Linear and Non Linear Rheological Measurements on … TA Instruments.… · TAINSTRUMENTS.COM...

38
TAINSTRUMENTS.COM TAINSTRUMENTS.COM Linear and Non Linear Rheological Measurements on Rubber Polymers and Compounds Thomas Rauschmann Copyright TA Instruments, USA

Transcript of Linear and Non Linear Rheological Measurements on … TA Instruments.… · TAINSTRUMENTS.COM...

Page 1: Linear and Non Linear Rheological Measurements on … TA Instruments.… · TAINSTRUMENTS.COM Physical description of Polymers Strain Sweep -LAOS 0.0 π 0.5 π 1.0 π 1.5 π 2.0 π-8000-6000-4000-2000

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Linear and Non Linear Rheological

Measurements on Rubber

Polymers and Compounds

Thomas Rauschmann

Copyright TA Instruments, USA

Page 2: Linear and Non Linear Rheological Measurements on … TA Instruments.… · TAINSTRUMENTS.COM Physical description of Polymers Strain Sweep -LAOS 0.0 π 0.5 π 1.0 π 1.5 π 2.0 π-8000-6000-4000-2000

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Standard Test: Mooney

Page 3: Linear and Non Linear Rheological Measurements on … TA Instruments.… · TAINSTRUMENTS.COM Physical description of Polymers Strain Sweep -LAOS 0.0 π 0.5 π 1.0 π 1.5 π 2.0 π-8000-6000-4000-2000

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0.0

16.0

32.0

48.0

64.0

80.0

0.0 1.6 3.2 4.8 6.4 8.0

Mo

on

ey-V

isko

sitä

t [M

U]

Zeit [min]

SCARABAEUS GMBH - [email protected] - Tel.:+49 (0) 6403/9034-0

Polymer C1

Polymer C1

Polymer B1

Polymer B1

Polymer A1

Polymer A1

SCARABAEUSMooneyprüfung

Entwicklung

• Mooney Viscosity• Mooney Relaxation• Mooney Scorch

Shear rate 1.6 s-1 (2 rpm)

0,01 0,1 1 10 100

0,01

0,1

1

.

η

shear rate, γ

vis

cosity

ML1+4

Standard Test: Mooney

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TA Instruments - RPA

Zeit

γ

-1.5

-1

-0.5

0

0.5

1

1.5

0 5 10 15 20 25 30 35 40

ω 1

ω 2

Zeit

γ1

-3

-2

-1

0

1

2

3

0 5 10 15 20 25 30 35 40

γ2

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Zeit

γ

-1.5

-1

-0.5

0

0.5

1

1.5

0 5 10 15 20 25 30 35 40

ω1

ω2

Frequency:

RPA 0.001…50.0 Hz

Step 0.001Hz

RPA Rheometer

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Effect of Branching on G’, G”, ηηηη* and tangent δδδδ

1000

10000

100000

1000000

10000000

0.01 0.1 1 10 100 1000

Frequency (Rad/s

Eta

* (P

a.s

)

Branched

Linear

Mooney shear rate

range

0.1

1

10

100

1000

0.01 0.1 1 10 100 1000

Frequency (Rad/s)

G' &

G"

(kP

a)

0

1

2

3

4

5

6

7

8

9

Tan

gen

t D

elt

a (

-)

∆δ or ∆Tan δ

“High performance EPDM polymers based on a new technology of controlled Long Chain Branching” H.J.H.

Beelen, IRC97, Nürnberg.

Page 7: Linear and Non Linear Rheological Measurements on … TA Instruments.… · TAINSTRUMENTS.COM Physical description of Polymers Strain Sweep -LAOS 0.0 π 0.5 π 1.0 π 1.5 π 2.0 π-8000-6000-4000-2000

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LCB and MWD (linear) effect on Tangent δδδδ

0

0.5

1

1.5

2

2.5

3

0.01 0.1 1 10 100 1000

Frequency (Rad/s)

Ta

ng

en

t D

elt

a (

-)B50

B100

Star-IIR

Mix4

Weight % B15 B30 B50 B100 B200

Mix 1 90.7 0 0 0 9.3

Mix 4 10.9 21.9 36.4 22 8.8

Page 8: Linear and Non Linear Rheological Measurements on … TA Instruments.… · TAINSTRUMENTS.COM Physical description of Polymers Strain Sweep -LAOS 0.0 π 0.5 π 1.0 π 1.5 π 2.0 π-8000-6000-4000-2000

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Correlation between ηηηη* and Mooney viscosity ML(1+4) – EPDM polymers

1000

10000

100000

1000000

10000000

0.01 0.1 1 10 100 1000

ηη ηη*

(Pa

.s)

Angular frequency (Rad/s)

Polymer 1-2

Polymer 2-2

Polymer 3-2

Polymer 4-2

Polymer 5-2

Polymer 6-2

Polymer 7-2

Mooney shear rate

range

Page 9: Linear and Non Linear Rheological Measurements on … TA Instruments.… · TAINSTRUMENTS.COM Physical description of Polymers Strain Sweep -LAOS 0.0 π 0.5 π 1.0 π 1.5 π 2.0 π-8000-6000-4000-2000

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EPDM (ML(1+4)@125° C 65 ± 5 MU

0

0.2

0.4

0.6

0.8

1

1.2

1.4

1.6

0.01 0.1 1 10 100 1000

Ta

ng

ne

δ

δ

δ

(-)

Angular frequency (Rad/s)

Polymer 1-2

Polymer 2-2

Polymer 3-2

Polymer 4-2

Polymer 5-2

Polymer 6-2

Polymer 7-2

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Zeit

γ1

-3

-2

-1

0

1

2

3

0 5 10 15 20 25 30 35 40

γ2

Strain:RPA 0.005…360.0 °

Step 0.01°

RPA Rheometer

Page 11: Linear and Non Linear Rheological Measurements on … TA Instruments.… · TAINSTRUMENTS.COM Physical description of Polymers Strain Sweep -LAOS 0.0 π 0.5 π 1.0 π 1.5 π 2.0 π-8000-6000-4000-2000

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Why Non linear viscoelasticity ?

PIPKIN Diagram

Page 12: Linear and Non Linear Rheological Measurements on … TA Instruments.… · TAINSTRUMENTS.COM Physical description of Polymers Strain Sweep -LAOS 0.0 π 0.5 π 1.0 π 1.5 π 2.0 π-8000-6000-4000-2000

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RPA Rheometer

0

100

100

200

200

300

300

400

400

1 10 100

Schubmodul G' [kPa]

Amplitude [%]

SCARABAEUS GMBH - [email protected] - Tel.:+49 (0) 6403/9034-0

Scarabaeus GmbHMeß- und Produktionstechnik

SIS V 50

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Physical description of PolymersStrain Sweep - LAOS

0.0π 0.5π 1.0π 1.5π 2.0π

-8000

-6000

-4000

-2000

0

2000

4000

6000

8000

-1200

-1000

-800

-600

-400

-200

0

200

400

600

800

1000

1200

PIB, ω=0.1 Hz, γ0=1000%, T=140°C

τ [P

a]

t×ω [Pa]

γ [%

]

•" S

tad

ler

FJ,

Le

yg

ue

A,

Bu

rhin

H,

Ba

illy

C (

20

08

) T

he

po

ten

tia

l o

f la

rge

am

plitu

de

osc

illa

tory

sh

ea

r to

ga

in a

n in

sig

ht

into

th

e

lon

g-c

ha

in b

ran

chin

g s

tru

ctu

re o

f p

oly

me

rs.

•In

: T

he

23

5th

AC

S n

ati

on

al

me

eti

ng

, p

oly

me

r p

rep

rin

ts A

CS

, vo

l4

9. N

ew

Orl

ea

ns,

LA

, U

SA

, p

p 1

21

–1

22

"

Page 14: Linear and Non Linear Rheological Measurements on … TA Instruments.… · TAINSTRUMENTS.COM Physical description of Polymers Strain Sweep -LAOS 0.0 π 0.5 π 1.0 π 1.5 π 2.0 π-8000-6000-4000-2000

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Physical description of PolymersStrain Sweep - LAOS

