Lecture_16_chapter 5

Mechanical Engineering Department

Dr. Khaled Mezghani

CHAPTER 5
Dynamic Mesurements
of Viscoelasticity

ME-578. Mechanical Prop. of Eng. Polym. Dr. Khaled Mezghani Lecture 12, Slide 1

Outline

1. Dynamic Mechanical Measurements

1. Complex Modulus
2. Complex Compliance
2. Forced Vibration Methods

ME-578. Mechanical Prop. of Eng. Polym. Dr. Khaled Mezghani Lecture 12, Slide 2

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Response for a Viscoelastic Material

 At short times (high frequencies) the

response is solid-like

 At long times (low frequencies) the

response is liquid-like

THE HISTORY OF LOADING IS CRUCIAL

ME-578. Mechanical Prop. of Eng. Polym. Dr. Khaled Mezghani Lecture 12, Slide 3

Time-Dependent Viscoelastic Behavior:

Solid and Liquid Properties of "Silly Putty"

T is short [< 1s] T is long [24 hours]

ME-578. Mechanical Prop. of Eng. Polym. Dr. Khaled Mezghani Lecture 12, Slide 4

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Dynamic Mechanical Testing:

Viscoelastic Material Response

Phase angle δ 0° < δ < 90°

Strain
e = e0 sin(ωt)

Stress

σ = σ0 sin(ωt+δ)

ME-578. Mechanical Prop. of Eng. Polym. Dr. Khaled Mezghani Lecture 12, Slide 5

Dynamic Mechanical Testing:

Response for Classical Extremes

Purely Viscous
Purely Elastic Response Response
(Hookean Solid) (Newtonian Liquid)
δ = 90°
δ = 0°

Stress Stress

Strain Strain

ME-578. Mechanical Prop. of Eng. Polym. Dr. Khaled Mezghani Lecture 12, Slide 6

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DMA Viscoelastic Parameters

The Modulus: Measure of materials
overall resistance to deformation. E* = Stress/Strain
The Elastic (Storage) Modulus:
Measure of elasticity of material. The
ability of the material to store energy.
E' = (stress/strain)cosδ

The Viscous (loss) Modulus:

The ability of the material to dissipate E" = (stress/strain)sinδ
energy. Energy lost as heat.

Tan Delta:
Measure of material damping - such
as vibration or sound damping. Tan δ = E"/E'
ME-578. Mechanical Prop. of Eng. Polym. Dr. Khaled Mezghani Lecture 12, Slide 7

Storage and Loss of a Viscoelastic Material

LOSS

TENNIS
X BALL

STORAGE

ME-578. Mechanical Prop. of Eng. Polym. Dr. Khaled Mezghani Lecture 12, Slide 8

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 Lecture_16_chapter 5

DMA Viscoelastic Parameters:

Damping, tan δ

E*
Dynamic measurement E"
represented as a vector
Phase angle δ

E'
zThe tangent of the phase angle is the ratio of the
loss modulus to the storage modulus.
tan δ = E"/E'
z"TAN DELTA" (tan δ) is a measure of the
damping ability of the material.
ME-578. Mechanical Prop. of Eng. Polym. Dr. Khaled Mezghani Lecture 12, Slide 9

Dynamic Mechanical Testing

Deformation
z An oscillatory (sinusoidal) e = e0 sin(ωt)
deformation (stress or strain)
is applied to a sample.
Response
z The material response σ = σ0 sin(ωt)
(strain or stress) is measured.

z The phase angle δ, or phase δ

Phase angle
shift, between the deformation e = e0 sin(ωt)
and response is measured.
σ = σ0 sin(ωt+δ)
ME-578. Mechanical Prop. of Eng. Polym. Dr. Khaled Mezghani Lecture 12, Slide 10

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 Lecture_16_chapter 5

Viscoelastic Parameters & Energy

The Modulus (G*): σ
Measure of materials overall G* = = G1 + i G 2
resistance to deformation. e
The Elastic (Storage) Modulus (G1): σ0 2E
Measure of elasticity of material. The G1 = cos (δ ) =
ability of the material to store energy (E). e0 e 02

The Viscous (loss) Modulus (G2): σ0 ΔE

The ability of the material to dissipate G2 = sin (δ ) =
energy. Energy lost (ΔE) as heat. e0 π e 02
Tan Delta (tan(δ)): G2 ΔE
Measure of material damping - such tan (δ ) = =
as vibration or sound damping. G1 2π E
ME-578. Mechanical Prop. of Eng. Polym. Dr. Khaled Mezghani Lecture 12, Slide 11

DMA Viscoelastic Parameters

i
G1
109

tan δ R
Log G (Pa)

G* = G1 + i G2
σ0
G2 G1 = cos (δ )
e0
σ0
G2 = sin (δ )
105 e0
G2
Rubbery Viscoelastic Glassy tan (δ ) =
Log ω G1
ME-578. Mechanical Prop. of Eng. Polym. Dr. Khaled Mezghani Lecture 12, Slide 12

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Example

A bar of polymer is of length 60 mm and has a

rectangular cross-section of dimensions 10 mm x 4 mm.
It is subjected to a force acting along the length of the
bar and oscillating sinusoidally between -150 and 150 N
at a frequency of 50 Hz. The imaginary part of the
complex tensile compliance of the polymer at 50 Hz is
J” = 3.7 x 10-9 Pa-1. Calculate the power input required
to sustain the oscillations.

ME-578. Mechanical Prop. of Eng. Polym. Dr. Khaled Mezghani Lecture 12, Slide 13

DMA

ME-578. Mechanical Prop. of Eng. Polym. Dr. Khaled Mezghani Lecture 12, Slide 14

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 Lecture_16_chapter 5

DMA

ME-578. Mechanical Prop. of Eng. Polym. Dr. Khaled Mezghani Lecture 12, Slide 15

DMA

ME-578. Mechanical Prop. of Eng. Polym. Dr. Khaled Mezghani Lecture 12, Slide 16

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 Lecture_16_chapter 5

DMA

ME-578. Mechanical Prop. of Eng. Polym. Dr. Khaled Mezghani Lecture 12, Slide 17

Dynamic Mechanical Analyzer (DMA)

¾ DMA is the general name given to an instrument

that mechanically deforms a sample and
measures the sample response. The deformation
can be applied sinusoidally, in a constant (or
step) fashion, or under a fixed rate. The
response to the deformation can be monitored as
a function of temperature or time.

ME-578. Mechanical Prop. of Eng. Polym. Dr. Khaled Mezghani Lecture 12, Slide 18

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 Lecture_16_chapter 5

Measure principles of DMA

Sample

Displacem ent Sensor - M easures Strain

M otor Applies Force (Stress)

•The DMA is a stress (force) controlled instrument.

•It is composed of the following ;
• A motor which applies the force (stress to the sample).
•A displacement sensor that measures strain (Amplitude).
•When programming an experiment the deformation is input in the
form of Amplitude or strain.
•The instrument then applies force (the control parameter) until it
measures the requested Amplitude or strain.

ME-578. Mechanical Prop. of Eng. Polym. Dr. Khaled Mezghani Lecture 12, Slide 19
Ó1996, TA Instruments, Inc.

Schematic of a typical DMA

BIFILAR-WOUND FURNACE
SAMPLE
CLAMPS

LOW MASS, HIGH STIFFNESS

CLAMPING FIXTURES

AIR BEARING
AIR SLIDE
BEARING

OPTICAL
ENCODER

DRIVE MOTOR

ME-578. Mechanical Prop. of Eng. Polym. Dr. Khaled Mezghani Lecture 12, Slide 20

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 Lecture_16_chapter 5

DMA Clamps & Geometries

Shear
Sandwich Bending or Compression
Cantilever

Tension
Motor Applies Force
Strain Read by
Optical Encoder.

ME-578. Mechanical Prop. of Eng. Polym. Dr. Khaled Mezghani Lecture 12, Slide 21

Viscoelastic Spectrum for a Typical Amorphous Polymer

Glassy Region
Transition
Region
Rubbery
log E' (G') and E" (G")

Plateau
Terminal Region
Region
Viscoelastic
liquid
Very hard and
rigid solid

Stiff to Soft rubber

Storage Modulus (E' or G')

Loss Modulus (E" or G")

Temperature
ME-578. Mechanical Prop. of Eng. Polym. Dr. Khaled Mezghani Lecture 12, Slide 22

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 Lecture_16_chapter 5

Dynamic Time Sweep

Deformation zThe material
Strain

response is
monitored at a
Time constant frequency,
amplitude and
temperature.

zUSES
ËCure Studies
ËDegradation

ME-578. Mechanical Prop. of Eng. Polym. Dr. Khaled Mezghani Lecture 12, Slide 23

Dynamic Strain Sweep

Deformation
zThe material response to
Strain

increasing deformation
amplitude is monitored
Time at a constant frequency
and temperature.

zUSES
ËIdentifyLinear
Viscoelastic Region
ËResilience

ME-578. Mechanical Prop. of Eng. Polym. Dr. Khaled Mezghani Lecture 12, Slide 24

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Dynamic Strain Sweep:

Material Response
Linear
Region: Non-linear Region:
Modulus Modulus is a function of strain
independent
of strain

E' or G'

Stress

Constant γc = Critical Strain

Slope

Strain (amplitude)
ME-578. Mechanical Prop. of Eng. Polym. Dr. Khaled Mezghani Lecture 12, Slide 25

Frequency Sweep
Deformation z The material response
Strain

to increasing
frequency (rate of
deformation) is
Time monitored at a
constant amplitude
and temperature.
zUSES
ËHigh and Low Rate (short
and long time) modulus
properties.
ËPolymer melt processing
(shear sandwich).
ËExtend range with TTS

ME-578. Mechanical Prop. of Eng. Polym. Dr. Khaled Mezghani Lecture 12, Slide 26

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Frequency Sweep:
Material Response
Transition
Rubbery Region
Terminal Plateau
log E' (G') and E" (G")

Region Region

Glassy Region

1
2 Storage Modulus (E' or G')
Loss Modulus (E" or G")

log Frequency (rad/s or Hz)

ME-578. Mechanical Prop. of Eng. Polym. Dr. Khaled Mezghani Lecture 12, Slide 27

Dynamic Temperature Ramp

¾A linear heating rate
is applied. The
material response is
monitored at a
constant frequency time between
Temperature

data points
and constant m = ramp rate
(°C/min)
amplitude of
deformation. Data is Denotes Oscillatory
taken at user defined Measurement
time intervals. time (min)

ME-578. Mechanical Prop. of Eng. Polym. