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Laboratory Investigation of Modified: Polymer Bitumens
Laboratory Investigation of Modified: Polymer Bitumens
ABSTRACT
This paper deals with laboratory characterization of various pure and polymer
modified bitumens, in which five bitumens from four sources and six polymers of different
types were used. The effects of base bitumen and polymer type and content on compatibility,
storage stability, rheology and aging were investigated. The results indicated that
compatibility and storage stability of polymer modified binders were largely dependent on
polymer content and were influenced by the charncteristics of base bitumens and polymers.
Polymer modification increased the elastic responses and dynamic moduli of bitumens
at intermediate and high temperatures, and influenced complex and stiffness moduli at low
temperatures. It also reduced the temperature susceptibility and the glass transition and
limiting stiffness temperatures of birumens. The degree of the improvement generally
increased with polymer content, but varied with bitumen sourceJgrade and polymer type.
Artificial aging may cause oxidation of bitumen and degradation of polymer, and
consequently, change the microstructure and rheological properties of the modified binders.
These changes were largely influenced by polymer nature and content. Due to temperature
and frequency dependence, aging index is not a suitable parameter for characterization of
aging susceptibility of polymer modified binders.
The effectiveness of polymer modification as reflected by different testing parameters
may vary considerably. The usefulness of empirical test methods (e.g. penetration, softening
point and Fraass breaking point) for characterizing polymer modified bilwnens is discussed.
To predict significant benefit from polymer modification in practice, it is necessary to use
appropriate and fundamental pararnetm .
INTRODUCTION
Materials
Five base bitumens, denoted A, B, C, 0 and E, were used in this study. They were
obtained from Venezuela (Laguna), Mexico, Saudi Arabia and Russia, respectively. The
physical properties of the bitumens are given in Table I.
Bitumen code
Gn'"
Soo~,
Penetration 5C, dmm
A
885
Venezuela
84
8
BISo
Venezuela
113 18.
C
BISo
Mexico
149
_.0
BI80
E
BI80
Russia
'81
Softening point C "J 46.0 ]S.S 41.0 42.8 44.3
Viscosity (al 1]5C, mm2fs (e) 3S4 21. 208 236 172
fraus breakin~ point, C to/ ·11 ·16 ·17 ·16 ·22
p, • -1.00 -0.89 -0.09 -0.10 1.29
PVN -0.60 -0.53 -0.57
. -0.59 -0.85
,.' ' '
• ASTM 0 5, ASl M0 3,6' (e) ASTM 021 0, IP 80,. Penetration mdex (8), Penetration
vi5(:osity number (9). '" '"
The polymers investigated are styrene-butadiene-styrene (SBS), styrene-ethylene-
butylene-styrene (SEBS), ethylene vinyl acetate (EVA) and ethylene butyl acrylate (EBA)
copolymers. The SSS polyme~ used are powdered ](raton D-1I01 and Kraton D-1184,
supplied by the Shell Chemical Company. Kraton 0-1101 is a linear SBS polymer containing
31 percent styrene, and Kralon-1184 a branched polymer containing 30 percent styrene. The
SEBS polymer is Kralon G 1650 (Shell), which contains 29 percent styrene. The two EVA
copolymers used are Elvax 260 (EVA I) and EJvax 420 (EVA2), supplied by DuPont. Melt
indices (MI) of Elvax 260 and Elvax 420 are 6 and ISS, and their vinyl acetate contents are 2S
and IS percent, respectively. The EBA polymer was produced by Neste and supplied by
Nynas Petroiewn.
Polymer modified bitwnens (totally 36) were prepared using a low shear mixer (RW
20 DZM-P4, Janke & Kunkel) at ISOC and a speed of 125 rpm. The polymer contents used
were ], 6 and 9 percent by weight of blend. In preparation, 600 g of the bitumen was heated to
fluid condition and poured into a 2000 ml spherical flask . Upon reaching 175C, a preweighed
amount of polymer was added to the bitumen. Mixing was then continued at ISDe for two
hour.;. After completion, the polymer-bitumen was removed from the flask and divided into
l
small containers. The blend was cooled to room temperature, sealed with aluminium foil and
stored for further tesling. The process for preparing the modified binders exposed the bitumen
to high temperature and air for an cxtended lime, which led to hardening of the bitumen. For
the accurate evaluation of polymer effects, the base bitumens were also subjected to the same
treatment as the polymer-bitumen blends.
