MULTI-DEFORMATION MODE PREDICTION OF TIRE TREAD

COMPOUND PERFORMANCE

Control No: N/A Requested by: Charles Herd

Reference No: LS-24657, LS-24904 Prepared for: NPD
RCB TECHNOLOGY Date Initiated: January 8, 2016 Date Issued: May 11, 2016
MARIETTA, GEORGIA Lewis Tunnicliffe, Specialist, RCB Product Technology
USA Prepared by: John Curtis, Chemist II
Aiying Wang, Chemist
Technical Report
Reviewed by: Zac Combs, Specialist, RCB Product Technology
Confidential
Approved by: Charles Herd, Director, RCB Product Technology

EXECUTIVE SUMMARY:
Tread compounds reinforced with N234, silica, and CD2125XZ fillers were prepared and tested in multiple dynamic
deformation modes. Tread compound preparation is detailed in LS-24657. The dynamic test methods are detailed in LS-24904.
The resulting data were used to correlate viscoelastic properties of the compounds across a range of strains and temperatures
with tire tread performance according to the ‘deformation index’ principle (background overview provided in this document).
Spider plots of compound performance showed a clear difference in behavior between N234 and silica-based compounds. The
silica compound was predicted to have improved performance in terms of rolling resistance, winter, and ice traction. The N234
compound out-performed silica in terms of predicted dry handling and dry traction. CD2125XZ/functionalized SBR compounds
lay somewhere between the performance of silica and N234 compounds depending on the processing route. Single step reactive
mixing produced CD2125XZ compounds with the most ‘silica-like’ predicted performance. Masterbatch blending routes
produced compounds with the most ‘N234-like’ performance. Spider plots of predicted performance offer an intuitive way to
assess the impact of mixing procedure on compound viscoelasticity and, potentially, tread performance. The nature of the
processing route seems to offer opportunities for tailoring the predicted performance of CD2125XZ compounds for a specific
application – for example winter tires versus summer tires.

OBJECTIVE:
This report builds on previous work (LS-24904 and LS-24657) on a series of tread compounds prepared using N234 carbon
black, precipitated silica (Solvay Zeosil 1165) and CD2125XZ functionalized carbon black. The goal of this work is to extract
differences between viscoelastic behavior (and hence possible tread performance) of the various filler systems.

SAMPLE IDENTIFICATION:
Test compounds, mixing procedures, cure conditions, and standard physical data are fully documented in LS-24657. A summary
of the test compounds and mixing procedure is given in Table I. PBR4088 is a functionalized SBR supplied by Lanxess, MBB
refers to masterbatch blending.

Table I: Summary of test compounds

Test compound name Reactive/normal mixing A-number
N234 SBR/BR Normal A-72982
Silica SBR/BR Reactive A-72983
CD2125XZ PBR4088/BR Reactive A-72984
MBB CD2125 PBR4088/BR Reactive masterbatches A-72985
MBB CD2125 PBR4088/N234 BR Reactive masterbatches A-72986
Preblend CD2125XZ PBR4088/N234 BR Reactive A-72987
 LS-24904
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EXPERIMENTAL:
Materials were tested in three deformation modes: rotational shear, double shear, and compression. The test methods are fully
defined in LS-24904 initial report. A summary of the test methods for the various deformation modes is presented in Table II.

Table II: Summary of deformation modes, test types and test conditions
Deformation
Test equipment Test type Thermal conditions Strain conditions
mode
Strain sweep Isothermal at 60°C 0.1-65% logarithmic,
ARES 10 Hz
Rotational shear
Rheometer Temperature sweep 70→-10 °C, 10 K steps 4% (-10→40°C),
7.5% (50→70°C)
Strain sweep Isothermal at 60°C 0.15-25%
MTS
Double shear logarithmic, 10 Hz
Servohydraulic
Temperature sweep 70→-10 °C, 10 K steps 2%
Strain sweep Isothermal at 60°C 0.2-25%, 10 Hz, 15%
MTS
Compression mean strain
Servohydraulic
Temperature sweep 70→-10 °C, 10 K steps 2%

EQUIVALENCE OF COMPRESSION AND SHEAR DATA:

