent the
material.
18
Chapter 4
Validation of Analytical
Solutions Using Simulations
In order to validate the analytical solutions simulations were performed to vali-

date at first the elastic solution upon which the relaxation and ramp load equa-
tions are based, and then the simulations are expanded to cover the viscoelastic
constitutive equations. The main goal of the simulations was to back-calculate
the properties that has been used as an input to the finite elements simulation.
4.1 Models Overview

All the models incorporated axis-symmetry to save on the computational time.
The half space was modelled as a rectangle with 8-nodes two dimensional axis-
symmetric elements using ANSYS’s PLANE183 elements. The mesh used has
been divided into three zones with different element sizes; the first and most
dense zone is at the location where the indentation takes place, the second
zone is where the surface circumferential strain measurement should be taken
and it is less dense than the first zone, the third zone is coarse meshed to act
as extra material to mimic the behaviour of the infinite half space. For all the
meshed zones the size of the elements increases as the distance from the indenter
increases.
The indenter was modelled as a quarter circle with the same type of elements,
but the degrees of freedom of all the nodes on its surface were constrained to have
the same value and thus the indenter behaves as a rigid body. The geometry
and boundary conditions are shown in figure 8, a zoomed in view of the mesh
is shown in figure 9, and a zoomed in figure of the indented geometry is shown
in figure 10.
19
The model used indenter radius R of 12.7 mm, the half space size from the
center of the indentation to the edge is equal to 200 × R to avoid any edge
effects.
Figure 8: The geometry and boundary conditions used in the analysis,

geometry to half-space scale is changed for illustration purposes
20
Figure 9: The zoomed-in view of the mesh and the different zones used
Figure 10: A plot showing the indented geometry with 26 elements in contact
4.1.1 Indentation Relaxation Test

To model the indentation relaxation test a prescribed displacement ho was ap-
plied on top of the rigid indenter. The relaxation test is modelled in two stages;
21
in the first stage the half space was modelled as an elastic material and the
displacement is increased linearly from zero to the prescribed value, in the sec-
ond stage the displacement is kept at the prescribed value after changing the
material of the half space into a viscoelastic material with the desired properties.
The controlled displacement was kept for 50 seconds with 5000 data points to
cover the time period. At each data point the summation of the reaction forces
was recorded as the value of the indentation load as well as the displacement
and the circumferential strain at a surface point chosen at a large distance from
the indentation area; in order to be far enough from the local effects of the
indenter as well as far away from the boundaries.
4.1.2 Indentation Ramped Load Test

To model the indentation ramped load test a prescribed pressure was applied on
the top of the indenter quarter circle and the load is increased linearly from zero
to the prescribed pressure value. In this model the half space material model is
viscoelastic from the beginning.
Similarly, 5000 data points were used where the indentation load, depth and
surface circumferential strain, at a large distance from the indentation area, has
been recorded.
4.2 Back-Calculation of the Viscoelastic Func-

tions from Model Data
This section pertains to the results obtained from the simulation and comparing
the obtained properties from the analysis with the properties used in the model.
4.2.1 Indentation Relaxation Test

The material used a four terms Prony series for the indented half space:
h
G(t) = G0 × 1 − g1 × 1 − e−t/τ1 − g2 × 1 − e−t/τ2
i
− g3 × 1 − e−t/τ3 − g4 × 1 − e−t/τ4
h
K(t) = K0 × 1 − k1 × 1 − e−t/τ1 − k2 × 1 − e−t/τ2
i
− k3 × 1 − e−t/τ3 − k4 × 1 − e−t/τ4
Where:
G0 = 82 M P a K0 = 792.6667
g1 = 0.447 g2 = 0.288 g3 = 0.165 g4 = 0.073
22
k1 = 0.150 k2 = 0.120 k3 = 0.100 k4 = 0.098
τ1 = 0.017 τ2 = 0.165 τ3 = 1.310 τ4 = 11.400
The load and circumferential strain are shown in figure 11 and 12, for both
the obtained data and the fitted data.
The viscoelastic shear relaxation function G(t), bulk relaxation function
K(t) and time-dependent Poisson’s ration ν(t) are shown in 13, 14 and 15
respectively, and the percentage error between the back-calculated and input
parameters is shown in figures 16 and 17.
50
Data Points
45 Fit Function
40
35
30
P (N )
25
20
15
10
0
0 5 10 15 20 25 30 35 40 45 50
time (s)
Figure 11: Relaxation load
23
0
-0.5
-1
ǫθ (t) × 106
-1.5
-2
-2.5
-3
Data Points
Fit Function
-3.5
0 5 10 15 20 25 30 35 40 45 50
time (s)
Figure 12: Relaxation circumferential strain
Shear Relaxation M odulus

