The Effects of Rigid Polystyrene Particles on the Glass Transition
Characteristics and Mechanical Wave Attenuation of Styrene-Butadiene
Rubber: Particle Size and Acoustic Mismatch
FARHAD FAGHIHI, NASER MOHAMMADI, MAJID HAGHGOO
Loghman Fundamental Research Group, Polymer Engineering Department, Amirkabir University of Technology,
P. O. Box 15875-4413, Tehran, Iran
Received 13 June 2009; revised 7 September 2009; accepted 8 September 2009
DOI: 10.1002/polb.21846
Published online in Wiley InterScience (www.interscience.wiley.com).
ABSTRACT: Glass transition characteristics and mechanical wave
attenuation of the neat and filled styrene-butadiene rubber (SBR)
containing 10 wt % of rigid monosize polystyrene particles of var-
ious diameters from several hundred microns down to several
tens of nanometers were investigated by dynamic mechanical
thermal analysis, impedance tube, and ultrasonic spectroscopy.
The results showed the matrix damping capacity and the breadth
of glass transition increase by reducing the size of rigid particles
due to the matrix-particles interfacial area increase as the major
governing parameter. Matrix glass transition broadening toward
higher temperatures was attributed to the increased dynamic het-
erogeneity induced by fillers, whereas the damping capacity
increase was assigned to contribution of interfacial friction loss
mechanism. The proposed postulation was confirmed based on
the calculated temperature distribution of the relaxing matrix vol-
ume fraction. Sound wave attenuation by the matrix and PS par-
INTRODUCTION Absorption and attenuation of mechanical
waves with polymers is of great importance in diverse appli-
cations. The behavior of polymers in response to mechanical
waves is dominated by their viscoelastic state, which
depends among other factors, to the frequency and the am-
plitude of incident wave. Various modes of molecular
motions, specifically local segmental one, provide the main
mechanism for mechanical energy damping with polymers.
Local segmental dynamics has the maximum contribution in
energy dissipation when its characteristic time coincides
with the vibration frequency.1 Therefore, polymers show
maximum mechanical wave energy dissipation in their
glass–rubber transition. Numerous attempts have been made
to extend the frequency span of the glass transition and
improve the damping capacity in this region by designing
phase separated multicomponent polymeric systems with
modified molecular dynamics.2,3 Among different app-
roaches, addition of rigid particles, specifically in nanosize
scale, to soft elastomeric matrices seems promising via mod-
ifying local segmental dynamics in a desired way and acti-
vating additional wave attenuation mechanisms. Investiga-
Correspondence to: N. Mohammadi (E-mail: mohamadi@aut.ac.ir)
C 2009 Wiley Periodicals, Inc.
Journal of Polymer Science: Part B: Polymer Physics, Vol. 48, 8288 (2010) V
82
ticles filled systems led to a broad absorption peak for the former
and appearance of a secondary absorption peak at lower frequen-
cies for the latter. Intensity of this secondary peak was highest
for the system containing PS nanoparticles. Finally, ultrasonic
attenuation enhanced by the PS particle size to wavelength ratio
increase according to asca
(d/k)0.38 scaling law and declined by
replacing the dense particles with larger hollow PS particles.
Comparison of the normalized attenuation of the PS particle filled
SBR in various mechanical wave attenuation regimes implied
low sensitivity to particle size in vibration, mild differentiation in
the sound, and finally severe differentiation in the ultrasound
regimes. V C 2009 Wiley Periodicals, Inc. J Polym Sci Part B: Polym
Phys 48: 82–88, 2010
KEYWORDS: acoustic; attenuation; glass transition; loss area;
mechanical waves; nanoparticles
tion of local dynamics of filled elastomers by different
techniques, such as, nuclear magnetic resonance,4 dielectric
spectroscopy,5 and neutron scattering6 have revealed some
evidences regarding the existence of an interfacial layer of
matrix chains with highly restricted segmental mobility.