Rubber materials are nearly incompressible with a Poisson’s ratio, 𝑣, approaching 0.5. The relationship between shear and
tensile moduli is a function of the Poisson’s ratio and is given by Equation 1:
𝐸 (1)
𝐺=
2(1 + 𝑣)

For the case of 𝑣 = 0.5

𝐸 (2)
𝐺=
3
This holds at small strains for most rubber compounds (foamed rubber compounds being an obvious exception). A complication
arises when performing testing in compression mode. Here the measured modulus is influenced by the constrained nature of the
sample specimen. Frictional adhesion or chemical bonding of the (cylindrical) sample to the compression plates results in a non-
homogeneous strain field across the sample, which raises the measured compressive modulus value due to purely geometrical,
non-intrinsic issues1. Assuming full bonding of the cylinder samples to the compression plates, the measured compressive
modulus, 𝐸𝑐 , can be related to the shear modulus by Equation 3:
𝐸𝑐 = 3𝐺(1 + 2Scylinder 2 ) (3)

where 𝑆cylinder is the shape factor of the cylinder given by the ratio of then unconstrained to constrained (bonded) surfaces:

𝑑 (4)
Scylinder =
4ℎ
Where 𝑑 is the cylinder diameter and ℎ is the cylinder height.

For the cylindrical compression samples used in this study, the calculated shape factor is quite low (0.17) resulting in a deviation
from the Poisson’s ratio relationship of less than 6 %. This shape factor effect was ignored during data analysis.
A further complication arising from the compression test mode is the requirement to apply a mean strain or pre-compression to
the sample. For practical reasons, a mean strain is required to ensure full contact between plate and sample during cyclic
deformation. The viscoelastic properties of filled rubbers are highly dependent on the level of mean strain. This is because the
modulus is defined by a partial unloading of the static stress strain curve as shown schematically in Figure 1. It should therefore
be expected to see some differences between the data collected in compression and in the two shear modes as a result of the
significant mean strain applied to the compression samples (15 %).
 LS-24904
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Figure 1: Schematic of a dynamic test performed on a filled rubber subject to a static mean strain. The dynamic modulus is a
function of the steepness of the static unloading curve, which depends on the level of mean strain (i.e. the Mullins effect). Image
reproduced from Reference 2.

In practice, a good correlation was found between rotational and double shear modes of testing  (See LS-24904 for an extended
discussion and associated correlation plots). Applying Equation 2 to the compressive moduli data generally resulted in a
reasonable correlation between all deformation modes. An example of this agreement is given in Figure 2 for temperature
sweep data for the control material (N234 SBR/BR).

45
ARES Rotational Shear
40
MTS Double Shear
35
Modulus G', E'c / MPa

30 MTS Compression

25
MTS Compression / 3 = G'
20

15

10

0
-20 -10 0 10 20 30 40 50 60 70 80
Temperature / °C

Figure 2: Dynamic moduli collect for the control material (N234 SBR/BR) in all deformation modes. Reasonable correlation is
found between shear modes and compression


Note on rotational versus double shear modes: it is important to note that in the double shear deformation mode, the strain is homogenous
throughout the test sample. In rotational shear mode, the strain depends on the radius of the sample: 𝛾 = 𝜃 𝑟⁄ℎ - where 𝜃 is the rotational
angle, 𝑟 is the sample radius and ℎ is the sample height. Therefore, torsional strain is non-homogeneous within the sample. Reported values
of dynamic moduli from rotational shear testing are therefore only strictly precise in the linear viscoelastic regime.
 LS-24904
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TIRE PERFORMANCE PREDICTORS - BACKGROUND:

Tire components undergo complex deformations, which are operating-condition specific. Since the tire tread is a viscoelastic
material, the performance of the tread is related in a non-trivial way to the viscoelastic spectrum of the tire tread. During a given
deformation, the energy loss or hysteresis of the deformation cycle is a key parameter defining the performance of the tire. In
some deformation cases, the damping factor, tan δ, dominates hysteresis; in others it is the modulus or compliance that dictates
the magnitude of energy loss through the degree of extensibility of the materials under a given loading 3. It is necessary to define
parameters that can reasonably correlate tread viscoelasticity as measured in the lab to actual tire/tread performance measured
under controlled conditions. A complication is that the relevant state of deformation experienced by the tread varies depending
on operating conditions – for example steady rolling deformations versus dry/wet traction deformations. In practice,
deformations can be split into those controlled by applied strain, those by applied stress and those by applied energy or
combinations thereof. Futamura4 highlighted the problems this can cause when considering the amount of energy dissipation
between two compounds. He used the case of two tread compounds of differing moduli but equivalent tan δ. In this case, the
amount of energy dissipated per cyclic deformation depends on the deformation control. This is illustrated in Figure 3, which
shows the cyclic behavior of two materials with different moduli but equivalent tan δ.