90
Obtained
80 Input
70
60
G (M P a)
50
40
30
20
10
0
0 5 10 15 20 25 30 35 40 45 50
time (s)
Figure 13: The shear viscoelastic function (relaxation test)
24
Bulk Relaxation M odulus
2200
Obtained
2000 Input
1800
1600
K (M P a)
1400
1200
1000
800
600
0 5 10 15 20 25 30 35 40 45 50
time (s)
Figure 14: The bulk viscoelastic function (relaxation test)
ν(t)
0.5
0.495
0.49
ν
0.485
0.48
obtained
input
0.475
0 5 10 15 20 25 30 35 40 45 50
time(s)
Figure 15: The time dependent Poisson’s ratio (relaxation test)
25
V iscoelastic F unctions Error
0.7
G-error
ν-error
0.6
0.5
P ercentage error (%)
0.4
0.3
0.2
0.1
0
0 5 10 15 20 25 30 35 40 45 50
time (s)
Figure 16: The error in the viscoelastic functions (relaxation test)
V iscoelastic Bulk F unction Error

30
25
20
15
10
0
0 5 10 15 20 25 30 35 40 45 50
time (s)
Figure 17: The error in the viscoelastic bulk function (relaxation test)
26
4.2.2 Indentation Ramped Load Test
Similarly to the previous section, The load, slope of square–root of cubed depth
and slope of circumferential strain are shown in figures 18, 19 and 20. While
the viscoelastic functions are shown in figures 21, 22 and 23. The percentage
error between the back-calculated and input parameters is shown in figures 24
and 25. It is worth noting that the error in the viscoelastic bulk relaxation
function is larger that the other functions due to the fact the the material is
almost incompressible.
The material used a one term Prony series for the indented half space:
G(t) = G0 × 1 − g1 × 1 − e−t/τ1

K(t) = K0 × 1 − k1 × 1 − e−t/τ1

Where:
G0 = 82 M P a g1 = 0.8, K0 = 792.6667 M P a k1 = 0.6

τ1 = 0.6
10
6
P (N )
0
0 5 10 15 20 25 30 35 40 45 50
time (s)
Figure 18: The ramped load
27
×10-4
-1
Data Points
Fit Function
-2
-3
-4
dh3/2 (t)
dt
-5
-6
-7
-8
0 5 10 15 20 25 30 35 40 45 50
time (s)
Figure 19: Slope of square–root of cubed depth
×10-8
-3
Data Points
Fit Function
-4
-5
-6
dǫθ (t)
dt
-7
-8
-9
-10
0 5 10 15 20 25 30 35 40 45 50
time (s)
Figure 20: Slope of circumferential strain
28
Shear Relaxation M odulus
90
Obtained
80 Input
70
60
G (M P a)
50
40
30
20
10
0 5 10 15 20 25 30 35 40 45 50
time (s)
Figure 21: The shear viscoelastic function (ramp test)
Bulk Relaxation M odulus

900
Obtained
Input
800
700
K (M P a)
600
500
400
300
0 5 10 15 20 25 30 35 40 45 50
time (s)
Figure 22: The bulk viscoelastic function (ramp test)
29
ν(t)
0.475
obtained
input
0.47
0.465
ν
0.46
0.455
0.45
0 5 10 15 20 25 30 35 40 45 50
time(s)
Figure 23: The time dependent Poisson’s ratio (ramp test)
V iscoelastic F unctions Error

0.5
G-error
0.45 ν-error
0.4
0.35
0.3
0.25
0.2
0.15
0.1
0.05
0
0 5 10 15 20 25 30 35 40 45 50
time (s)
Figure 24: The error in the viscoelastic functions (ramp test)
30
V iscoelastic Bulk F unction Error
4.5
3.5
2.5
1.5
0.5
0
0 5 10 15 20 25 30 35 40 45 50
time (s)
Figure 25: The error in the viscoelastic bulk function (ramp test)
31
4.3 Effect of Finite Specimen Dimensions
The solutions obtained for the viscoelastic contact problem apply to infinitely
large samples. Applying the same equations to a real sample with a finite size
would introduce errors. These errors have been estimated by obtaining the shear
relaxation function and the bulk viscoelastic function for models with a different
size. The results are represented in figure 26.
Shear Relaxation F unction V iscoelastic Bulk F unction

1.2 50
45
1
40
35

0.8
30
0.6 25
20
0.4
15
10
0.2
5
0 0
0 50 100 150 200 0 50 100 150 200
Indentation Radius/Distance to Edge Indentation Radius/Distance to Edge
Figure 26: The errors obtained in the calculation of the viscoelastic functions
vs. the quotient of the contact radius to the distance from the center of
contact to the sample edges
4.4 Effect of Errors in Strain Measurement

A number of factors could affect the strain measurement; the strain gauge align-
ment, the accuracy of distance measurement to the strain gauge and also the
effect of averaging the strain over an area. The strain represented in the equa-
tions is a point strain which is impossible to obtain experimentally, so in the
case of using strain gauges the gauge will cover a distance of a few millimetres
and outputs an averaged value.
The effect of errors in θ is investigated analytically and the results are shown
in figure 27.
32
Average V iscoelastic F unctions Errors
30
G(t)
K(t)
ν(t)
25
20
15
10
0
0 2 4 6 8 10 12 14 16 18 20
ǫθ error (%)
Figure 27: The errors in the obtained viscoelastic functions due to errors in
strain measurement
33
Chapter 5
Experimental Tests
To validate the method used, a tensile test will be firstly performed on the POM
samples and extract two independent viscoelastic functions. The results from
the tensile tests will be compared to the indentation of the POM samples using
the method developed in this thesis.
5.1 Tensile Test on POM Samples