Based on NMR spectroscopy, Berriot et al.7 confirmed glass
transition gradient in the vicinity of dispersed particles.
Induction of a network of domains with slow dynamics
extending few nanometers from particles surfaces toward
the bulk was suggested due to polymer-particles interac-
tions.7 However, controversial results have been published
on the extent to which this localized effect could influence
the glass transition of the filled polymer.8 Tsagaropoulos and
Eisenberg9 reported an additional peak in tan d of nanopar-
ticles filled vinyl polymers at temperatures higher than the
main glass transition peak of matrix. This new relaxation
was attributed to the glass transition of the matrix chains
with restricted mobility at particles surfaces. The appear-
ance of a secondary relaxation in tan d spectra of nanosilica
filled styrene-butadiene rubber (SBR) matrix has also been
reported.10 The intensity of this relaxation was proposed to
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be proportional to the filler volume fraction and polymer–fil-
ler interfacial strength. Rao and Pochan11 have quantitatively
related the depression in the tan d peak of the matrix glass
transition to the number of immobilized chain segments
in the interfacial region. Nevertheless, recent works12–14
showed no indication of additional relaxation or perceivable
change in overall glass transition of filled polymers associ-
ated with immobilized matrix layer around particles. The
decrease in the intensity of dielectric loss peak at a-relaxa-
tion and tan d peak at glass transition temperature was
attributed to the reduced polymer volume fraction and
increased storage modulus of filled polymer, respectively.
Besides changing molecular dynamics of the matrix, the
presence of rigid particles may also activate additional me-
chanical wave dissipation and attenuation mechanisms. It
has been demonstrated that dispersed rigid particles with
high specific surface area cause significant increase in loss
modulus of polymeric composites.15 This is due to energy
dissipation by frictional sliding at the polymer-particle inter-
face. The extent of contribution of this mechanism to overall
energy dissipation is determined by several factors, such as,
the oscillatory deformation amplitude, the strength of inter-
facial interactions, and the effective sliding area.15 Alterna-
tively, acoustic attenuation in filled polymers can be acti-
vated due to wave scattering from rigid inclusions. This
additional mechanism becomes specifically important at ul-
trasonic frequencies. A theoretical model for ultrasonic wave
attenuation in viscoelastic particulate composites was pro-
posed by Beltzer and Brauner assuming independent scatter-
ing from particles.16 Biwa et al.17,18 utilized a differential
scheme to investigate ultrasonic attenuation in rigid particle
filled polymers. It was shown that the scattering loss
depends remarkably on the wavelength-to-particle size ratio.
When the wavelength is sufficiently large compared with the
particle radius, scattering loss is negligibly small and pres-
ence of rigid particles decrease wave attenuation capacity by
decreasing matrix volume fraction. However, as the particle
size to wavelength ratio grows toward unity, the contribution
of scattering loss rises significantly and improves overall ul-
trasonic attenuation of the composite.
In this article, vibration damping and acoustic attenuation
behavior of SBR filled with polystyrene particles of various
sizes are investigated. The influence of rigid particles on
glass transition characteristics and various mechanical
energy dissipating mechanisms of the elastomeric matrix are,
then, evaluated.
EXPERIMENTAL
Materials
Styrene-butadiene random copolymer (styrene content  23
wt %) latex with solid content of 20 wt % was obtained
from Bandar Imam petrochemical complex (Iran). Expanda-
ble polystyrene (EPS) was obtained from Tabriz petrochemi-
cal complex (Iran). Styrene monomer, sodium lauryl sulfate
and Triton X-100 (surfactants), potassium persulfate (initia-
tor), and tertiary dodecyl mercaptan (TDM, chain transfer
EFFECTS OF RIGID POLYSTYRENE PARTICLES, FAGHIHI, MOHAMMADI, AND HAGHGOO
ARTICLE
agent) were supplied by Merck Co. and used without further
purification.