Figure 3: Schematic of the role of deformation control on the total hysteresis of deformation. The mechanical response of two
materials with differing moduli but equivalent damping is plotted for deformation at equal strain, energy, and stress. The total
hysteresis of the deformation (blue shaded areas) of each material ranks differently depending on the deformation control. Image
reproduced from Reference 5.

The key question when considering correlation between viscoelastic properties and tire performance is what is the appropriate
deformation control (or combination of controls) that best describes the deformation of the rubber. Only once this is known can
the viscoelastic parameter that defines total deformational hysteresis during operation be determined.
The energy loss, 𝐸𝑙𝑜𝑠𝑠 , of a material under cyclic deformation under either strain or stress control is defined by Equation 5:

𝐸𝑙𝑜𝑠𝑠 = 𝜋𝜀0 2 𝐸 ′′ = 𝜋𝜎0 2 𝐽′′ (5)

where 𝜀0 is the applied strain and 𝐸 ′′ is the dynamic loss modulus for the case of strain control, 𝜎0 , is the applied stress and 𝐽′′ is
the dynamic loss compliance for the case of stress control.
From linear viscoelastic theory, the loss compliance can be defined in terms of the dynamic moduli by Equation 6:

𝐸′′ 1/𝐸′′ (6)

𝐽′′ = =
(𝐸′2 + 𝐸′′ ) 1 + (tan2 𝛿)−1
2

Given that 𝐸 ∗ = 𝐸 ′ + 𝑖𝐸 ′′ , it is possible to define the energy loss of the deformation process in terms of a “deformation index,”
the magnitude of which defines the control of the deformation (i.e. stress or strain control). This is presented as defined by
Futamura3 in Equation 7:
𝐸′′ (7)
Energy loss of deformation process = D +F
(𝐸 ∗ )𝑛

where 𝑛 is the deformation index of value between 0 and 2 and D and F are constants that define the geometrical design of the
tire and other sources of energy dissipation. The solutions to Equation 7 for various integer values of 𝑛 are given in Table III.
Non-integer values of 𝑛 indicate combinations of the three key deformation controls.
 LS-24904
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Table III: Form of Equation 7 for different values of deformation index and the corresponding appropriate mode of deformation

Integer value of 𝑛 Form of Equation 7 Mode of control

2 𝐸′′ Stress
= 𝐽′′
(𝐸′ + 𝐸′′2 )
2

1 𝐸′′ Energy
= sin𝜎 ≅ tan𝛿
𝐸∗
0 𝐸′′ Strain

Fukamura4,5 showed that by performing a linear regression between a measured tire performance indicator (e.g. rolling
resistance) and the energy loss equation calculated using measured material viscoelastic parameters using varying values of 𝑛, it
is possible to define the mode of deformation and therefore the appropriate viscoelastic parameter that best correlates with tire
performance. Such an example is presented in Figure 4, which shows the coefficient of correlation between tire performance
and energy loss (Equation 7) calculated from viscoelastic parameters with varying deformation index values, 𝑛, for wet and dry
traction performance. Maxima in the correlation curves correspond to the appropriate value of 𝑛 describing the deformation
mode.

Figure 4: Plot of correlation coefficient versus deformation index for dry (dashed line) and wet (solid line) traction. Reproduced
from Reference 4.