Three tensile test POM samples have been prepared, the samples shape and
dimensions can be seen in figure 28 with the smallest diameter for each speciment
is shown in table 5. The test is performed on three maximum stress levels: 20,
15 and 10 MPa approximately. The stress levels has been chosen to be less or
equal than 20 MPa so as to avoid the deviation from linear viscoelasticity, as
suggested by the experimental investigations on POM samples of Starkova and
Aniskevich (2007).
The tests goals are to measure the viscoelastic relaxation function and the
Poisson’s ratio simultaneously, but due to the testing equipment limitations
either the axial strain x or the circumferential strain θ has to be measured
separately; thus the performed tests are separated into the viscoelastic relax-
ation function tests and Poisson’s ratio tests.
Figure 28: The uniaxial creep test sample
34
Table 5: Smallest diameter du for each uniaxial test sample
Sample No. du (mm)

1 5.03
2 5.01
3 5.00
5.1.1 The Experimental Setup

An INSTRON load frame is used for the the experimental setup, as shown in
figure 29. An INSTRON extensometer is used with gauge length of 12.5 mm
that can measure up to 20% strain. An INSTRON load cell is used to measure
the load with a dynamic rating of ±2 kN.
Figure 29: The uniaxial creep test experimental setup
Figure 30: The strain gauge on the uniaxial creep sample
The specimens’ smallest diameter is measured using a digital caliper. Be-

fore mounting the specimens the load cell was calibrated using the automated
35
command on the load frame’s software, after that one specimen at a time was
mounted on the load frame using uniaxial test fixtures.
For measuring the viscoelastic relaxation function, the extensometer was
mounted on the specimen as in figure 29, and the load frame was controlled
manually until at least a force of one newton was recorded by the load cell.
The Specimens were tested in uniaxial creep by assigning the constant loads of
400, 300 and 200 Newtons that approximately correspond to the pre-determined
stress levels, at each load level the specimen creep (i.e. the strain) was measured
in the time domain. Due to the load frame limitations the load was applied from
zero to the specified level in approximately 0.86 seconds to mimic a Heaviside
step function. Each specimen was tested at least two times at each load level
for 15 minutes and allowed to recover the strain in 25 minutes. The recovery
period has been determined after recording the amount of time required for the
extensometer to record approximately zero strains.
As for measuring the Poisson’s ratio, the extensometer was changed with a
5 mm strain gauge glued around the specimen circumference as in figure 30.
The Specimens were tested in uniaxial creep by assigning the constant loads
of 400 and 200 Newtons. The procedure then followed the same steps used for
measuring the viscoelastic relaxation function but the circumferential strain was
recorded instead of axial strain.
5.1.2 Mathematical Formulation

The creep compliance function can be determined directly for the creep test,
the uniaxial test stress is given using the following equation:
P 4P
σx = = (19)
Au πd2u
For uniaxial creep the constant stress is related to the strain by the creep
compliance function:
x (t)
J(t) = (20)
σx
The relaxation function can be obtained from the creep compliance function
by using the correspondence principle as in equation 21.

1
E(t) = L−1 (21)
˜
s2 × J(s)
The Poisson’s ratio is calculated from the axial strain and the circumferential
strain as follows:
36
˜θ
s × ν̃ = − (22)
˜x

−1 ˜θ
ν(t) = L − (23)
s × ˜x
5.1.3 Experimental Results

The direct recordings from the tensile test are the load, axial strain and cir-
cumferential strain. The load is converted to stress using equation 19, the creep
compliance is obtained using equation 20 and the Poisson’s ratio is obtained
using equation 23. An example of the obtained axial stress, axial strain and
circumferential strain are shown in figures 31, 32 and 33. The obtained creep
compliance is shown in figure 34.
Axial Stress
16
14
12
10
σx (M P a)
0
0 100 200 300 400 500 600 700 800 900 1000
time (s)
Figure 31: The axial stress for sample 3 at 15 M P a load level
Using equation 21 on the data collected from the creep test yielded the
following relaxation function:
h
E(t) = E0 × 1 − e1 × 1 − e−t/τ1 − e2 × 1 − e−t/τ2
i (24)
− e3 × 1 − e−t/τ3 − e4 × 1 − e−t/τ4
Where:
37
Axial Strain
0.6
0.5
0.4
ǫx (%)
0.3
0.2
0.1
0
0 100 200 300 400 500 600 700 800 900 1000
time (s)
Figure 32: The axial strain for sample 3 at 15 M P a load level
×10-3 Circumf erential Strain