Fluorescence Microscopy
Fluorescence microscopy was used to study morphology (compatibility) of polymer
modified binders. The modified binder was illuminated using a blue light for excitation and
the fluorescent yellow light re-<:mitted by the swollen polymer phase was observed using an
optical microscope. The instrument (Leitz, LABORLUX II) was equipped with a Polaroid
camera and a blue filter system. The wavelength of excitation is in the range 390 to 490 MI.
Squashed slides of modified binders were prepared using very small amounts of the heated
sample and viewed under the microscope with a magnification of250 at room temperature.
_.
"' _ f _
!
; I .... /
ru:
- GPC
Bitumen Code A B C 0 E
Saturates % 11.3 13.0 10.4 10.9 16.9
Aromatics % 54.7 56.4 64.8 63.6 51.1
Resins % 18.7 17.3 III 14.8 18.3
Asphahenes (% J 5.4 III 11.1 10.7 J]J
Molecular weight, M. 650 600 750 140 720
Molccular weight. M. ])00 ])00 1400 1300 1800
Polydispmiry (MJM.) 1.1l6 2.08 1.84 1.80 2.49
l 11 11
Fraction with Mw >2.Sxl0 (%) IJ II 18
70
55J
17.2
85.1
·16
·17
· 19
2.70
5.61
5.95
0.40
1.10
2.44
B + 6Y, branched SSS 2390 84 82.5 ·18 6.14 2.24
B+ J!/tSE8S 577 III 58.0 ·19 lOS 0.48
8 + 6Y, SE8S 1630 61 66.8 ·18 2.84 L22
B +9Y. SEBS 3950 46 78.S ·ll 3.90 2.05
8+3%EVA I
8 +6%EVAI
469
1140
141
97
42.2
53.4
."
·20
.(l.61
1.48
0.48
IJ'
B+ 9%EVAI 2970 76 59.8 ·19 2.15 2.40
B+3% EVA2
B+6%EVA2
342
602
129
96
46.8
57.4
."
·20
0.64
2.39
-0.16
0.35
B+9%EVA2
B+)%EBA
1070
472
77
121
64.4
51.6
."
·20
3.10
1.80
0.9)
0.28
8 +6%EBA 1180 82 70.2 ·18 4.33 1.16
8 +9'hIEBA
Bitumen C
3040
237
61
151
77.8
41.5
."
·16
4.58
.{l.44
2.10
-0.51
C + )% linear SSS
C + 6% linear SBS
C + 9% linear SBS
461
])50
3450
.
120
67
51.2
77.2
85J
· 18
·20
·20
1.60
5.61
5.81
0.23
1.45
2.42
C + 6% branched SBS
C+6%SEBS
3890
1490
89
67
85.4
70.5
."." 6.12
3.74
3.06
1.22
C+6%EVAI
C+6%EVA2
C + 6Y. ESA
940
584
1080
.
100
n
57.7
59.8
7J.l
."
·21
·20
2.60
2.62
4.06
1.09
0.20
0.85
Bitumen D 250 110 41 0 ·1 6 -0.6 1 -0.66
D + 6% linear SBS 1220 80 75.2 ·19 5.00 1.17
D + 6% branched SBS 4360 77 84.0 ·19 6.12 2.98
Bimmen E 187 166 44.0 ·ll 0.72 -0.85
E+ 6% linear SBS 1640 70 75.2 ·26 4.58 1.4\
.
E + 6Y. branched SSS 3220 69 81.5 ·25 5.52
The but bitumens have been subJet!ed to the same treatment IS the polymer.bitumen blends .
2.37
Compatibility and Storage Sillbilily
Fluorescence Microscopy Studies Due to the chemical dissimilarity (e.g. differences in
molecular weight, polarity and structure) between bitumen and polymer, most of the modified
binders obtained by mechanical mixing are thermodynamically immiscible. In describing
such systems, the term ~compati bility" is often used. Compatibility can be defined as the slate
of dispersion between two dissimilar components. The property was studied using
fluorescence microscopy by characterizing the nature of the continuous phase and the fineness
of the dispersion of the discontinuous phase. At room temperature and a magnification of 250,
the modified binders may show either a continuous bitumen phase with dispersed polymer
particles or a continuous polymer phase with dispersed birumen globules, or two interlocked
continuous phases. as illustrated in Figure 2.
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The morphology (compatibility) is the result of the mutual effect of polymer and
bitumen, and consequently is influenced by bitumen composition and polymer nature and
content. In general, at a low polymer content, the small polymer spheres swollen by bitumen
compatible fractions (e.g. aromatic oils) are spread homogeneously in a continuous bitumen
phase. Compared with 3 percent elastomer (SBS and SEBS) modified binders, those
containing thermoplastics (EVA and EBA) of the same polymer conlent revealed much finer
dispersion of the polymer. Belter dispersion of the polymers was also observed for the
modified binders prepared from the bitumens with higher aromatic and lower asphaJtenc
contents. By increasing polymer content, a continuous polymer phase may be obtained
(Figure 2). The minimum pcrcentagl! of polymer to ensure the fonnation of its continuous
phasc depends to a great extent on the base bitumen and the polymer itself. In most cases,
•
appearance of a continuous polymer structure was observed to begin a\ a polymer content of
about 6 percent.
The morphology should also be influenced by testing temperature, This means that the
morphology of polymer modified binders observed at ambient temperature does not
necessarily reflect thai at high temperatures.
Phase Separalion Polymer modified binders may separate inlo JXllymcNich and
asphaltene·rich pbases during hot storage. The phase separation has been CQnfirmcd by
tluorescence micrographs and Fourier Transform Infrared Spectroscopy (FTJR) of the
modified binders before and after lube storage al 180C for three days (\ 0). The two phases
differ widely in their rheological properties and chemical constitutions. In this study, the
logarithm of the ratio of complex modulus (DMA al 25C) of the asphaltene·rich phase to that
of the JXI1ymer-rich phase is defined as the separation index, I" and is used to evaluate the
slorage stability of the modified binders (Figure 3),
\.ooE+09 r - - - - - - - - - - - - - - - - ,
--Bilumen A + 6% lOB'" bc:fln stonge
, l.ooE+08 - . _. Top sroion iIfIa storage
••• • •• Bottom sectiOll after $Iorage
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I.00E+{I1 L_~~=_~~~~~~~....J
l.ooE-01 l.ooE+OO I.(IOE+OI l.ooE+{I2
The investigation indicates that the storage stability decreases with increasing polymer
content. For the modified binders with a low content of polymer (3 percent), almost no phase
separation (I, close to 0) was observed. The storage stability is also influenced by
characteristics of the base bitumen and the polymer. Higher content of aromatics and/or lower
content of asphaltenes are observed to be favourable with regard to storage stability, as
illustrated in Figure 4. Among all the modified binders prepared, the modified binders with
EBA display the lowest storage stability. For the elastomer (SBS and SEBS) modified
binders, those containing branched SBS show the lowest storage stability, For the EVA
modified binders, better storage stability is observed for those containing the polymer with
lower VA content and higher Mr.
The storage stability wa~ also assessed by softening point. Unfortunately, the
conventional evaluation did not show any correlation with DMA method. This implies that
different conclusions could be drawn from the storage stability if using different evaluation
methods.
9
Since many polymer modified bitumens display a tendency towards phase separation,
some agitation is recommended during the storage of hoI blends. However, such a measure
should not be taken wilhoullimil and at the expense of the oxidative degradation of polymers.
2' ,-------~~~-.
2' ,-----__________,
O·''IIINIrSES O' nlftMS8S
,. . · n~SBS
2.' " ''''_sas
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50.0 SSO 600 6S 0 700
'---~-----------'
LO.O ,,. ...
CMI..L" ",.",,"II..n 1% . , ••",
.
,
Figure 4 Relationship between the SeparttioD Index (at 1 radls) orSBS Modifi ed
Binder! lod Bitumen Composition
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than 75° is denoted T11' , and used to quantitatively compare the clastic response of the
binders. II was observed thai polymer modification increased T15' of the binders. and the
improvement may increase with polymer content. The improvement is also dependent on the
base bitumen and polymer Iype. The innuence of the polymers tested may be ranked as
branched SBS, SEBS/linear sas. EBA, EV A2 and EVA I, branched sas being the most
II
effective. This temperature is observed 10 statistically correlate with the softening point, as
illustrated in Figw-e 6. For all the binders studied, the correlation coefficient obtaioed is 0.95.