As can be seen from Figure 4, the 𝑛 value best describing the deformation mode for dry traction is ~1.8, which indicates a
stress-dominated deformation best described by the loss compliance at the appropriate temperature. Conversely, wet traction is
best correlated with viscoelastic parameters at an 𝑛 value of 0. This indicates that wet traction is predominantly a strain
controlled deformation mode, which necessitates a correlation with the dynamic loss modulus. These correlations are borne out
in practice. Note: there are reports in the literature for good correlations between wet traction and both the loss modulus and loss
compliance6. It has also been suggested to use the loss compliance to characterize wet traction in cases where the coefficient of
friction between road and tread is low and the loss modulus in cases where it is high7. This suggests a switch between
deformation mechanisms (stress and strain control) depending on the coefficient of friction 8. The tire performance indicators
used in this correlation report are detailed in Table IV.
 LS-24904
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Table IV: breakdown of tire performance indicators used in this report, their condition of measurement and the desired trend of
the indicator versus the control compound for performance improvement

Performance Property
Performance Indicator Condition Reference
Parameter Improvement
Rolling resistance tanδ 5 % strain, 60 °C, SS* Reduction 5
Dry handling Storage modulus, G’ or Ec’ 5 % strain, 60 °C, SS Increase 8
Dry traction Loss compliance, J’’ 5 % strain, 60 °C, SS Increase 4
Wet traction: high Loss modulus, G’’ or Ec’’ 2 % strain, 0 °C, TS** Increase 4,6,7,8
coefficient of friction
Wet traction: low Loss compliance, J’’ 2 % strain, 0 °C, TS Increase 6,7,8
coefficient of friction
Ice/winter traction Storage modulus, G’ or Ec’ 2 % strain, -10 °C, TS Reduction 8
*SS = strain sweep **TS = temperature sweep

PERFORMANCE INDICATOR SPIDER PLOTS:

All data are normalized and suitably presented so that an increase in the magnitude along the performance index axis
corresponds to an improvement in the compound performance. The N234 SBR/BR compound is the control compound and all
compound values are normalized to the performance of this compound.
The spider plots are prepared in two ways. First, the predicted performance indicators make up the axes and the compound data
are plotted out and differentiated by line color. Second, the individual compound performance scores make up the axes and the
performance data are plotted out and differentiated by line color.
 LS-24904
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Rotational Shear Mode

Rolling
Resistance
1.8
1.6
1.4 N234 SBR/BR
1.2
Winter/Ice 1 Dry handling
Traction 0.8 Silica SBR/BR
0.6
0.4 CD2125XZ PBR4088/BR
0.2
0
MBB CD2125XZ PBR4088/BR

Wet Traction MBB CD2125XZ PBR4088/N234 BR

Dry Traction
Low Friction
Preblend CD2125XZ PBR4088/N234
BR

Wet Traction
High Friction

N234 SBR/BR
2

Preblend 1.5
CD2125XZ Rolling Resistance
1 Silica SBR/BR
PBR4088/N234
BR Dry Handling
0.5
Dry Traction
0
Wet traction: high friction
MBB Wet traction: low friction
CD2125XZ CD2125XZ
PBR4088/N234 PBR4088/BR Winter/Ice Traction
BR

MBB
CD2125XZ
PBR4088/BR

Figure 5: Performance indices for rotational shear properties A(top), B(bottom)

 LS-24904
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Double Shear Mode

Rolling
Resistance
1.8
1.6
1.4
1.2
Winter/Ice 1 Dry handling N234 SBR/BR
Traction 0.8
0.6 Silica SBR/BR
0.4
0.2 CD2125XZ PBR4088/BR
0
MBB CD2125XZ PBR4088/BR

MBB CD2125XZ PBR4088/N234 BR

Wet Traction
Dry Traction Preblend CD2125XZ PBR4088/N234 BR
Low Friction

Wet Traction
High Friction

N234 SBR/BR
2
1.8
1.6
Preblend 1.4
CD2125XZ 1.2
1 Silica SBR/BR
PBR4088/N234 0.8 Rolling Resistance
BR 0.6 Dry Handling
0.4
0.2 Dry Traction
0
Wet traction: high friction
Wet traction: low friction
MBB CD2125XZ Winter/Ice Traction
CD2125XZ
PBR4088/N234
PBR4088/BR
BR

MBB CD2125XZ
PBR4088/BR

Figure 6: Performance indices for double shear properties A(top), B(bottom)

 LS-24904
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Compression Mode

Rolling
Resistance
1.8
1.6
1.4
1.2
Winter/Ice 1 N234 SBR/BR
Dry handling
Traction 0.8
0.6 Silica SBR/BR
0.4
0.2 CD2125XZ PBR4088/BR
0
MBB CD2125XZ PBR4088/BR