3.1
2.9
2.8
ǫθ (%)
2.7
2.6
2.5
2.4
0 100 200 300 400 500 600 700 800 900 1000
time (s)
Figure 33: The axial strain for sample 3 at 20 M P a load level
38
Creep Compliance F unction
0.037
0.036
0.035
0.034
J ( MP a)
1
0.033
0.032
0.031
0.03
0.029
0 100 200 300 400 500 600 700 800 900
time (s)
Figure 34: The creep compliance for sample 3 at 15 M P a load level
E0 = 3366 M P a
e1 = 0.077 e2 = 0.053 e3 = 0.042 e4 = 0.038
τ1 = 609.4 τ2 = 80.3 τ3 = 15.6 τ4 = 2.5
Using equation 23 on the data collected from the creep test yielded the
following Poisson’s ratio:
h
ν(t) = ν0 × 1 − ν1 × 1 − e−t/τ1 − ν2 × 1 − e−t/τ2
i (25)
− ν3 × 1 − e−t/τ3 − ν4 × 1 − e−t/τ4
Where:
ν0 = 0.3973 M P a
ν1 = 0.0274 ν2 = 0 ν3 = 0.0047 ν4 = 0.0217
τ1 = 609.4 τ2 = 80.3 τ3 = 15.6 τ4 = 2.5
Figures 35 and 36 show the average relaxation function and Poisson’s ratio
for POM graphically with a 95% confidence interval.
Results from individual tests are presented in appendix B.
39
E(t)
3500
3400
3300
3200
E(M P a)
3100
3000
2900
2800
2700
2600
-200 0 200 400 600 800 1000
time(s)
Figure 35: The relaxation function for POM
P oisson′ s ratio
0.42
0.41
0.4
ν (−)
0.39
0.38
0.37
0.36
0.35
0 100 200 300 400 500 600 700 800 900
time (s)
Figure 36: The Poisson’s ratio for POM
40
5.2 Indentation Tests on POM Samples
A cubic POM sample was prepared from the same batch as the uniaxial test
sample, with dimensions of 7 x 7 x 7 cm. The surface was initially ground using
fine sandpaper and then using a super fine ISO P1200 sandpaper. Two kinds
of tests were performed, relaxation indentation test and ramped displacement
test.
5.2.1 The Experimental Setup

A hydraulic INSTRON load frame was used for the indentation tests, shown in
figure 37. A load cell of 50 kN is the default cell of the load frame and it is used
throughout the tests.
For the measurement of Poisson’s ratio a half-bridge strain measurement
setup was used with two 5 mm active strain gauges, shown in figure 38. The
strain gauges were aligned so as to give the average value of the circumferential
strain of an indentation performed in the middle of the space between them.
For the indentation relaxation tests, four indentation depths were performed
(with five tests at each depth) that represent different load levels in order to
probe the material’s stress dependent behaviour. The final depth was applied
in 0.2 milliseconds and approximately a pseudo-Heaviside step function loading
was performed. The depth was kept constant for 10 minutes and the reaction
load and circumferential strain were monitored for the duration. Table 6 shows
the depths used and whether the strain gauges were used in that test or not.
As for the ramped displacement tests, a certain loading scheme was used:
indenting until a prescribed initial depth hi and allowing the material to relax
while keeping the depth constant, and then ramping the depth from hi to a
final prescribed depth hr . The initial indentation depth is used to minimize the
uncertainties involved in measuring at very small depths: uncertainties related
to the surface roughness and measuring equipment accuracy at very low values.
Table 7 shows the initial and final depths used in the tests, five tests were
performed at each loading configuration.
Table 6: Depths used in the indentation relaxation test
Depth (µm) Strain gauge usage

40 Yes
50 No
60 No
70 Yes
41
Figure 37: The indentation tests setup
Figure 38: The strain gauges glued to the POM specimen
Table 7: Depths used in the indentation ramped test
hi (µm) hr (µm)
20 50
30 60
42
5.2.2 Machine Compliance
To measure the compliance of the testing setup and approximate method was
used. An indentation was performed on a high strength steel specimen with the
fully assembled indenter setup, with the assumption that the high strength steel
specimen deformation is negligible then all the recorded displacement could be
attributed to the testing machine. Only the unloading curve was considered to
mitigate any effects of plastic deformation. The unloading load-depth curve for
the machine is shown in 39, fitted with a linear equation.
All the obtained indentation depth results are then corrected by subtracting
the amount of machine displacement that corresponds to the applied load.
Load − Displacement Curve (T esting Setup)

12
10
6
h (µm)
2
Data
Fit
0
-2
0 50 100 150 200 250 300 350 400
Load (N )
Figure 39: Load displacement curve for the testing machine
5.2.3 Relaxation Indentation Tests Results

