Rubber Testing

- Emphasis on Mooney Viscometer,

MDR & RPA

Sky Xue
National Rubber Conference in Mumbai
Sky.Xue@alpha-technologies.com
Outline
• Introduction
• Raw Elastomer Tests - Mooney Viscometer
• Concept of Viscoelasticity
• Curemeters – ODR & MDR
• Multi-Test Systems – RPA 2000

2
Rubber Processability Tests
• Stress Strain Testing (1900s)
• Mooney Viscosity (1930s)
• Plastometers (1930s)
• Mini Process Tester (1950s)
• ODR Cure Meters (1960s)
• Capillary Rheometers (1970s)
• Mooney Stress Relaxation (1980s)
• Rotorless Curemeter, MDR (1980s)
• Rubber Process Analyzer (1990s)
• PPA and RPA auto (2000s)

3
Raw Elastomer Tests

4
 Mooney
Viscometer

5
MV 2000 Test Area

Rotor

Lower Die

6
MV 2000 Test Area
Sealed & pressurized sample
chamber usually at 100 C or 125 C

Serrated rotor moves at 2 rpm

7
Mooney Viscometer
• Established Test (Since
1930s)
• Test Sequence
– Load Sample
– Wait for Sample to Warm Up (1
minute)
– Turn Motor On for Set Time

MoneyUnits
(often 4 minutes or 8 minutes)
• Labor Intensive Test
• Not Sensitive to Polymer T
i
me
Elasticity or High Shear Rate
Flow Behavior

8
Vairables in Mooney Testing
• Test Temperature (100 C, 125 C)
• Size of rotor [ML (large) or MS (small)]
• Preheat Time (usually 1 minute)
• Rotor Running Time
• Example: ML1+4
– Large rotor. 1 minute preheat. 4 minute
run time. Lowest value in last 0.5 minutes.

9
 5 unit rise

10
11
Mooney Viscosity of Raw
Polymers
• Mooney Viscosity Indicates Polymer Molecular
Weight Differences but Often Not Other
Differences
• Used to grade polymers
• Does not always predict mixing / processing
behavior

12
 Mooney
Stress Relaxation

13
Stress Relaxation describes how
polymers relieve stress with time

Stress Relaxation Test measures a

phenomenon that occurs after the rotor
is suddenly stopped.

14
Mooney Stress Relaxation Test

M
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15
Stress Relaxation Data

100 100% elastic

–T80, time to 80%
decay
Viscosity (MU)

–X30, % decay after 30

sec.
10
–Power law decay,
slope & intercept

viscoealstic
100% viscous
1
0.1 1 10 100
Time (s)
16
 Principles of
Viscoelasticity

17
Elasticity
Hooke’s Law for Perfectly Elastic Materials

• Hooke’s Law
In 1678, Robert Hooke stated:
The power of any spring is in the same proportion with the
tension thereof.

18
So, Hooke’s Law is as follows:

F = MX

Where:
F = Stress (in Psi or Pascals)
X = Strain (∆L/L, deformation per unit length)
M = Proportionality constant

19
Elasticity
Hooke’s Law for Perfectly Elastic Materials
•A force is generated when a deformation is applied

•The force is proportional to the magnitude of deformation

•The force is retained if the deformation is maintained

•The applied energy is stored and is returned as a recovery

force if deformation is released

•It gives the perfect storage of deformational energy without

any loss.

20
• Which material is more elastic?

• Rubber
• Steel

21
22
Viscosity
Newton’s Law for Perfectly Viscous Fluids

• Viscosity relates to a material’s

resistance to flow.

23
Viscosity

• Viscosity (η) is the resistance of a fluid to flow

under stress.
shear stress

shear rate
• With a Newtonian Fluid such as water, the shear
stress is proportional to the shear rate.