MBB CD2125XZ PBR4088/N234 BR

Wet Traction
Dry Traction Preblend CD2125XZ PBR4088/N234
Low Friction BR

Wet Traction
High Friction

N234 SBR/BR
2

Preblend 1.5
CD2125XZ
1 Silica SBR/BR
PBR4088/N234 Rolling Resistance
BR
0.5 Dry Handling
Dry Traction
0
Wet traction: high friction
We traction: low friction
MBB CD2125XZ Winter/ice traction
CD2125XZ
PBR4088/N234
PBR4088/BR
BR

MBB CD2125XZ
PBR4088/BR

Figure 7: Performance indices for compressive properties A(top), B(bottom)

 LS-24904
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The spider plots emphasize significant differences between the predicted performances of the various test compounds. Some
variations are observed between the data of the various test modes; most notably between shear and compression-based modes.
In general, the silica-based compound consistently out performs the N234 carbon black compound in terms of rolling resistance,
winter/ice traction, and low friction wet grip performance indicators. Silica is substantially worse in terms of predicted high
friction wet grip, dry handling, and dry traction performance. This is consistent with the observed trend of silica having a
reduced modulus across the rubbery region (LS-24904), which is broadly the result of reduced filler-filler networking in silane-
treated silica compounds.

Depending on the method of processing, the CD2125-filled compounds prepared with functionalized SBR lie somewhere in
between the performance of N234 and silica but tend to track the shape of the silica performance envelope over the N234
envelope. Within the CD2125 series, there is clear performance differentiation between compounds processed via masterbatch
blending and those processed in a single reactive mixing step. In the two shear modes, there are differences between the absolute
values of the performance indices but the trends are reasonably consistent. These trends are summarized in Table V, which
gives the change in compound performance upon moving from a single reactive mix to masterbatch blending. Masterbatch
blending recovers the dry handling and high friction wet traction predicted performance of the compound at the expense of
winter/ice traction, low friction wet traction and, to a lesser extent, rolling resistance and dry traction. This seems to be broadly
consistent with masterbatch blending producing compounds with higher storage moduli (more filler networking?) across the
rubbery region meaning that masterbatch blending tends to skew the performance envelope shape of CD2125 back towards the
performance of N234. Note that sample ‘MBB CD2125XZ PBR4088/N234 BR’ actually contains N234 as part of one of the
masterbatch mixes.
These trends are also reflected in the compression mode data although there are differences in the absolute rankings of each
compound for each performance index. These differences may be due to the relatively large mean strain applied across the
sample cylinders as discussed in the ‘Equivalence of compression and shear data’ section of this report.

Table V: Summary of the effects of masterbatch mixing of CD2125 versus a single reactive mix pass

CD2125 change in performance upon

masterbatch blending
Rolling resistance -
Dry handling ++
Dry traction -
Wet traction: high friction ++
Wet traction: low friction --
Winter/Ice traction --
 LS-24904
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LOSS COMPLIANCE PROPERTIES:

It is of interest to examine in more detail the loss compliance properties of the compounds as calculated from strain sweep data.
The importance of loss compliance as a performance predictor for dry traction was highlighted earlier in this report using the
‘deformation index’ approach. Loss compliance was calculated from strain sweep data using Equations 2 and 6. Example data
are presented in Figure 7 from the rotational shear measurements.

0.14
Improved predicted
dry traction
0.12
Loss Compliance, J'' / MPa-1

0.1

0.08

0.06 N234 SBR/BR

Improved predicted
dry handling Silica SBR/BR
0.04 CD2125XZ PBR4088/BR
MBB CD2125XZ PBR4088/BR
0.02 MBB CD2125XZ PBR4088/N234 BR
Preblend CD2125XZ PBR4088/N234 BR
0
0.1 1 10 100 1000
Shear Strain %

Figure 8: Loss compliance for the various compounds calculated from strain sweep data in rotational shear deformation mode