However, al the softening point, all the base bitumens are purely viscous, as indicated by
phase angles of 90°, while the modified binders still display considerable elasticity. This
observation suggests that the softening point is related to dilTerent properties when applied to
pun: and polymer modified bitumens.
., 70 80
JO
" " Soflnln~ Point [OC1
90 100
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Figure 8 C·/sinS as a Fundion of Frequency (at 60C) and Temperature (It 1 rad/s)
15 r---------------------,
10 •
R'" O.U
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R" o.as
5 R " O.93
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35 55 65 75 85 95 105
Sobnln" Poin t reI
Figure 9 Relationship between G"sino (at 10 radls and 60C) and Softening Point
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Low-Tempuafure Propertits
For a flexible pavement, one of the failure modes is low-temperature cracking. This
occurs when the Ulenna] stress induced at low temperatures exceeds the tensile strength of the
asphalt pavement. Low-temperature cracking can be a serious problem in cold areas. To
reduce the risk of crack.ing, the binder should have good flexibility (low stiffness and complex
modulus and high ability of stress relaxation) at the lowest pavement temperature. In this
paper, the influence of polymer modification on the low.temperature properties of bitumens is
studied using DMA and BBR.
DMA CharaclerizaliQn The DMA observations indicate that, in low temperature
regions (below OC), all the modified binders show a lower complex modulus titan the
corresponding base bitumens. However, the glassy modulus G,· of the binders is close to I
GPa and insignificantly influenced by polymer modification. This value of glassy modulus
reflects the rigidity of the carbon hydrogen bonds as the bitwnens reach their minimum
thennodynamic equilibrium voiwne {i4}.
B tllalllU Codt
0
A
• C
-j
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-15
": ·20
..<•
;; ·25
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• -35 .bo.sc ~il"",." 9 • 6% Ii,",,,, sas o• 6% br,"ciltd SBS
-40 O~6%SEBS Q '6%EVAI 1I'!I' 6%EVA2
1iI ~6%EBA
-45
i
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_
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..... .. "'...
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--_ .........-
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• ..II
A
•• L_~_~~~~_---'
51 100 151
LoM,..T·· I-!
180 150
•
Figure 12 Creep Responses orthe Base Ind SEOS Modified Bitumen 0 at -2SC
Table 4 indicates that polymer modified binders generally display a lower creep
stiffness than the corresponding base bitumen, especially at temperatures lower than ·15e.
The improvement increases with polymer content, but varies with the base bitumen and
polymer type. At ·35C and for a given polymer content, the modified binders containing
elastomers (SSS and SEBS) show a higher reduction in creep stiffness than those with
thermoplastics (EVA and EBA). However, al the other three low temperatures, varying
changes are observed in the creep stiffness. Some modified binders (e.g. bitumens A and B
modified with SEBS) even show an increased creep stiffness at ·15C. Moreover, the usc of a
softer bitumen seems favourable for reducing creep stiffness (cf. B85 and BI80). As a result
of the reduced creep stiffness, the modified binders exhibit a lower limiting temperature (by
definition, the temperature at 300 MPa creep stiffiless) than the base bitumens. However,
degree of the improvement is comparatively low. As regards the effect of polymer
modification on binder stress retaxation ability, both increased and decreased m·values are
observed, depending on the testing temperature and loading time. Therefore, no definite
conclusions could be drawn on this mailer.
Table 4 Cmp Stiffness and m-value of the Binders at a Loading Time of 60 sec anti
Dirrerent Temperatures
Tempua(ure SlISctptibility
Temperature susceptibility of the binders is one of the important parameters
detennining asphalt perfonnance in road service. Asphalt mixtures containing the binders
with lower temperature susceptibility should be more resistant to cracking and rutting at low
and high temperatures, respectively. Temperature susceptibility is usually defined as the
change in binder properties as a function of temperature. Since binder properties may be
characterized by means of various parameters, different approaches have been proposed to
evaluate temperature susceptibility. Traditionally, temperature susceptibility is quantified
through consistency measurements made at two different temperatures. Two classical
methods are the Penetration Index, PI, and Penetration Viscosity Nwnber, PYN. Lower values
of PI and PVN indicate higher temperature susceptibility. The results obtained (Table 3) show
that the classical parameters are improved by polymer modification. For all the binders, PI
may statistically correlate with PVN (R = O.S3). However, the temperature susceptibility of
binders may be ranked differently by PI and PVN. As mentioned earier, tests of penetration
and softening point are empirical and, in principle, only valid for unmodified bitwnens.