24
25
Viscosity
Newton’s Law for Perfectly Viscous Fluids
• A force/stress is generated when deformation is applied

• The force/stress is proportional to the speed of deformation

(not magnitude of deformation)

• The force/stress disappears when the motion stops

• The applied energy is dissipated as fluid motion

26
Visco-Elasticity of Rubber Compounds

• Force versus deformation is not linear

• Elastic energy is stored
• Viscous energy is dissipated as molecular motion and
heat generation

27
Relevance of Visco-Elasticity to Rubber Compounds
Highly elastic compounds
• Store energy during deformation and return that energy as a
retraction force
• Display memory, with preference to return to initial shape after
deformation
• More difficult to process
• Cool running, Generate less heat

Highly viscous compounds

• Dissipate energy during deformation by molecular flow
• Tendency to retain deformed shape after deformation
• Relatively easier to process
• Generate more heat
The balance between elastic and viscous properties determines how
compounds perform during processing, moulding and product
application

28
How to Measure Viscoelastic Properties
under Variable Conditions

29
MDR: Variable temperature, frequency & strain fixed
RPA: Variable frequency, strain and temperature

30
RPA, MDR – Using Oscillatory Strain to
Measure Viscoelastic Properties
S*
S'
Strain

S''


The Complex Torque (S*) is split into two components:

• Elastic Torque (S’) in phase with the applied strain
• Viscous Torque (S”) 90 deg out of phase with the strain

31
Tan Delta = S”/S’
32
Elastic Torque
• Elastic Torque (S‘) relates to the pure elastic
quality of the rubber
• This is the torque response which is precisely in-
phase with the applied strain.

• Rubber characteristics
– Formation of crosslinks from vulcanization process
causes S‘ to rise
– Increasing chain entanglements and gel cause S‘ to rise
for uncured rubber.
– This quality can relate to “nerviness” in rubber
processing
– This quality can relate to hardness in cured rubber
33
Viscous Torque

• Viscous Torque (S’’) relates to the pure viscous

quality of the rubber.
• This is the torque response which is esponding to
the rate of change of the applied strain.
• It is precisely 90° out-of-phase with the applied
strain
• Rubber characteristics
• Relates to the pure flow characteristics of the rubber
• Decreases with a lower frequency or higher
temperature
• Predicts heat build-up with applied strain
• Reduced or remains constant during cure
34
Tangent δ
• Tangent  (delta) is simply the ratio of the viscous
quality (S”) divided by the elastic quality (S’).
• It is also referred to as tan  or V/E Ratio.
• Since it is a ratio, it is a dimensionless parameter
• Rubber Characteristics
– The ratio of a rubber compound is always relatively high in
the uncured state (0.5 to 1.5) and low in the cured state
(0.01 to 0.2).
– This ratio relates to the processability of rubber in the
uncured state relates to rebound (resiliency) for rubber in the
cured state.

35
 Curemeters
(Viscosity, Cure Rate
and Final Modulus)

36
Oscillating
Rheometers
ASTM D2084

37
R100 Oscillating Disc Rheometer

38
ODR invented as a rubber curemeter
Oscillating Disc Rheometer

Operator sets temperature and time.

Frequency and strain are fixed.
9
39
ODR Test Cavity

U
p
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e
r
Di
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u
b
b
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r

L
o
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rD
i
e O
s
c
i
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l
at
i
ng
Di
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k

Disk does not rotate but oscillates at a fixed angle.

40
41
42
Advantages of ODR
• Provides several measurements
– Viscosity
– Scorch Time or Scorch Safety
– Cure Rate
– Hardness of final product (at cure
temperature)
• Applications
– Mix quality
– Formulation development

43
Disadvantages of ODR Rotor
• Acts as “heat sink” - lengthens
temperature recovery
• Measuring torque through rotor shaft causes
problems in measuring dynamic properties
• Time required to remove sample from
rotor after test completed
• No film can be used, constant cleaning
required
• Automation very difficult

44
Rotorless
Curemeter
ASTM D5289

45
 MDR Lower Die

Operator sets temperature and time.

Oscillation frequency and strain are fixed.

46
 MH

Minimum
Viscosity
(0% Cure)
ML

Melt

47
Important Data Points
• ML – minimum torque
• S” at ML
• MH – maximum torque
• S” at MH

• ts1 – time to reach 1 torque unit about ML

• ts2 – time to reach 2 torque units above ML
• t10 – time to reach 10% cure
• t50 – time to reach 50% cure
• t90 – time to reach 90% cure

• Maximum S’ rate
• Time at maximum S’ rate
48
49
50
51
52
Comparison to MDR 2000

Premier™ MDR MDR 2000

25% smaller - 70 pounds lighter
53
Premier™ MDR Design Overview
• Wrap-around front
cover for easy
disassembly and service
• Smart Alignment™ -
Floating Crosshead gives
more accurate die
alignment
• Smart Seal™ (seal-
less) An optional upper
die assembly to
eliminate the
conventional seal while
maintaining a closed,
pressurized cavity for
improved long-term
stability and reduced
torque calibrations
• Dynamic Symmetry™
- 4 posts, ensure parallel
die closing,
54
•Multi-color LED back-lit
logo for status indication
•Independent upper and
lower air cooling on dies
for productivity and VTA
control
• Touch-screen user
interface for diagnostic
information
• Rapid Change™ -
allows simple and fast
oscillation angle
changes without the
need for re-calibration
• Storage drawer for
tools, software, spares
 Premier™ MDR
Performance with
Smart-Seal™ System

55
 Reproducibility
12

10

8
S' (dNm)

4
3 MDR2000’s
5x samples on each
2

0
0 2 4 6 8 10 12 12
Elastic Torque vs.. Time, SBR 177°C from
Time (min) MDR 2000 (3 units)
10
STA
6 Premier™ MDR’s NDA
RD
8 A1
5x samples on each S', dNm STA
NDA
6 RD
A2

4 STA
NDA
RD
A3
2

0
0 5 10 15
Time, Min.

56
 Effect of Seal System
– 300 Samples over 7 days
12.00

11.80
MDR 2000

11.60

Data shift is Standard Silicone

11.40
MH (dNm)

due to use of
different 11.20
batches of Long Life
Premier™ MDR
compound 11.00

10.80
Premier™ MDR
Seal-less

10.60
0 50 100 150 200 250 300 350
Sample Number

57
Long Term Repeatability
First 5 and Last 5 Samples
Over 120 Days

Premier MDR with Smart Seal™ has excellent long term Repeatability

58
Long Term Repeatability

MH - Long Term Stability (Range 0.2dNm)

11.20

11.10

11.00

10.90
MH

10.80

10.70

10.60

10.50
1 3 5 30 50 70 90 110 130 150 170 190 210 230 250 270 290 301 303 305
Sample Number

Premier™ MDR with Smart Seal has excellent long term

Repeatability
59
 TM
Rapid Change
Variable Oscillation Angle

Rapid Change™ variable oscillation eccentric allows torque to

be easily optimised for specially hard and soft compounds
60
Premier MDR - Automation Systems

5x Sample Queue and Haul-off Multiple Sample Automation

61
Multi-Test Systems

62
RPA 2000

ASTM D6204
ASTM D6601
ASTM D7050

63
Test Conditions

Oscillation Frequency: 0.0016 ~ 50 Hz (0.1 ~ 3000 cpm),

Strain: ± 0.7 ~ ±1256 % (±0.05° - ±90°)
Temperature: RT to 230 C (standard)
RT to 350 C (high temperature option)
Torque Range: 0.01 ~225 dN-m

With EDR:
Strain: ± 0.07 ~ ±1256 % (±0.005° - ±90°)
Torque Range: 0.0023 ~225 dN-m

1 lb-in = 1.13 dNm

64
Frequency

• C.P.M. (cycles per minute)

• Hz (Hertz or cycles per second)
• Rad./Sec (Radians per second)

60 cpm = 1 Hz
1 cycle = 360o = 2 π radians
1 Hz = 2 π rad./sec = 6.28 rad./sec

65
Strain
• Degrees arc
• % strain (SSA, Single Strain Amplitude)
• % strain (DSA, Double Strain Amplitude
or PTP, Peak to Peak )
• Strain (decimal fraction of ∆L/L)

66
67
Dynamic Shear Moduli

• Elastic (Storage) Modulus (G‘)

• Viscous (Loss) Modulus (G‘’)
• Complex Modulus (G*)
• G' = (KS') / Strain
• G'' = (KS'') / Strain
• G* = [ (G’)2 + (G’’)2] ½
• TanD = S”/S’ = G”/G’

68
Dynamic Viscosity

• Complex Dynamic Viscosity *

• Real Dynamic Viscosity ‘
• Imaginary Viscosity ‘’
• ' = G ''/ 
• '' = G '/ 
– Where  is frequency is Radians / Sec.

69
 RPA 2000 Applications

RAW COMPOUND DYNAMIC

ADVANCED
POLYMER PROCESSABILITY MECHANICAL
CUREMETER
TESTER TESTER TESTER

Relevant to: Relevant to: Relevant to: Relevant to:

• Viscosity • Mixing / Extrusion • Process Scorch • Modulus
• MW Distribution • Die Swell • Cure Rate & Time • Elasticity
• Branching • Mould Flow • Reversion • Viscoelasticity
• Ageing • Process Viscosity • Non-isothermal • Heat Build-up
Curing • Damping

70
RPA2000 - Available Test Procedures

Cure Variation of torque or modulus vs. time at programmable

strain, temperature and frequency (Isothermal condition)

VTA Variation of torque or modulus vs. time at programmable

strain, temperature and frequency (Non-isothermal,
temperature profile)

Frequency Modulus, torque, viscosity under a range of frequency at

Sweep programmable strain and temperature.

Strain Sweep Modulus, torque, viscosity under a range of frequency at

programmable frequency and temperature.

71
RPA2000 - Available Test Procedures

Temperature Modulus, torque, viscosity under a range of frequency at

Sweep programmable frequency and strain.

Matrix Sweep Modulus, torque, viscosity under a range of frequency at

programmable strain, frequency and temperature.

Stress Modulus and torque vs. time after step strain

Relaxation (programmable in temperature and strain)

Delay Sample ageing and conditioning at programmable time,

strain, frequency and temperature.

72
RPA2000 – Multiple Subtest Capability

Characterise materials before, during and after cure

73
 RPA2000
Raw Polymer
Characterization

74
Measurements From Frequency Sweeps on Two Elastomers
RPA 2000 Frequency Sweep of
with similar Mooney Viscosity Values
Two Different Grades of a Polymer

5
S' Torque (in.lb.)

0
1 10 100 1000 10000
Frequency (cpm)
75
Frequency Sweep
Effect of Branching & MWD on Tan Delta

76
Branching and Molecular Weight of BR

Similar Mw/Mn
Low Branching

High Branching

77
Crossover Point in Frequency Sweep

78
Crossover Point

+ AMW

+M
WD

79
 RMA Nitrile Comparison of MW with a Freq. Sweep

5
0
0
+
0
.7
%S
t
ra
i
n,
01
3
0 0
0C
2
0
0
M
w
=1
0
6,
00
0
1
0
0 A

B
5
0 RMA Nitrile Comparison
Mw=79,
000 of
0MW
3
ComplexSharStes,G*kPa

0with a Frequency Sweep

2

1
0
0
.0
10.
03 0
.
1 0
.
3 1 3 1
0 3
0
F
r
e
que
n
cy
,
Hz
80
 RMA Nitrile Comparison of ACN Content using a Freq. Sweep

5
0
0
+
0
.7
%S
t
ra
i
n,
1
0
0C
3
0
0

3
8
.
3%A
C
N
2
0
0
A
RMA Nitrile Comparison of B
1
0
0 29
.3
% AC
N
ACN
Content using a Frequency
ElasticShearStes,G'kPa

5
0
Sweep
3
0
0
.0
10.
03 0
.
1 0
.
3 1 3 1
0 3
0
F
r
e
que
n
cy
,
Hz
81
 RMA Nitrile Comparison of MWD using a Frequency Sweep

2
0
0
+
0
.7
%S
t
ra
i
n,
1
0
0C
1
0
0
M
w
/
Mn=
3
.9
A
5
0
M
w
/
Mn=
2
.8 B
3
0
RMA Nitrile Comparison of
2
0
MWD
ViscouShearStes,G"kPa

Using a Frequency Sweep

1
0
0
.0
10.
03 0
.
1 0
.
3 1 3 1
0 3
0
F
r
e
que
n
cy
,
Hz

82
 RMA Nitrile Comparison of Gel Using a Frequency Sweep

0
.
9
+
0
.7
%S
t
ra
i
n,
0
.
8
1
0
0C
0
.
7 N
B
Rw
/
oGe
l
0
.
6
Tan 

0
.
5

0
.
4 RMA Nitrile Comparison of
3Gel
0
.
N BR wit
hGe
l
2Using a Frequency Sweep
0
.