From Figure 8, a clear difference in performance can be noted between N234 and silica compounds. A crossover in loss
compliance at roughly 1.2% strain is observed. The demands of dry handling performance and dry traction require a low loss
compliance (high modulus) at low strains and high loss compliance at high strains as indicated on the figure. The N234
compound offers the best predicted performance over the whole strain range. Silica’s predicted performance is considerably
worse than N234 excepting the crossover strain. CD2125XZ/functionalized SBR compounds are intermediate between the two
extremes of N234 and silica compounds depending on processing route.
The loss compliance profiles for these compounds are intimately related to the nature of the Payne effect. It has been repeatedly
observed in NPD studies that the use of functionalized CB in a functionalized elastomer shifts the onset of the non-linear
dependence of the viscoelastic moduli to higher strains versus an equivalent, unmodified CB. Interestingly, the same
observation can be made for silica compounds versus unmodified CB. This is illustrated with rotational shear strain sweep data
from this study. Figures 9 A and B show the dynamic moduli data for N234, silica, and CD2125 filled compounds. Figure 10
shows the same data but normalized to the small strain modulus in each data set. This highlights the shifting to higher strains of
the decay in storage and peak in loss moduli for silica- and CD2125XZ-based compounds. Currently the mechanisms for this are
not completely understood but are key to traction and handling performance of these compounds.
 LS-24904
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12
A
Carbon Black
10
Carbon Black XZ
8 Silica
G' / MPa

0
0.1 1 10 100 1000
Strain %

1.6
B
1.4 Carbon Black

1.2 Carbon Black XZ

1 Silica
G'' / MPa

0.8

0.6

0.4

0.2

0
0.1 1 10 100 1000
Strain %

Figure 9: A) Storage and B) Loss moduli for N234, CD2125XZ, and Silica filled compounds
 LS-24904
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1.2
A
Carbon Black
1
G' / G'Low strain Carbon Black XZ
0.8 Silica

0.6

0.4

0.2

0
0.1 1 10 100 1000
Strain %

1.6
B
1.4 Carbon Black

1.2 Carbon Black XZ

G'' / G''Low strain

1 Silica

0.8

0.6

0.4

0.2

0
0.1 1 10 100 1000
Strain %

Figure 10: A) Normalized storage and B) Normalized loss moduli for N234, CD2125XZ, and Silica filled compounds

CONCLUSION:
Viscoelastic data for tread compounds collected in three different modes of deformation showed reasonably
consistent trends in terms of predicted tread compound performance using the “deformation index” approach to
define the appropriate viscoelastic performance parameters.
Spider plots created from the viscoelastic data showed clear differences in the predicted performance of N234- and
silica-based compounds. CD2125XZ compounds generally lie intermediate between these two performance
extremes and can be made to more closely follow the silica or carbon black performance trends based on the
mixing/processing route. The standard CD2125XZ compound prepared with a single reactive mix step shows
remarkably similar predicted performance to that of the silica-based compound.
 LS-24904
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REFERENCES:
1. PB Lindley, Engineering Design with Natural Rubber, MRPRA, 5 th Edition, 1992
2. AD Roberts (Ed), Natural Rubber Science and Technology, Oxford Science Publications, 1990
3. W Mars, Analysis of Stiffness Variations in Context of Strain-, Stress-, and Energy-Controlled Processes, Rubber
Chem. Technol., 84, 2, 2011, pp. 178-186
4. S Futamura, Deformation Index – Concept for Hysteretic Energy Loss Process, Rubber Chem. Technol., 63, 3, 1990,
pp. 315-367
5. S Futamura, AA Goldstein, Prediction and Simulation of Tire Performance Characteristics based on Deformation
Index Concept, Rubber Chem. Technol., 89, 1, 2016, pp. 1-21
6. SK De, JR White, Rubber technologist’s handbook vol. 1, RAPRA, 2001
7. European Central Laboratory report: RE6578, Dynamic charaterisation of tread compounds for Sumitomo, 2008
8. H Moneypenny, ‘Product performance/durability prediction’, course notes, HR&RC

The test results, statements, opinions and/or recommendations contained herein are based on information, data, reports or tests believed to be reliable. HOWEVER, BIRLA
CARBON MAKES NO WARRANTY OR GUARANTEE OF ACCURACY OR COMPLETENESS IN CONNECTION THEREWITH, NOR, WITH RESPECT TO ANY BIRLA
CARBON PRODUCTS INVOLVED, ANY WARRANTY OR MERCHANTABILITY OR FITNESS FOR A PARTICULAR PURPOSE OR USE. Statements concerning the
possible use of Columbian products are not intended as recommendations to use such products in the infringement of any patent.