Journal of ELECTRONIC MATERIALS, Vol. 39, No.

4, 2010
DOI: 10.1007/s11664-010-1078-7
Ó 2010 TMS

Characterization of the Viscoelasticity of Molding Compounds

in the Time Domain

SEUNG-HYUN CHAE,1,3 JIE-HUA ZHAO,2 DARVIN R. EDWARDS,2

and PAUL S. HO1

1.—Microelectronics Research Center, The University of Texas at Austin, 10100 Burnet Rd., Bldg.
160, R8650, Austin, TX 78758, USA. 2.—Texas Instruments, Inc., 13536 N. Central Expy.,
MS 940, Dallas, TX 75243, USA. 3.—e-mail: chaes@mail.utexas.edu

Although polymer-based materials are widely used in microelectronics

packaging and viscoelasticity is an intrinsic characteristic of polymers, visco-
elastic properties of polymeric materials are often ignored in package stress
analyses due to the difficulty in measuring these properties. However, it is
necessary to consider the viscoelastic behavior when an accurate stress model
is required. Viscoelastic properties of materials can be characterized in either
the time or the frequency domain. In this study, stress relaxation experiments
were performed on a molding compound in the time domain. A thermorhe-
ologically simple model was assumed to deduce the master curve of relaxation
modulus using the time–temperature equivalence assumption. A Prony series
expansion was used to express the material’s relaxation behavior. Two meth-
ods to determine the Prony pairs and shift factors were compared. After they
were determined, the master curve at a reference temperature was shifted to
every measured temperature for comparison with experimental data.

Key words: Viscoelasticity, molding compound, stress relaxation,

master curve, Prony series

INTRODUCTION while the time-dependent part is often ignored. This

Polymeric materials are extensively used in
microelectronic applications. One of the most
important characteristics of these materials is vis-
coelasticity. The mechanical behavior of a visco-
elastic material depends on both temperature and
time. In many cases, the reliability of microelec-
tronic packages is assessed using the finite element
method (FEM). However, the viscoelastic behavior
of polymeric materials is often neglected, either to
save computational cost or because full character-
ization of the viscoelastic properties is not available.
The elastic approximation for viscoelastic materials
does not lead to satisfactory results and often
overestimates the stresses.1–4 The temperature-
dependent part of viscoelastic properties is usually
reported by using dynamic mechanical analysis
(DMA) measurements at some fixed frequency,
(Received November 11, 2009; accepted January 4, 2010;
published online February 4, 2010)
could be a reasonable approximation if the temper-
ature is well below the glass-transition temperature
(Tg) and the time scale is short. Otherwise, both
temperature- and time-dependent data are required
to obtain stresses more accurately.
There are two categories of methods to charac-
terize viscoelastic properties.5 One is frequency-
domain measurements using DMA, in which
dynamic responses of a material are measured at
multiple oscillation frequencies over a wide range of
isothermal temperatures. Then the complex moduli
(storage modulus and loss modulus) in the fre-
quency domain can be converted to the relaxation
modulus in the time domain by using an appropri-
ate relationship or formula.6–9 The other approach
is to characterize the relaxation (or creep) behavior
of a material directly in the time domain. This is
achieved by applying a fixed displacement (or load)
for a certain duration of time at various isothermal
temperatures. Using either approach, a master curve
can be constructed using the time–temperature

419
420 Chae, Zhao, Edwards, and Ho

equivalence which holds for thermorheologically where rk,0 (=Eke0) is the initial stress at t = 0, and sk
simple materials (TSM). is the relaxation time of the kth element. Then the
Molding compounds are encapsulating materials total stress is given by
used to protect microelectronic devices mechani-
X
n
cally, electrically, and environmentally from their rðtÞ ¼ E1 e0 þ rk;0 expð
t=sk Þ
surroundings. Since molding compounds are usu- k¼1
ally epoxy-resin-based materials, viscoelastic char- " # (3)
X
n
acterization should be conducted to estimate the ¼ e0 E 1 þ Ek expð
t=sk Þ :
stresses in packages more accurately. In this study, k¼1
the viscoelasticity of a molding compound was
characterized in the time domain by performing The relaxation modulus E(t) is defined as
uniaxial stress relaxation tests at several tempera-
X
n
tures. In order to implement viscoelastic material EðtÞ ¼ rðtÞ=e0 ¼ E1 þ Ek expð
t=sk Þ; (4)
properties in FEM, the master curve was fitted with k¼1
a Prony series. Two approaches were utilized to
determine the master curve and shift factor so that which is essentially the Prony series representa-
they should describe the material’s behavior closely. tion.6,10 Here, E1 is the final (or equilibrium) modulus,
After Prony pairs were determined, a virtual stress Pn

relaxation experiment was performed using FEM to and E0 ¼ E1 þ Ek is the instantaneous modulus.
k¼1
cross-check the material input. A pair of Ek and sk is referred to as a Prony pair.
THEORETICAL BACKGROUND
Time–Temperature Equivalence
Prony Series Representation of Linear
Viscoelasticity In general, the relaxation modulus is a function of
both time and temperature. For a certain class of
Linear viscoelastic behavior can be described by materials, the effect of time and temperature on the
the generalized Maxwell model shown in Fig. 1.6,10 material’s behavior can be treated in the same
An extra isolated spring (E1) is added to represent manner through the time–temperature equivalence
arrheodictic behavior. A material is called arrheod- (TTE) principle, which is also called the time–
ictic if it has a preferred configuration.6 temperature superposition (TTS) principle or
The behavior of each Maxwell element, where a time–temperature reducibility.5,9,11 The following
spring and a dashpot are connected in series, is relation states the TTE:
expressed as
t
r_ k rk Eðt; TÞ ¼ Eðf; T0 Þ; f¼ ; (5)
e_ k ¼ þ ; k ¼ 1; 2; . . . ; n; (1) aT ðTÞ
E k gk
where T is the measurement temperature, t is the
where Ek is the elastic modulus, and gk is the vis- actual time of measurement, T0 is an arbitrary
cosity of the kth element. If a constant strain e0 is reference temperature, f is called the reduced time,
imposed at t = 0, the solution of Eq. 1 is given by and the scaling factor aT(T) is called the tempera-
g ture shift factor. According to the TTE, the visco-
rk ðtÞ ¼ rk;0 expð
t=sk Þ; sk ¼ k ; (2) elastic behavior at one temperature can be related
Ek
to that at another temperature by a shift in the time
scale.5,9,11 From Eqs. 4 and 5, the change in the
relaxation time of a Maxwell element due to a
temperature change is also determined by the
temperature shift factor. Thus
t sðTÞ
aT ðTÞ ¼ ¼ ; (6)
f sr
E1 E2 ··· Ek ··· En where s(T) is the relaxation time at temperature T,
E∞ and sr is the relaxation time at the reference tem-
h1 h2 hk hn perature (T0). When temperature varies with time,
the reduced time is obtained by9,12
Zt Zt
dt sr
fðtÞ ¼ ¼ dt: (7)
Fig. 1. Schematic of a generalized Maxwell model consisting of n aT ðTðtÞÞ sðTðtÞÞ
Maxwell elements connected in parallel. In each Maxwell element, a 0 0
spring (Ek) and a dashpot (gk) are connected in series. An extra
isolated spring is added in parallel to represent the final (or equilib- The class of materials obeying this TTE are called
rium) modulus (E1). thermorheologically simple materials. Based on the
Characterization of the Viscoelasticity of Molding Compounds in the Time Domain
TTE assumption, a master curve can be constructed
at an arbitrary reference temperature by shifting the
relaxation moduli at all other temperatures to the
reference temperature. In a log–log plot of relaxation
modulus versus time, this is equivalent to a shift of
the curves horizontally by a distance log aT(T). This
is why aT(T) is normally called the temperature shift
factor. The importance of the TTE assumption is that
the mechanical behavior of a material at any tem-
perature can be anticipated beyond the range of an
experimental time scale. In our experiment with a
molding compound, the time scale of the master
curve ranged over about 20 decades.
One of the most common functions for the
shift factor is the Williams–Landel–Ferry (WLF)
equation5,9,11,12:
C1 ðT
T0 Þ
log aT ðTÞ ¼
; (8)
C2 þ ðT
T0 Þ
where C1 and C2 are material constants. Another
common shift function is expressed in Arrhenius
form5,9,11,12:



E 1 1 1 1
ln aT ðTÞ ¼
¼ D1
; (9)
R T T0 T T0
where E is the activation energy, R is the universal
gas constant, and D1 (=E/R) is the material
constant. T and T0 are in absolute temperature
(Kelvin). In many cases, the WLF equation is
applied for T > Tg, while the Arrhenius expression
is used for T < Tg.12–14 Other empirical expressions
including polynomial functions have also been used
to better fit the shift function to experimental
data.4,12,14,15
EXPERIMENTAL PROCEDURES
The material characterized in this study was an
epoxy-based molding compound with a filler content
of 87 wt.%. Bar-type tensile specimens were pre-
pared by transfer molding at 175°C with an in-mold
cure time of 90 s. Then the specimens were post-
mold cured at 175°C for 4 h. Tg was 120°C to 140°C
based on DMA and thermomechanical analysis
(TMA). The specimen dimensions were 127 mm
(L) 9 12.7 mm (W) 9 3.17 mm (T).
The stress relaxation tests were conducted using
an electromechanical testing system under strain
control. Special grips were custom-machined to
minimize grip slippage. The specimen grip length
was about 25 mm at both ends. Displacements were
measured by an extensometer whose gage length
was 25 mm. A strain of e0 = 0.1% was applied within
1 s and was then kept constant throughout the test.
The resulting stress r(t) was monitored for 10 min
to 60 min. The relaxation modulus E(t) was calcu-
lated using the relationship EðtÞ ¼ rðtÞ=e0 . Several
tests were carried out at the same temperature to
confirm consistency.
Practically, a finite duration of time is needed to
impose a strain in stress relaxation tests, since the
421
theoretical instantaneous strain is not achievable.
In addition, the initial portion of the relaxation
behavior after loading with a finite strain rate
deviates somewhat from the case of ideal instanta-
neous loading, while the behavior of the former
becomes essentially equivalent to the latter in about
ten times the loading time.16,17 For this reason, the
data obtained during the first 10 s after loading
were discarded.
RESULTS AND DISCUSSION
The relaxation moduli measured at various
temperatures ranging from 20°C to 150°C are
depicted in Fig. 2. At low and high temperatures,
the relaxation moduli were nearly constant, indi-
cating that stress relaxation at these temperatures
was not significant. However, the rate of relaxation
was significantly increased between 100°C and
120°C, indicating the effect of the glass transition of
the material.
The master curve was generated by shifting the
relaxation moduli data horizontally with respect to
a reference temperature using the shift factor
defined in Eq. 6. Two different approaches for con-
structing the master curve and determining the
associated Prony pairs and shift function were
investigated using the viscoelastic material curve-
fitting utility of commercial FEM software ANSYS.
In the first approach, the shift factors were deter-
mined first while individual relaxation modulus
curves were shifted with respect to a reference
temperature, T0, one by one. Then the data of
the reduced time and relaxation modulus were
imported into ANSYS. Subsequently, Prony pairs
were determined for the master curve at T0 by the
curve-fitting routine of ANSYS. In the second
approach, both Prony pairs and shift function
constants were determined simultaneously using
the curve-fitting routine. This was done by loading
the raw experimental data at every measurement
temperature directly into ANSYS.
100
20C
30C
40C
50C
10 60C
70C
E(t) (GPa)
80C
90C
100C
1 110C
120C
130C
140C
150C
0.1
1 10 100 1000 10000
Time (s)
Fig. 2. Stress relaxation moduli of an epoxy-based molding
compound as a function of time at 14 isothermal temperatures.
422
100
Data
Curve fit
10
E(t) (GPa)
1 -5
0.1
-12 -9 -6 -3 0 3 6 9 12 15
log t (s)
Fig. 3. Master curve generated by shifting the relaxation moduli
horizontally at different temperatures in Fig. 2 with respect to the
reference temperature of 110°C. The horizontal axis is the logarithm
of reduced time at 110°C. The vertical axis is the relaxation modulus.
Approach I
The individual relaxation moduli in Fig. 2 were
shifted with respect to T0 = 110° to form a master
curve. The relaxation modulus at the temperature
closest to T0, i.e., E(t,100°C) or E(t,120°C), was
shifted first. The associated shift factor, aT(100°C)
or aT(120°C), was determined to make the shifted
relaxation modulus and the nonshifted one at T0 lie
along a single smooth curve. The reduced time was
obtained from Eq. 6. Subsequently, the relaxation
modulus at the next closest temperature was shifted
in the same manner, and so forth. The master curve
and shift factors determined by this process are
plotted as open circles in Figs. 3 and 4, respectively.
The determined master curve needs to be
expressed as a Prony series (Eq. 4) for the material
property to be used in the FEM. The nonlinear
curve-fitting utility in ANSYS was used to deter-
mine the Prony pairs. As it is recommended to use
one Prony pair for each decade of time,13,18 21 Prony
pairs were defined at the beginning of the fitting
process. Initially the relaxation time sk was fixed in
such a way that every sk was evenly spaced on the
log t axis. After ANSYS finished the predefined
iteration steps to solve for the 21 values of Ek,
subsequent iteration steps proceeded with sk
unfixed. By using this procedure, 43 unknowns of Ek
and sk were obtained, which are listed in Table I.
The resulting master curve is plotted as a solid line
in Fig. 3.
In Fig. 4, the shift factors were fitted by different
shift functions. The constants in the WLF and
Arrhenius shift functions were determined by the
‘‘Solver’’ macro in Microsoft Excel. It is apparent
that the trend for the temperature dependency was
not simple, so either the WLF or Arrhenius equation
alone did not fit the data very well. In fact, the WLF
equation is usually applied for T > Tg, while the
Arrhenius expression works well for T < Tg.12–14
Chae, Zhao, Edwards, and Ho
15
10
5
log aT(T)
0
Data
WLF fit
Arrhenius fit
-10
Polynomial fit
-15
0 25 50 75 100 125 150 175
Temperature (°C)
Fig. 4. Horizontal (temperature) shift factor with a reference tem-
perature of 110°C and curve-fit results of different shift functions.
A polynomial equation (Eq. 10) provides a better fit than WLF (Eq. 8)
and Arrhenius (Eq. 9) equations.
Besides, the high filler content of the molding com-
pound could add further complexity. Therefore, a
single WLF or Arrhenius equation did not lead to a
good fit.
A better fit was achieved with a polynomial
equation (Fig. 4), which is also a common approach
in FEM analyses.4,14 A third-order polynomial was
chosen as an approximation for the logarithm of the
shift factor:
log aT ðTÞ ¼ a1 ðT
T0 Þ þ a2 ðT
T0 Þ2
þ a3 ðT
T0 Þ3 : ð10Þ
The three coefficients were determined to be
a1 =
0.170, a2 =
1.25 9 10
3, and a3 =
5.88 9
10
6 by the least-squares best-fit method using the
Excel ‘‘Solver’’ macro. As seen in Fig. 4, this poly-
nomial equation described the temperature-depen-
dent shift factor much more closely than either the
WLF or Arrhenius equation. Figure 5 shows master
curves shifted by using Eq. 10 with respect to
T0 = 110°. The master curves agreed well with the
experimental data, although some disagreement
still exists. This disagreement was attributed to a
relatively small mismatch of the shift function with
data (Fig. 4). The polynomial form of the shift
function can be employed in commercial FEM soft-
ware by using a user-defined subroutine.
Approach II
The viscoelastic material curve-fitting routine of
ANSYS has the capability to determine Prony pairs
and shift function constants simultaneously. It is
not necessary to shift experimental data one by one
to construct a master curve before Prony pairs are
determined. After loading raw experimental data
for each temperature into ANSYS, curve fitting is
performed to find the best fit to the temperature-
dependent relaxation data. Thus, this is an easier
Characterization of the Viscoelasticity of Molding Compounds in the Time Domain 423

Table I. Prony pairs for the master curve shown in Fig. 3 with a reference temperature of 110°C
k sk (s) Ek (MPa) k sk (s) Ek (MPa) k sk (s) Ek (MPa)

1 – 530 8 2.7 9 10
1 1938 16 8.6 9 105 300

1 1.6 9 10
8 522 9 1.7 2082 17 1.1 9 107 145
2 2.8 9 10
7 483 10 1.2 9 10 2663 18 9.8 9 107 94
3 4.4 9 10
6 522 11 4.8 9 10 2265 19 109 96
4 5.4 9 10
5 589 12 2.5 9 102 2295 20 1010 34
5 6.2 9 10
4 817 13 2.2 9 103 2155 21 1011 71
6 6.0 9 10
3 984 14 1.5 9 104 720
7 4.1 9 10
2 1143 15 1.0 9 105 408

100 (a) 100

20C 30C 40C 50C 60C 70C 80C 20C 30C 40C 50C 60C 70C 80C
90C 100C 110C 120C 130C 140C 150C 90C 100C 110C 120C 130C 140C 150C

10 10

E(t) (GPa)
E(t) (GPa)

1 1

0.1 0.1
-6 -4 -2 0 2 4 6 8 10
-6 -4 -2 0 2 4 6 8 10
log (t (s)) log (t (s))

Fig. 5. Master curves at various temperatures shifted by a third- 20

order polynomial function, shown together with experimental data. (b)
Data
The solid line represents the master curve at a reference tempera-
ture of 110°C, and the dotted lines represent the shifted master 15 WLF fit
curves. The experimental data are depicted as markers.
10
log aT(T)

5
and more convenient approach than the previous
method. Its limitations, however, include: (1) the
0
available shift functions are limited to only two
types (either WLF or Arrhenius), and (2) the
determined shift function constants are often -5
dependent on an initial input (or guess). Neverthe-
less, this method provides greater flexibility to -10
0 25 50 75 100 125 150 175
adjust the shift function constants as well as Prony
Temperature (°C)
pairs at the same time.
Both WLF and Arrhenius shift functions were Fig. 6. Master curves and WLF shift function determined simulta-
evaluated, and the former was found to give a neously by the nonlinear curve-fitting routine in ANSYS. (a) Master
curves at various temperatures shifted by the WLF equation, shown
slightly better fit for this material. Figure 6 shows together with experimental data. The solid line represents the master
the master curves and WLF shift function resulting curve at a reference temperature of 120°C, and the dotted lines
from this method. Twenty-one Prony pairs were represent the shifted master curves. The experimental data are de-
activated at first, but some of the Ek values became picted as markers. (b) WLF fit with a reference temperature of 120°C.
negligible or zero during the curve-fitting routine.
The resulting Prony pairs are summarized in
Table II. The WLF constants were determined to be
C1 = 2.01 9 1011 and C2 = 1.51 9 1012 with a ref- erly, as mentioned earlier. Still, a reasonable fit was
erence temperature of T0 = 120°C. These large achieved between experimental data and the master
numbers resulted in an almost linear result, as curve over a certain temperature range, as shown in
shown in Fig. 6b. This is attributed to the fact that Fig. 6a. This method would provide great conve-
the WLF equation alone could not describe this nience and efficiency if the shift factor can be fitted
material’s temperature-dependent behavior prop- well by either the WLF or Arrhenius equation.
424 Chae, Zhao, Edwards, and Ho

Table II. Prony pairs for the master curve in Fig. 6a which was determined together with WLF constants
by ANSYS with a reference temperature of 120°C
k sk (s) Ek (MPa) k sk (s) Ek (MPa) k sk (s) Ek (MPa)

1 – 504 7 8.3 9 10
5 981 14 103 335

1 1.6 9 10
12 516 8 2.0 9 10
3 1282 15 104 169
2 2.2 9 10
11 274 9 2.0 9 10
2 1209 16 105 108
3 4.6 9 10
10 438 10 2.2 9 10
1 3704 17 106 40
4 9.2 9 10
9 306 11 3.8 6188 18 107 72
5 2.2 9 10
7 524 12 10 1757
6 3.5 9 10
6 774 13 9.9 9 10 1758

100 behavior of a molding compound. The nonlinear

curve-fitting routine of ANSYS was employed to
determine Prony pairs, which can be used as input
for subsequent FEM stress simulations. The curve
10 fitting was carried out in two ways. In the first
E(t) (GPa)

method, the temperature shift factor for each

temperature was determined one by one to con-
struct a master curve. Then the Prony pairs were
1 determined for the reference temperature using
the curve-fitting routine. The temperature depen-
dency of the shift factor could be described by a
polynomial equation as well as the WLF or
0.1 Arrhenius equation. In an alternative method, the
-6 -4 -2 0 2 4 6 8 10 temperature-dependent relaxation modulus data
log (t (s)) were loaded directly into the curve-fitting routine
20C (Data) 30C (Data) 40C (Data) 50C (Data)
to determine the Prony pairs and shift function
60C (Data) 70C (Data) 80C (Data) 90C (Data) constants at the same time. This provided greater
100C (Data) 110C (Data) 120C (Data) 130C (Data) convenience and efficiency, although only the WLF
140C (Data) 150C (Data) 20C (Model) 30C (Model)
40C (Model) 50C (Model) 60C (Model) 70C (Model)
or Arrhenius equation is available as a shift func-
80C (Model) 90C (Model) 100C (Model) 110C (Model) tion. The viscoelasticity constitutive law of the
120C (Model) 130C (Model) 140C (Model) 150C (Model) molding compound was obtained from the resulting
Fig. 7. Verification of the viscoelastic property of a molding com-
Prony pairs.
pound with a FEM model. The lines indicate the relaxation moduli
defined by the Prony pairs and shift function as shown in Fig. 6a. The
markers represent the responses of the material in the FEM model,
ACKNOWLEDGEMENTS
calculated by stress divided by strain for a bar sample. The authors would like to acknowledge Prof.
Raymond A. Pearson at Lehigh University for
valuable discussion on the viscoelastic material
testing.
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