0
.
1
0.
010
.
03 0
.
1 0
.
3 1 3 1
0 3
0
F
r
e
que
n
cy
,
Hz
83
High Strain Polymer Testing
Effect of Long Chain Branching on tanD

Variation of Tg  1 vs. shear strain

Bn=0 Bn=0.03 Bn=0.15 Bn=0.23 Bn=0.36 Bn>1

9.000
8.000
7.000
6.000
Tangent 

5.000
4.000
3.000
2.000 Increasing LCB
1.000
0.000
10 100 1000
Shear strain (%)

84
High Strain Testing of Natural Rubber

Expected
higher LCB

85
Low and High Strain Differentiation Natural Rubber

Viscosity

Branching

86
Large Amplitude Oscillatory
Shear(LAOS)
to Measure Long Chain
Branching (LCB）
Testing Domain
G' & G"( K Pa)
1,000

Non
li
nea
r
L
i
nea
r
v
i
sco
e
l
asti
ci
ty
v
i
sco
e
las
t
i
ci
ty
L
A
OS
100

10
G
*
=f
(
 G
*
=f
(



1
1 100 10,00
10 1,000

St rain ( % SSA

88
As Strain Increases,
Sine Wave Response Becomes Distorted
Shear stress (Pa) Strain (Norm alized)
300000 1.5
Sample B
Sample C
200000 Strain 1

100000 0.5

0 0

-100000 -0.5

-200000 -1

-300000 -1.5
0.00 1.00 2.00 3.00 4.00 5.00 6.00 7.00
Tim e (s)
89
Plot Shear Stress(t) versus Shear Rate(t) for one cycle.
LCB index Positive LCB Materials with loops are linear
Negative Linear

Materials without loops

Are branched

90
Heat and Shear Stability of Raw Polymers

91
 RPA2000
Compound Applications

92
Intelligent Compound Testing

93
Uncured Rheological Properties

ASTM D6204
• 1 to 4 minute Pre-heat
• 100°C, 2.8% Strain, 0.5 Hz
• Timed subtest to allow temperature and internal
stresses to stabilize
• Frequency Sweep (Part A)
• 100°C, 7% Strain
• Frequencies of 0.1, 2, 20 Hz
• Viscosity Measurement
• Frequency Sweep (Part B)
• 100°C, 0.1, 1 Hz, 100% Strain
• Mixing capability

94
ASTM D6204 Frequency Sweep at 7% Strain
for 6 Different SBRs

Values in this area

correlate to Mooney
Viscosity and MW

95
ASTM D6204 Frequency Sweep at 7% Strain
for 6 Different SBRs
Lower values indicate more
difficulty in processing
(rougher sheets)

96
RPA vs Mooney Viscosity

C
o
mpa
r
is
onf
or2
3P
ol
yme
r
s
1
20
M
V=
71
.4(
S*)
+ 1
.
25
R=0.9
5
1
00

8
0
ML-1+4@10C

6
0

4
0

2
0
0.
4 0
.
6 0.8 1 1 .2 1 .
4 1
.
6
R
PAS
*
,@10
0C
,7
%St
rai
n,0
.
1 H
z
97
Polymer-Black Masterbatch
MV and RPA Results on 2 Supplies

Supplier A

Supplier B

98
RPA Test Sensitivity – Processability

Processability Testing - Test Sensitivity

Test Type

RPA S" at 280%

RPA S" at 70%

RPA TD at 70%

RPA S' at 280%

RPA S' at 70%

MV SR Slope

MV ML(1+4)

0 5 10 15 20 25 30 35 40
Test Sensitivity (Signal/Noise Ratio)

99
RPA (300% strain) vs Extrusion Die Swell

T an g en t d el ta @ 300%
Di e sw
1. 46 36. 5
Ta nge nt D

D ie 36.
sw 0
e ll
1. 48

35. 5

1. 50
35. 0

1. 52 34. 5

34. 0
1. 54

33. 5

1. 56
33. 0

1. 58 32. 5

100
RPA in Mix Studies

101
Tanδ vs G* ，numbers refer to mixing time.
102
 Two Wing Rotor

N Rotor

Four Wing Rotor

103
 0.61

0.6

0.59

2 Wings (40 rpm)

0.58
tanD@20.000 Hz

2 Wings (50 rpm)

2 Wings (60 rpm)

0.57 4 Wings (40 rpm)

4 Wings (50 rpm)
4 Wings (60 rpm)
0.56 N (40 rpm)
N (50 rpm)
N (60 rpm)
0.55 Trend Line

0.54

0.53
580 590 600 610 620 630 640 650 660
G*@20.000 Hz

Tanδ versus G* at 7% strain, 20 Hz and 100 C.