The direct recording from the relaxation indentation tests are the load, inden-
tation depth and axial strain. Equations 11 and 12 can be applied directly and
solved simultaneously with the assumption of constants Poisson’s ratio/Bulk
viscoelastic function; this assumption has been used due to the noisiness of the
strain gauge measurements and the difficulty of obtaining a strain chan. Exam-
ples of the obtained load, indentation depth and axial strain are shown in fig-
ures 40, 41 and 42.
As previously mentioned, only indentations at depths 40 µm and 70 µm
43
Indentation Load
75
70
65
Load (N )
60
55
50
45
0 100 200 300 400 500 600
time (s)
Figure 40: Load change in time during the relaxation indentation test
Indentation Depth
43
42
41
h (µm)
40
39
38
37
0 100 200 300 400 500 600
time (s)
Figure 41: Indentation depth change in time during the relaxation indentation
test
have been performed with strain measurements. The distance from one strain
gauge to the indent has been measured using a microscope to be 6.7873 mm.
44
Axial Strain
-19
-20
-21
ǫx (microstrain)
-22
-23
-24
-25
-26
-27
0 100 200 300 400 500 600
time (s)
Figure 42: Strain change in time during the relaxation indentation test
For each indentation depth 5 tests were performed and averaged, figure 43
shows the averaged results of the shear relaxation modulus for each indentation
depth together with the result from the uniaxial tensile test.
Figure 44 shows the averaged shear relaxation modulus between all tests
except the test at 70 µm; due to its clear deviation from the linear viscoelasticity
regime. The error bars represent a 95% confidence interval. A comparison
between the shear relaxation modulus obtained from the indentation relaxation
test and the uniaxial test is shown in figure 45 and the calculated difference
error is shown in figure 46.
The mean shear relaxation modulus obtained follows the following function:
h i
G(t) = G0 × 1 − g1 × 1 − e−t/τ1 − g2 × 1 − e−t/τ2 (26)
Where:
G0 = 1297 M P a
g1 = 0.1260 g2 = 0.2152 τ1 = 27.35 τ2 = 273.50
The obtained Poisson’s ratio for the 40 µm and 70 µm is averaged and

evaluated as 0.4459. Compared to Poisson’s ratio obtained from the uniaxial
tensile test (averaged over time as 0.4129) it has an error of about 8%.
Results from individual tests are presented in appendix B.
45
Indentation Relaxation T est
1700
40 µm
1600 50 µm
60 µm
1500 70 µm
Uniaxial
1400
1300
G (M P a)
1200
1100
1000
900
800
700
0 100 200 300 400 500 600
time (s)
Figure 43: Shear relaxation modulus obtained at different depths for the
indentation relaxation test
M ean Shear Relaxation M odulus

1500
1400
1300
1200
G (t)
1100
1000
900
800
700
-100 0 100 200 300 400 500 600 700
time (s)
Figure 44: Averaged shear relaxation modulus for the indentation relaxation
test with 95% confidence interval
46
1350
Indentation Relaxation Test
1300 Uniaxial Creep Test
1250
1200
1150
G (t)
1100
1050
1000
950
900
850
0 100 200 300 400 500 600
time (s)
Figure 45: Averaged shear relaxation modulus from indentation relaxation

compared to uniaxial creep test
47
P ercentage Dif f erence Between the U niaxial and Indentation Relaxation T ests
12
10
8
P ercentageerror(%)
0
0 100 200 300 400 500 600
time(s)
Figure 46: Difference error between shear relaxation modulus from indentation
relaxation and the uniaxial creep test
48
5.2.4 Ramped Indentation Tests Results
The direct recording from the ramped indentation tests are the load and in-
dentation depth. Due to the inaccuracy of the used strain gauges the strain
measurement was not used. This allowed the freedom to indent on any surface
of the specimen. The average bulk modulus function value obtained from the
uniaxial tests was used and considered a constant value. Equation 15 is used
to obtain the the viscoelastic parameters of the shear relaxation modulus. Two
Prony series parameters were used to describe the shear relaxation function;
and thus the non-linear regression has to obtain five parameters that would
minimize the equation. Examples of the obtained load and indentation depth
are shown in figures 47 and 48.
Indentation Load
80
70
60
Load (N )
50
40
30
20
10
0 100 200 300 400 500 600
time (s)
Figure 47: Load change in time during the ramped indentation test
As described previously, for each indentation depth 5 tests were performed

and averaged, figure 49 shows the averaged results of the averaged shear relax-
ation function obtained using the ramped test together with the results from
the indentation relaxation test and the uniaxial test.
Figure 50 shows the averaged shear relaxation modulus with error bars rep-
resenting a 95% confidence interval. The difference error between the shear
relaxation modulus obtained from the indentation ramped test and the uniaxial
test is shown in figure 51.
49
Indentation Depth
55
50
45
40
h (µm)
35
30
25
20
15
0 100 200 300 400 500 600
time (s)
Figure 48: Indentation depth change in time during the ramped indentation
test

2200
Indentation Ramped Test
Indentation Relaxation Test
2000
Uniaxial Creep Test
1800
1600
G (t)
1400
1200
1000
800
0 100 200 300 400 500 600
time (s)
Figure 49: Averaged shear relaxation modulus from indentation ramped test
compared to the indentation relaxation and uniaxial creep tests
The mean shear relaxation modulus obtained follows equation 26 where:
50
G0 = 2025 M P a
g1 = 0.3475 g2 = 0.2754 τ1 = 24.28 τ2 = 305.90

3000
2500
2000
G (t)
1500
1000
500
-100 0 100 200 300 400 500 600 700
time (s)
Figure 50: Averaged shear relaxation modulus for the indentation ramped test
with 95% confidence interval
51
P ercentage Dif f erence Between the U niaxial T est and Indentation Ramped T ests
90
80
70
60
P ercentageerror(%)
50
40
30
20
10
0
0 100 200 300 400 500 600
time(s)
Figure 51: Difference error between shear relaxation modulus from indentation
ramped test and the uniaxial creep test
52
Chapter 6
Discussion
6.1 Analytical Solutions