Page 15: Linear and Non Linear Rheological Measurements on … TA Instruments.… · TAINSTRUMENTS.COM Physical description of Polymers Strain Sweep -LAOS 0.0 π 0.5 π 1.0 π 1.5 π 2.0 π-8000-6000-4000-2000

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Henri Burhin, Polymer Process Consult, 2012

Physical description of PolymersStrain Sweep - LAOS

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LAOS – Sensitivity to branching content

A (Branched) 2.5% branched in linear H (Linear)

G'1/G'5 6,91 6,09 3,74

A3/A5 -2,97 -3,44 -3,00

E1 3,91 5,32 4,00

E2 -3,97 -4,44 -4,00

E3 4,94 5,93 5,00

G'1/G'5-E3 1,97 0,16 -1,27

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EPDM polymers ML(1+4), 125° C 65 ± 5 MU

0

0.2

0.4

0.6

0.8

1

1.2

1.4

1.6

0.01 0.1 1 10 100 1000

Ta

ng

ne

δ

δ

δ

(-)

Angular frequency (Rad/s)

Polymer 1-2

Polymer 2-2

Polymer 3-2

Polymer 4-2

Polymer 5-2

Polymer 6-2

Polymer 7-2

-300000

-200000

-100000

0

100000

200000

300000

-8 -6 -4 -2 0 2 4 6 8

Sh

ea

r st

ress

(P

a)

Shear rate (s-1)

Polymer 6-2

Polymer 7-2

Polymer 5-2

Polymer 4-2

Polymer 3-2

Polymer 2-2

Polymer 1-2

-2

0

2

4

6

8

10

12

Polymer 7-2 Polymer 6-2 Polymer 5-2 Polymer 4-2 Polymer 3-2 Polymer 2-2 Polymer 1-2

mean

LCB

In

de

x (

G'1

/G'5

-E

3)

Page 18: Linear and Non Linear Rheological Measurements on … TA Instruments.… · TAINSTRUMENTS.COM Physical description of Polymers Strain Sweep -LAOS 0.0 π 0.5 π 1.0 π 1.5 π 2.0 π-8000-6000-4000-2000

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RPA Rheometer – Tan Delta

LCB Index:BR1: 3.7BR2: 2.2

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Strain-Sweep / tan δ δ δ δ @ 1000%aging @ 150°C, 400%

2.7

4

53.7

6

0

10

20

30

40

50

60

BR 1 BR 2

Tan Delta

percentage differencesbefore and after aging

0.000

0.500

1.000

1.500

2.000

2.500

3.000

3.500

4.000

4.500

BR 1 BR 2

Tan Delta

before aging

after aging

2 types of BR with:45MUcis-1,4 Content % > 96

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Strain-Sweep / LCB @ 1000%

aging @ 150°C, 400%

14.45

101.74

0

20

40

60

80

100

120

BR 1 BR 2

LCB Index

percentage differencebefore and after aging

0

1

2

3

4

5

6

7

8

BR 1 BR 2

LCB Index

before aging

after aging

2 types of BR with:45MUcis-1,4 Content % > 96

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Strain-Sweep / tan δ δ δ δ @ 1000% aging @ 150°C, 400%

2.74

53.76

14.45

101.74

0

20

40

60

80

100

120

BR 1 BR 2

dif

fere

nce b

efo

re/a

fter

ag

ing

[%

]significant differences in LCB Index

Tan Delta

LCB Index

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Practical example, linear and branched Polymer

Keltan 6950 Nordel 5565

Mooney ML 1+4 [MU] 65 65

Ethylen [%] 48 50

ENB content [%] 9 7.5

Distribution medium medium

Degree of branching Branched Linear

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Practical example, linear and branched Polymer

Frequency Sweep

Shear - thinning

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Practical example, linear and branched Polymer

Frequency Sweep

Mooney

Low

Frequency

Page 25: Linear and Non Linear Rheological Measurements on … TA Instruments.… · TAINSTRUMENTS.COM Physical description of Polymers Strain Sweep -LAOS 0.0 π 0.5 π 1.0 π 1.5 π 2.0 π-8000-6000-4000-2000

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Physical description of Polymers

Strain Sweep - LAOS

High Strain

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Physical description of PolymersStrain Sweep - LAOS