104
Extrusion Process Quality

Tan Delta vs S' (100%/0.1Hz)

1.535
1.53
1.525
1.52
Tan Delta

1.515
1.51
1.505
BAD
1.5
BAD
1.495
1.49
4.1 4.2 4.3 4.4 4.5 4.6 4.7
S' dNm

105
 RPA2000
Advanced Curometer

106
Non-Isothermal Cure Test (VTA)

107
Non-Isothermal Cure Simulation

108
Non-Isothermal Cure Simulation

Cure Simulation - Post-Cure Properties

80C/10Hz
0.18

0.175
Tan Delta at 10%

Tread Outer
0.17
Strain

0.165
Tread Inner
0.16

0.155

0.15
1200 1300 1400 1500 1600 1700 1800
G' at 10% Strain

109
 RPA2000
After cure dynamic
properties evaluation

110
After Cure Dynamic Properties
ASTM D6601
• Cure Subtest
• Select Cure Temperature
• 0.0% Strain (Delay Subtest) or 2.79% Strain
• 100 cpm or 60 cpm
• Strain Sweep
• 100°C and / or 60°C
• 1%, 2%,5%, 10% & 20%
• Frequencies of 1 and / or 10 Hz
• Strain Sweep
• 100°C and / or 60°C
• 1%, 2%,5%, 10% & 20%
• Frequencies of 1 and / or 10 Hz

111
Payne Diagram for Filled Rubber Compoun

112
 Figure 14
Effects of Silica Surface Area with and Without Silane
on the Payne Effect in the Cured State
12000 60ºC, 1 Hz
Cpd 1: 70 phr N234
80 phr Silica @ 135 SA,
Cpd 2: 80 phr Silica 55 SA
No Silane
Cpd 3: 80 phr Silica 135 SA
10000 80 phr Silica @ 160 SA Cpd 4: 80 phr Silica 160 SA HD
No Silane
Cpd 5: 80 phr Silica 195 SA
G' Storage Modulus (kPa)

80 phr Silica @ 195 SA,

Cpd 6: 80 Silica 55 with X50
No Silane
Cpd 7: 80 phr Silica 135 SA with X50
8000
Cpd 8: 80 phr Silica SA 160 HD with X50
Cpd 9: 80 phr Silica 195 SA with X50
80 phr Silica @ 135 SA,
6000 with X50 Silane

80 phr Silica @ 195 SA,

with X50 Silane
4000
80 phr Silica @ 160 SA HD,
with X50 Silane
70 phr N234
Control
80 phr Silac @ 55 SA
2000 with and without Silane

0
0.01 0.1 1 10 100
% Strain
 Figure 19
Master Curve of both the Uncured and Cured G' Response
12000
For Series 1 Silica Tread Variations
Two Back-to-Back Strain Sweeps in Cured State
10000 Cpd 1: 70 phr N234
Cpd 2: 80 phr Silica 55 SA
Uncured Strain Sweep Cpd 3: 80 phr Silica 135 SA

8000 Cpd 4: 80 phr Silica 160 SA HD

G' Elastic Moduus (kPa)

Cpd 5: 80 phr Silica 195 SA

1st Strain Sweep Cpd 6: 80 Silica 55 with X50

6000
After Cure Cpd 7: 80 phr Silica 135 SA with X50
Cpd 8: 80 phr Silica SA 160 HD with X50
Cpd 9: 80 phr Silica 195 SA with X50

4000

2000

2nd Strain Sweep

0 After Cure
Hot De-mould Tearing
FP Hot Tear: Static Cure 6 min @ 190 °C;
Strain Sweep
Hot Tear: @Cure
Static 1906°C
minand 2 Hz
@ 190 C
Strain Sweep @ 190 C and 2 Hz
140
120
Torque S' [dNm]

100
80
60 A 1 less
A 2 less
40
B 1 more

20 B 2 more

0
0 50 100 150 200
Strain [%]

115
RPA Correlation with Standard Laboratory
Tests
Hardness

116
RPA Correlation with Standard Laboratory
Tests
Rebound Resilience

117
118
119
120
Thank you!

121
122