As it is evident from chapter 3, the derived solutions for both the relaxation
indentation and ramped indentation tests can capture the viscoelastic functions
accurately. In practice, however, uncertainty in the measurements is expected
to affect the calculated viscoelastic parameters. This has been investigated
especially for the uncertainty in the measurement of circumferential strain and
the effect of finite sample size.
From figure 27 it is apparent that the uncertainty affects the calculation
of the bulk viscoelastic function much more that it affects the shear relaxation
modulus. But it can also be observed that a relatively large error in K(t) results
in a much smaller error in ν(t) and it can be surmised that a moderate error in
the measurement of the circumferential strain should result in small amount of
error for G(t) and ν(t).
From the investigation of the effect of finite size of the specimen and exam-
ining figure 26, it is apparent that for the accurate determination of the shear
relaxation function the quotient of indentation radius to the distance from the
center of indentation to the specimen edge for any value above 10 would yield
less than 1% error. On the other hand, the Bulk viscoelastic function is much
more affected by the specimen finite dimensions but it also gets below 5% error
at any value of the quotient larger than 40. It is worth mentioning that the
the increase in error in the Bulk viscoelastic function after a quotient value of
90 is most probably due to small simulation errors. It can be surmised that a
value of the quotient above 50 should yield relatively accurate results. This is
essentially the same result reached by Hill, Storakers, and Zdunek (1989) where
they determined that a minimum value of 50 for the quotient, where they have
performed a more thorough study.
53
6.2 The Tensile Test
Creep tests were performed due to the observation that the load frame could
control the load better than the axial extension or piston position. As mentioned
in section 5.1.1, two different tests were performed at the same load level to
record the axial extension/strain and the circumferential strain; this has been
done due to the limitations of the output channels that could be connected to
the testing machine simultaneously.
From figures 35 and 36 is is apparent that the POM material shows a large
scatter which is expected from polymer materials. The scatter depends on the
specimen, test number and the load level. The scatter due to the different
specimens is expected, though the scatter due to the test number is probably
due to the relaxation behaviour of the material, i.e. the material needs a very
large amount of time to return to its original state. The scatter due to the load
level however shows that the material has a slight load dependency although
the efforts made to stay in the linear viscoelastic regime. The tests data with
the mentioned scatter can be seen in figures 52, 53 and 54 in appendix B. It is
worth mentioning that the relaxation behaviour or the E(t) curve retains the
same shape for the different tests.
6.3 The Indentation Relaxation Test

After performing preparatory tests the strain measurement during the inden-
tation relaxation was found to be very noisy and unreliable; due to the small
change in strains involved in the indentation. The foil strain gauges used are
not suitable for soft and highly temperature dependent materials like polymers
due to the following:
• The strain gauge backing should have a lower stiffness than the tested
material to avoid specimen reinforcement.
• The strain gauge temperature compensation should be suitable for poly-

mers; materials with higher coefficient of thermal expansion than steel.
Although the tests are performed at room temperature, there is a non-negligible

heating on the specimen due to conducted heat from the strain gauge that is
generated by the feed voltage.
Upon examining figure 45, it is apparent that the indentation relaxation
has a slightly different relaxation pattern than the one obtained in the uniaxial
creep tensile test, this is postulated to be due to the errors introduced to the
larger load cell used in the indentation tests. But overall the error shown in
54
figure 46 can be considered small. Further examining of individual tests as in
figures 55, 56, 57 and 58 shows that there is little stress dependency except for
the case of indentation at the depth of 70 µm. This is speculated to be due
to the deviation of the material from the linear viscoelastic behaviour at high
stress/strain levels.
6.4 The Indentation Ramped Test

The ramp test has been developed to alleviate the problem of the machine acting
as spring to push the indenter into materials with very high relaxation rates and
low stiffness as observed and discussed by Jelagin and Larsson (2013).
The indentation ramped test have been performed from a prescribed initial
depth to a prescribed final depth; the reason of doing that is to reduce the
uncertainties pertaining to the surface roughness at low indentation depths.
Upon examining figure 49 it is apparent that the indentation ramped test
has a more different time dependent behaviour than the uniaxial creep test
and the indentation relaxation test; this can be understood by exploring figure
50 and figure 51. The figures show that the largest deviation from the mean
value is found at the beginning of the testing period, and it diminishes as time
advances, indicating that the there is large uncertainty at the beginning of the
test. Since the derived equations depend primarily on the slope of the load
and displacement, that leads to the conclusion that either the load or depth
measurement is not accurate enough. By comparing figure 47 and figure 48 it
is more probable that the problem lies within the load measurement due to the
higher amount of noise and the sudden jumps in the measurements. Using a
smaller load cell should improve the obtained results.
55
Chapter 7
Conclusion
The ramped indentation method was developed to measure two independent

viscoelastic functions while alleviating the problems associated with the much
more used relaxation indentation:
• The inaccuracy due to the impossibility of applying a real Heaviside step