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Recipe of Compounds

Keltancompound

Nordelcompound

phr phr

EPDM (LCB) 100

EPDM, linear 100

Fast Extrusion Furnace (FEF) carbon black 95 95

Chalk 50 50

Paraffinic Oil 65 65

ZnO 6 6

Stearic acid 1 1

Drying agent 9 9

Antiaging agent 0,5 0,5

Sulfur and accelerator 4,5 4,5

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Physical description of filled Polymers

Strain Sweep - PAYNE

Tensile Strength [Mpa]

Keltan cmp. 9.25

Nordel cmp. 8.32

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Kinetic description of filled PolymersVulcanisation

Keltan compound

Nordelcompound

S' Min [dNm] 1.21 1.4

S' Max [dNm] 20.44 23.17

ENB content [%] 9 7.5

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Physical description of filled PolymersFrequency Sweep

Shear thinning

15%

5%

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Extrusion – Machine parameters

Extrusion Keltan compound Nordel compound

Temp. extruder [°C]70 70

Pressure die [bar]91.3 102

Current [A]111.5 124

Speed [m/min]10.5 10.5

Temp. Mass [°C]

114 114-125

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Rubber compound process troubleshooting

Rubber compound extrusion.

Serious processing problem in production

Summary of observations:

• All batches passed standard QC tests.

• QC test involves rheometer only (MDR).

• One batch gave higher extrusion head pressure and temperature,

higher swell and surface defect (“Orange skin”) suggesting possible

scorch in the extruder.

• The faulty batch was compared to a trouble free batch.

Good

Bad

160° C

GoodBad

Both compounds have identical or almost identical ML and

MH.

The faulty compound exhibits a lower cure rate (?)

The faulty compound exhibits a significantly LONGER

scorch time (??????)

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Rubber compound process troubleshooting

Good

Bad

Non isothermal cure test (80° C – 180° C)

Some differences in

the uncured state

Non isothermal cure test confirms

identical ML and MH and longer

cure time for the faulty batch

Some differences are observed on

G’ and Tangent δ before cure

suggesting that viscoelastic

properties of uncured compounds

being different.

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Rubber compound process troubleshooting

Good

Bad

RPA testing “Payne” diagram – 100° C

Bad compound shows higher

modulus at both low and high

strain.

This suggest that filler

dispersion is not the cause of

the problem.

The problem therefore stays

in either polymer quality of

filler content.

Page 35: Linear and Non Linear Rheological Measurements on … TA Instruments.… · TAINSTRUMENTS.COM Physical description of Polymers Strain Sweep -LAOS 0.0 π 0.5 π 1.0 π 1.5 π 2.0 π-8000-6000-4000-2000

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Rubber compound process troubleshooting

Frequency sweep at 100° C Strain sweep at 100° C

Bad and good batches show almost

identical viscoelastic properties in both

frequency and strain sweep.

Only some significant difference is

observed at very low shear rate

(frequency) on Tangent δ.

Page 36: Linear and Non Linear Rheological Measurements on … TA Instruments.… · TAINSTRUMENTS.COM Physical description of Polymers Strain Sweep -LAOS 0.0 π 0.5 π 1.0 π 1.5 π 2.0 π-8000-6000-4000-2000

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Rubber compound process troubleshooting

W disp.

(J)

Good 168.94

Bad 177.11

ISO Standard method 4664-1

Where ε is the ellipse area or the energy lost per

oscillation

γ0 is the maximum strain

σ0 is the maximum stressε = π.γ0.σ0.sin δ

The bad compound has been

found to dissipate almost

10% higher energy per cycle

in non-linear conditions.

Premature scorch for this

compound is produced by

large heat generation in the

extruder.

LAOS test 100° C, 90° arc, 0.2 Hz

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Summary and Conclusion

• The combination of linear and non linear

viscoelasticity measurements offers a unique tool for

polymer characterization.

• It clearly differentiates between MWD effect from

LCB effect

• It proved itself the fastest and most sensitive test for

detection of ultra low LCB content in polymers.

• This technique was successfully demonstrated on

SBR, BR, IIR, EPDM, NR, PE, PP, FKM, PC etc.

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Thank You

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Rheology, and Microcalorimetry