Synthesis and Fractionation of Polystyrene Particles
Narrow size distribution polystyrene nanoparticles, 80 nm in
diameter with particle size distribution (PSD) of 1.05, were
synthesized by emulsion polymerization.19 Monosize 1 lm
with PSD of 1.07 and larger PS particles were synthesized
by dispersion polymerization20 and suspension polymeriza-
tion, respectively. Due to broad size distribution of suspen-
sion polymerized PS and EPS samples, they were sieved to
narrow size distribution fractions with different average
diameters and PSD of around 1.15.
Particle Size Characterization
The size and size distribution of nanoparticles were deter-
mined using dynamic laser light scattering (SEMAtech,
France) by a He-Ne laser beam with wave length of 632.8
nm. The average size of dispersion particles was determined
by scanning electron microscope (Cambridge, 630ST).
Sample Preparation
Neat and filled SBR sheets, 2 mm in thickness, were pre-
pared by latex-film formation in a Teflon-coated pan at room
temperature for 1 week. To prepare the filled systems, poly-
styrene latex (15 wt % solid content) or dried polystyrene
particles were mixed with the SBR latex before film forma-
tion using magnetic stirrer at 300 rpm for 5 min.
Techniques
Dynamic mechanical behavior of the neat and filled SBR
samples was studied in temperature range of 100 to 50  C
with heating rate of 5  C/min at fixed frequency of 1 Hz by
Dupont-DMA, model 983. The test was performed in cantile-
ver bending deformation mode on rectangular samples,
2 mm in thickness, at strain amplitude around 0.1%.
Dynamic strain sweep experiments were performed at 1 Hz
and two different temperatures, 20 and 23  C in the
dynamic strain range of around 0.01–1% before the main
experiments. The results clearly indicated that all samples
are within linear viscoelastic region at 0.1% strain ampli-
tude. Normal incident sound absorption coefficient of the
samples was measured in the frequency range of 500–6300
Hz using B&K impedance tube according to ASTM-E1050.
Ultrasound attenuation was measured by trough-transmis-
sion method21 at 3.8 MHz and room temperature. Two ultra-
sound transducers (Karl Deutsch, TS 10wB4) were mounted
coaxially with 10 cm separation inside a water bath. The test
specimen was placed halfway between two transducers. The
transmitted wave through the specimen was analyzed by an
oscilloscope.
RESULTS AND DISCUSSION
Dynamic mechanical behavior of the neat and three filled
SBR samples containing 10 wt % of monosize polystyrene
particles with different sizes are shown in Figures 1–3. Addi-
tion of the glassy polystyrene particles increased the filled
systems storage modulus at glass transition and rubbery
regions, Figure 1. The storage modulus increase is rather
similar for micron size particle filled samples. However,
83
JOURNAL OF POLYMER SCIENCE: PART B: POLYMER PHYSICS DOI 10.1002/POLB
FIGURE 1 Temperature dependence of the storage modulus
of the neat SBR and monosize polystyrene particles filled
systems.
particle size decrease to 80 nm, markedly improved the rein-
forcing effect of the dispersed particles and more interest-
ingly, reduced the slope of the storage modulus–temperature
variation at the matrix glass–rubber transition region. At
glass transition the loss modulus peak height decreased
from around 370 MPa for the neat SBR to about 280 MPa
for the filled samples, whereas the peak temperature varia-
tion did not follow any definite trend with particle size. The
influence of particle size decrease on segmental relaxation of
the matrix is also evident in Figures 2 and 3 as the transi-
tion region is extended toward higher temperatures by
including the nanoparticles. Its worth mentioning that the
damping capacity variation may also be analyzed based on
tan d–temperature curves, Figure 3. Nonetheless, appreciable
E0 increase by addition of rigid particles, specifically nano-
particles, can reduce the intensity of tan d peak significantly.