function, especially in the materials with high relaxation behaviour like
bitumen.
• The machine acting as a spring exerting force on the sample for low stiff-
ness high relaxation materials.
From chapter 4 it is determined that the solutions obtained using the functional
integrals method are valid and can accurately measure the shear relaxation
modulus and the bulk viscoelastic function/Poisson’s ratio.
In experiments on POM however, measurement uncertainties introduced er-
rors into the extracted viscoelastic functions, especially in the beginning of the
testing period, these errors could be summarized into three sources: depth mea-
surement, load measurement and strain measurement.
• Depth Measurement Errors: The hydraulic load frame piston position

provided some reasonable measurement of contact depth, but a mechanical
frame could provide better resolution and accuracy for the small depths
involved in measuring the small indentations involved in testing POM,
and that should apply directly to bitumen.
Another improvement that could be done is the measurement of the ma-
chine compliance. The non-linear regression of the curve of total compli-
ance (machine and specimen) with contact force/area method suggested
by Ullner et al. (2010) should provide a more accurate measurement on the
machine compliance that the method used in the analysis in this report.
56
• Load Measurement Errors: This is the major source of error in this
report as argued in the discussion chapter in section 6.4. A small load
cell should be used. This is especially essential for a soft material like
bitumen.
• Strain Measurement Errors: A very accurate and high resolution

strain gauge should be used that is suitable for the material being tested.
For POM a foil strain gauge suitable for polymers can be found commer-
cially. For bitumen however measuring the strain using foil strain gauge
has the potential to prove problematic; due to it’s very high coefficient
of thermal expansion compared to the other materials that the foil strain
gauge is usually designed for, and the problem of the strain gauge reinforc-
ing the bitumen. A suggested method is to use optical strain measurement
on the surface during the indentation to obtain the strain fields. The ob-
tained Poisson’s ratio from the indentation relaxation with relatively small
error is a good indicator that with suitable measurement instruments cal-
culation of the Poisson’s ratio is robust.
In conclusion, the indentation ramped tests have been successfully applied

on POM and the developed method can be directly applied on bitumen if the
aforementioned sources of uncertainties are addressed properly.
57
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Appendices
61
Appendix A
Linear Elastic Equations
This appendix pertains to the derivation of the linear elastic equations in section
3.1 that are used to derive the viscoelastic solution.
A.1 Load–Depth Equation

Johnson (1985) elaborated on the linear elastic solution of the contact problem
originally solved by Hertz (1882). The contact pressure is given by:
p(r) = po a2 − r2 /a

(27)
Which is used to obtain the relation between the pressure and the total load
can be obtained as:
3 P
po = (28)
2 πa2
The indentation depth is given by:
1 − ν2 πpo a
h = ūz (r = 0) = × (29)
E 2
Substituting equation 28 into 29 while recognizing the geometrical relation

7 and the material constants relation E = 2G(1 + ν) and rearranging gives
equation 5.
8 Ga3
P = 3 (1−ν)D
62
A.2 Circumferential Strain Relation
Using the relation relating the circumferential strain, outside the contact area,
to the contact pressure and the contact area from Johnson (1985):
1 (1 − 2 ν) (1 + ν) pa2
θ (r) = − (30)
2 Er2
The relation between the pressure and the applied load outside the contact
area can be given as in equation 31:
P
p= (31)
π a2
By substituting 31 into 30 and using the relation E = 2G(1 + ν) equation 6

can be obtained:
1 (2 ν−1)P
θ (r) = 4 πr 2 G
63
Appendix B
Experimental Results
In this appendix, results from individual tests will be presented.
B.1 Uniaxial Tensile Tests

The results from the uniaxial tensile tests are presented in the figures below.
The total averaged value, between all the tests, for E(t) is also presented in the
figure for comparison.
U niaxial T ensile T est E(t) [Specimen 1]

3600
400 N, Test 1
3500 400 N, Test 2
400 N, Test 3
3400 300 N, Test 1
300 N, Test 2
300 N, Test 3
3300
200 N, Test 1
200 N, Test 2
E (M P a)
3200 200 N, Test 3

All tests average
3100
3000
2900
2800
2700
0 100 200 300 400 500 600 700 800 900
time (s)
Figure 52: E(t) for the tensile tests on Specimen 1
64
3400
400 N, Test 1
400 N, Test 2
3200 300 N, Test 1
300 N, Test 2
200 N, Test 1
200 N, Test 2
3000
All tests average
E (M P a)
2800
2600
2400
2200
0 100 200 300 400 500 600 700 800 900
time (s)

3500
400 N, Test 1
3400 400 N, Test 2
300 N, Test 1
3300 300 N, Test 2
200 N, Test 1
200 N, Test 2
3200
All tests average
E (M P a)
3100
3000
2900
2800
2700
2600
0 100 200 300 400 500 600 700 800 900
time (s)
65
B.2 Indentation Relaxation Tests
The results from the relaxation indentation tests are presented in the figures
below for the different indentation depths. The uniaxial tensile test averaged
value for G(t) is also presented in the figure for comparison.
Relaxation T est 40 µm
1600
test1
1500 test2
test3
1400 test4
test5
Uniaxial
1300
G (M P a)
1200
1100
1000
900
800
700
0 100 200 300 400 500 600
time (s)
Figure 55: G(t) for the relaxation indentation test at 40 µm depth
66
1600
test1
test2
1400 test3
test4
test5
Uniaxial
1200
G (M P a)
1000
800
600
400
0 100 200 300 400 500 600
time (s)
1800
test1
test2
1600
test3
test4
test5
1400
Uniaxial
G (M P a)
1200
1000
800
600
400
0 100 200 300 400 500 600
time (s)
67
2000
test1
test2
1800 test3
test4
test5
Uniaxial
1600
G (M P a)
1400
1200
1000
800
0 100 200 300 400 500 600
time (s)
68
B.3 Indentation Ramped Tests
The results from the ramped indentation tests are presented in the figures below
for the different indentation depths. The uniaxial tensile test averaged value for
G(t) is also presented in the figure for comparison.
20 µm (initial) 50 µm (f inal)
4500
test1
4000 test2
test3
test4
3500 test5
Uniaxial
3000
G (M P a)
2500
2000
1500
1000
500
0 100 200 300 400 500 600
time (s)
Figure 59: G(t) for the ramped indentation test at depths 20 µm initial and 50
µm final
69
30 µm (initial) 60 µm (f inal)
2600
test1
2400 test2
test3
2200 test4
test5
2000 Uniaxial
1800
G (M P a)
1600
1400
1200
1000
800
600
0 100 200 300 400 500 600
time (s)
Figure 60: G(t) for the ramped indentation test at depths 30 µm initial and 60
µm final
70
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DEGREE PROJECT IN ENGINEERING MECHANICS,

SECOND CYCLE, 30 CREDITS

Towards the Measurement of Two

KTH ROYAL INSTITUTE OF TECHNOLOGY

List of Tables vii

List of Symbols viii

A Linear Elastic Equations 62

1 ZHU zwickiLine a commercial indenter for universal hardness

3 Predicted and experimental results for Polyurethane (left) and

7 A schematic of the indentation showing relevant parameters . . . 16

8 The geometry and boundary conditions used in the analysis, ge-

28 The uniaxial creep test sample . . . . . . . . . . . . . . . . . . . 34

52 E(t) for the tensile tests on Specimen 1 . . . . . . . . . . . . . . 64

1 Flat punch indentation validation error, Larsson and Carlsson

5 Smallest diameter du for each uniaxial test sample . . . . . . . . 35

Instrumented indentation is a promising testing technique for obtaining the time

I would like to start by expressing my deepest gratitude to my supervisors,

Indentation tests are used extensively in characterizing materials in the scientific

multi-scale characterization of bitumen and bitumen based materials.

Figure 2: Schematic of multi-scale modeling of bitumen, mastic and asphalt by

Indentation testing is a well-established method for measuring the elastic prop-

2.1 Indentation of Viscoelastic Materials

Material/Property G0 error (%) ν error (-)

VanLandingham et al. (2005) used rounded conical and Berkovich indenters

• Post-yield behaviour due to the concentrated stresses under the sharp

• Difficulty of indenter-tip contact detection especially for PDMS.

Material/Property G(t) error (%)

2.1.2 Lee and Radok’s Functional Integrals

Table 3: Maximum validation errors for different materials and different

Berkovich error (%) Spherical error (%)

Material/Property G0 error (%) K0 error (%)

2.1.3 Other Methods

2.2 Indentation of Bitumen and Bitumen-based

Figure 4: non-linear dash-pot model, Jäger, Lackner, and Stangl (2007)

Figure 5: Validation of nano-indentation results, Jäger, Lackner, and Stangl

Veytskin, Bobko, and Castorena (2014) explored the nano-indentation tech-

2.2.3 Other Methods

1. Relaxation indentation test: the machine will be used in displacement

2. Ramped test: the machine will be operated in either load control or

3.1 The Linear elastic solution

The independent equations are:

• Laplace transform of P and θ into P̃ and ˜θ .

• The relaxation functions in the time domain are obtained by perform-

3.3 Ramp test

By recognizing that the inverse Laplace of the terms multiplied by the

Taking the inverse Laplace of 13 and 14 give respectively:

– Each part of P , h3/2 and θ is separated into equal time intervals

• The viscoelastic functions G and K are expressed in the Prony series

• Equations 15 and 16 are obtained in a symbolic form, by substituting

In order to validate the analytical solutions simulations were performed to vali-

4.1 Models Overview

Figure 8: The geometry and boundary conditions used in the analysis,

4.1.1 Indentation Relaxation Test

4.1.2 Indentation Ramped Load Test

4.2 Back-Calculation of the Viscoelastic Func-

4.2.1 Indentation Relaxation Test

Figure 11: Relaxation load

Figure 12: Relaxation circumferential strain

Shear Relaxation M odulus

Figure 13: The shear viscoelastic function (relaxation test)

Figure 14: The bulk viscoelastic function (relaxation test)

Figure 15: The time dependent Poisson’s ratio (relaxation test)

Figure 16: The error in the viscoelastic functions (relaxation test)

• Laplace transform of P and θ into P̃ and ˜θ .

– Each part of P , h3/2 and θ is separated into equal time intervals