Consequently, conventional temperature susceptibility parameters such as PI and llYN are
probably not relevant indicators in the case of polymer modified binders.
In DMA, the temperature susceptibility of binders may be evaluated by measurements
of various viscous and elastic parameters at different temperatures and frequencies.
Observations described earier indicate that polymers modify the rheology of bitwnen.
Through polymer network and/or crystallinity, the modified binders become more elastic and
less temperature susceptible over the nonnal service temperature range compared 10 the base
bitumens (Figure S). AI high temperaltU"es, however, the polymer modified binders are likely
to cxhibit temperature susceptibility that is the same as, or slightly higher than, thaI of the
base bitumens. This is a result of the weakening and dissociation of the polystyrene domains
(SSS and SEBS) or the melting of Ihe crystalline portions (packed polymer segments of EVA
and EBA). To perfonn an evaluation similar 10 viscosity temperature susceptibility (VTS)
(16), the double logarithm of complex modulus, complex viscosity (,, ' .. O'/ro) and dynamic
viscosity (,,' = GM/Il) was plotted against the logarithm of temperature in K for both
unmodified and modified binders. Unfortunately, these plots were not straight lines over a
wide temperature range, and the slope (temperature susceptibility) changed with the
temperature range being considered. This means that temperature susceptibility cannot be
evaluated as a single-valued parameter such as VTS.
Aging Properties
Aging of the binders was perfonned using the Thin Film Ovcn Test (TFOT, ASTM D
1754) and the Rolling Thin Film Oven Test (RTFOT, ASTM D 2872), respectively.
Aluminium pans (TFOD and glass containers (RTFOD were heated to 160C before loading
the sample. The sample holders were kept in an oven at 160C for about IS minutes (RTFOT
"
glass containers in horizontal position) and then aged according 10 the standardized
procedures: 163C and 75 minutes for RITOr and, 163C and 5 hours for TFOT, The aged
binders were evaluated by measuring their rheological properties.
Figure I) reveals the viscoelastic changes oflhe binders after aging. AI the frequency
studied ( I radls), aging increases the complex modulus of the base bitumens. However, the
innuence of aging on polymer modified binders is temperature dependent. For the base
bitumens and modified binders with 3 percent SSS, as well as those containing
thermoplastics, the elastic response was slightly increased by aging, as indicated by a small
decrease in phase angle in a temperature range of 0 10 about 7OC. In contrast, when aging is
performed on the modified binders with 6 or 9 percent SBS and SEBS, large increases in
phase angle were observed at high temperatures, and consequently, the depth of the phase:
angle minimum is reduced, which would imply polymer network damage.
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Figure 13 Effect of RTFOT Aging on Tempel'lllture DependeD~e of Complu Modulus
and Pbase Angle
and bitumen is changed, as shown in Figure 15. On the other hand, breakdown of polymer
reduces the number of large polymer molecules, and consequently, the effectiveness of the
polymer in significantly modifying bitumen rheology is reduced. Obviously, the rheological
changes in aged modified binders are dependent on a combined effect of bitumen oxidation
and polymer degradation, which varies with types of bitumen and polymer, as well as
polymer content.
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Figure 14 Complex ModulU5lnd Phase Angle It 60C as I Funttion or Frequenty Cor
Base and Polymer Modified Bitumen B berore Ind after RTFOT
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~ ~ G 10 ~ ~ ~ ]00 ]M ]~ 1.00&-411 1.00£+«1 I.OOE+Gl
Tom"".. t." for Mouori"1 AItiDJ: ladn t"tl
CONCLUSIONS
ACKNOWLEDGEMENTS
The authors wish to thank Jonas Ekblad, Britt Wideman and Clarissa Villalobos for their
laboratory assistance. The authors also gratefully acknowledge the Swedish Transpon and
Communications Research Board (KFB) for the financial support of this study, and Nynas
Petroleum for supplying a number ofbase bitumens and polymers.
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