Therefore, determination of energy damping capacity and the
quantity of relaxing segments based on tan d curves can be
misleading for the case of filled systems. In filled systems,
matrix-particle interaction may cause significant local dy-
namics slowdown and lead to formation of interfacial layer
FIGURE 2 Temperature dependence of the loss modulus of the
neat SBR and monosize polystyrene particles filled systems.
84
FIGURE 3 Temperature dependence of the tan d of the neat
SBR and monosize polystyrene particles filled systems.
of matrix chains with hindered segmental relaxation.7 How-
ever, this local effect only becomes appreciable when the ma-
trix-particle interfacial area grows sufficiently high with par-
ticle size decrease, Table 1. This could be the underlying
reason differentiating viscoelastic behavior of microparticle
and nanoparticle filled systems. To further investigate the
influence of rigid particles on matrix segmental relaxation,
the relaxing matrix volume fraction distribution in the glass
transition region was derived from storage modulus data. It
is well established that increased dynamic heterogeneity in
glass formers increases the breadth of a-relaxation22 and
this, in turn, reduces the slope of storage modulus decrease
at Tg, as for instance is the case for interpenetrating polymer
networks. Therefore, the slope of storage modulus can be
considered as a measure of the breadth of a-relaxation.
Moreover, the slope of storage modulus versus time curve is
proportional to the intensity of relaxation at each relaxation
time within the whole spectrum of glass transition.23 Assum-
ing that the normalized relaxation intensity is proportional
to the fraction of relaxing domains, and considering the
time–temperature correspondence, we can calculate the vol-
ume fraction of matrix segments relaxing between T and T þ
DT from normalized storage modulus decrease, DE0 , at this
temperature interval24:
TABLE 1 Interfacial Characteristics and Loss Area of the Neat
and 10 wt % PS Particle Filled SBR
The Size of the PS Filler
Neat
Sample SBR 500 lm 250 lm 75 lm 1 lm 80 nm
Interfacial – 11 22 74 5560 69,500
area per
unit volume
(cm2/cm3)
Ligament – 461 230 69 1 0.07
thickness (lm)
Loss area (a.u.) 7150 – 6830 – 6860 8010
INTERSCIENCE.WILEY.COM/JOURNAL/JPOLB

FIGURE 4 Distribution of relaxed matrix volume fraction of the
neat SBR and filled systems. Each curve is normalized to its
peak intensity.
!
0
ETþDT  ET0
Durelaxed ¼
Er0  Eg0
where Eg0 and Er0are the glass and rubber storage modulus,
respectively. The normalized relaxation curves of the neat
and filled SBR samples were plotted in Figure 4 (the relaxa-
tion spectrum of the sample containing 250 lm particles
was omitted for the sake of clarity). Matrix-particle contact
area increase clearly shifted the segmental relaxation of cer-
tain fraction of matrix chains to higher temperatures, con-
firming local dynamics slowdown in the vicinity of particles.
Therefore, the breadth of matrix softening dispersion
increase in the nanoparticle filled system could be attributed
to the particle induced dynamics heterogeneity in the elasto-
meric matrix phase. It is to be noted that filled rubbers can
show strain-induced nonlinearity in their modulus and
undergo pseudo-glass transition under oscillatory strain due
to dejaming process of filler network.25 This process is influ-
enced by various factors, such as, dynamic strain amplitude,
filler volume fraction, and temperature.25 In our samples,
possible occurrence of filler network breakdown under
applied dynamic strain should increase the steepness of stor-
age modulus, |dE/dT|, at matrix glass transition. However,
the storage modulus steepness of micron and nanosize PS
particle filled samples did not change or even decreased in
comparison with the neat matrix. Therefore, we postulated
that the network structure of rigid PS particles, if there
existed any, remained intact during matrix glass transition
due to low temperature and strain amplitude (
0.1%) and
the storage modulus decrease was mainly originated from
matrix chains segmental relaxation. Damping capacity of me-
chanical energy in both neat and filled systems under
dynamic deformation at temperatures below the glass transi-
tion of PS particles,
100  C, was calculated from the area
under the loss modulus curves (loss area), Figure 2, and
tabulated in Table 1. Replacing a part of matrix phase with
rigid particles may decline the glass transition overall damp-
EFFECTS OF RIGID POLYSTYRENE PARTICLES, FAGHIHI, MOHAMMADI, AND HAGHGOO
ARTICLE
ing through the number of relaxing chains decrease. How-
ever, friction at the matrix-particle interface may provide
additional energy dissipating mechanism and increase the
area under the loss modulus curve of filled samples.15 The
contribution of the new mechanism becomes important
when the matrix-particle interfacial area grows sufficiently
high. Therefore, the loss peak area increase of samples con-
taining nanometer size polystyrene particles with high sur-
face area is observed due to the extra contribution of the
interfacial friction, whereas the ineffective large particles
reduced the loss peak area, Table 1. It should be mentioned
that particles synthesized by different methods may have dif-
ferent surface chemistry and roughness. However, consider-
ing possible influence of the particles surface chemistry and
roughness on viscoelastic behavior of filled samples besides
the effect of particle size, can make the analysis far more
complicated which is not in the scope of this article.
Viscoelastic behavior of the matrix phase in the acoustic
frequency range was estimated by applying WLF time–
temperature superposition principle to the DMTA results,
eq 2:
(1)
C1 ðT  T0 Þ
log aT ¼  (2)
C2 þ ðT  T0 Þ
The constants C1 ¼ 17.44 and C2 ¼ 51.6 were selected from
literature26,27 and confirmed by the time–temperature super-
position studies on the SBR.28 Matrix glass transitions were
estimated to be 60  C and 38  C for the lower (500 Hz)
and upper (3.8 MHz) acoustic frequencies, respectively.
Therefore, the matrix phase was anticipated to behave rub-
bery under conditions applied in both sound absorption and
ultrasound attenuation measurements. The sound absorption
coefficient of the neat SBR and three filled samples in fre-
quency range of 500–6300 Hz at room temperature are pre-
sented in Figure 5. The sound absorption capacities of all
samples were rather low due to their poor impedance match
with air. Nevertheless, the sound absorption spectra revealed
some interesting features. The neat SBR showed a single
broad absorption peak at high frequencies, whereas in all
filled systems, additional sound absorption peak appeared at
lower frequencies. The intensity of low frequency peak
increased with the PS particle size decrease down to 80 nm.
The absorption peak at high frequency, which is more pro-
nounced in the neat sample, can be attributed to the acoustic
energy dissipation by the molecular motions of elastomeric
matrix. The low frequency peak, appeared only in the filled
samples, might be due to the particles vibration under the
influence of sound wave.29,30 Vibrational motions of particles
provide additional energy dissipation mechanism by inducing
shear deformation in the matrix ligament between adjacent
particles. This mechanism is magnified by the particles num-
ber density increase and the matrix ligament thickness
decrease, Table 1.
The ultrasound attenuation of the neat and filled SBR con-
taining 10 wt % of dense and hollow PS particles with dif-
ferent sizes is presented in Figure 6. Despite decreased
85
JOURNAL OF POLYMER SCIENCE: PART B: POLYMER PHYSICS DOI 10.1002/POLB
FIGURE 5 Normal sound absorption coefficients of the neat SBR (a) and SBR filled with 80 nm (b), 250 lm (c) and 500 lm (d)
monosize polystyrene particles.
matrix viscoelastic attenuation in the filled systems, their
attenuation coefficient rose monotonically with the dense PS
particle size increase. This could be assigned to additional
energy dissipation due to wave scattering from the dispersed
particles. The contribution of wave scattering mechanism is
most significantly influenced by the particle size to wavelength
ratio (d/k) as well as the acoustic mismatch between the dis-
persed particles and the matrix.17,18 Considering the similarity
of acoustic mismatch for all filled samples, the particle size to
wavelength ratio is the key controlling factor of the scattering
FIGURE 6 The influence of particles size and morphology on
ultrasound attenuation of filled systems.
86
loss contribution. To evaluate the influence of this factor quan-
titatively the scattering attenuation was correlated with the
particle size to wavelength ratio, Figure 7. Scattering attenua-
tion (asca) for each sample was derived by subtracting the ma-
trix attenuation (am) from the composite attenuation (am):
asca ¼ a  /m am (3)
where /m is the matrix volume fraction. The ultrasound
wavelength inside the filled systems was calculated 421 lm
FIGURE 7 Scattering attenuation versus particle size to wave-
length ratio of the rigid polystyrene particle filled systems.
INTERSCIENCE.WILEY.COM/JOURNAL/JPOLB

FIGURE 8 Normalized attenuation of the neat SBR and PS par-
ticle filled systems in different regimes of mechanical waves.
(k ¼ cf1) assuming the longitudinal phase velocity to be
unaffected by the presence of particles. To avoid mathemati-
cal complexities in calculation of scattering cross-section,16,17
a simple power equation was fitted to the experimental data,
Figure 7. Least square fitting procedure yielded the scaling
law asca
(d/k)0.38 in the studied range. This relation clearly
indicates the increasing contribution of scattering loss mech-
anism as the particle size to wavelength ratio grows to unity.
It is interesting to note that the variation rate of asca is
higher for smaller values of d/k and tends to level off as d/k
approaches unity and grows higher. The above trend did not
hold for EPS filled systems as they showed lower attenuation
despite greater particle size. The lower sound attenuation
might be originated from lower density of the EPS particles
(q  0.92 g/cm3), which reduced the acoustic mismatch and
resultant scattering loss.
Normalized energy dissipation of monosize polystyrene
particle filled systems in different regimes of mechanical
waves is summarized in Figure 8. In the vibration regime,
addition of PS particles with different sizes did not improve
the energy dissipation capacity so much. Taking the samples
to the acoustics domain differentiated the filled samples in
two distinct directions. The sound absorption capacity was
magnified by inclusion of nanosize rigid particles. However,
ultrasound attenuation capacity was improved by increasing
particle size to the micron range. The observed trends of
attenuation capacity are originated from different major
energy dissipation mechanisms effective in various regimes
of mechanical waves.
CONCLUSIONS
It was observed that the matrix glass transition characteris-
tics in rigid particles filled samples were dominated by ma-
trix-particles interfacial properties. Addition of rigid particles
with high surface area imparted additional dynamics hetero-
geneity to the matrix and consequently extended the matrix
glass transition toward higher temperatures. Although the
matrix viscoelastic state at applied acoustic frequencies was
EFFECTS OF RIGID POLYSTYRENE PARTICLES, FAGHIHI, MOHAMMADI, AND HAGHGOO
ARTICLE
not affected by the rigid particles, acoustic attenuation of the
filled systems was significantly modified in comparison with
the neat SBR. Additional peak appeared in the sound absorp-
tion spectra of the filled systems at frequencies lower than
the matrix absorption. The intensity of the secondary peak
was much more pronounced in the nanofilled sample. By
increasing the applied wave frequency to the ultrasonic
range, inverse trend was found in the variation of normal-
ized attenuation with PS particle size. It was attributed to
the contribution of the scattering loss mechanism which fol-
lowed the scaling law asca
(d/k)0.38 in the range of studied
particle size to wavelength ratio. Furthermore, ultrasound
attenuation coefficient was decreased in the filled samples
containing hollow PS particles, due to their lower acoustic
mismatch with the matrix phase.
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88 INTERSCIENCE.WILEY.COM/JOURNAL/JPOLB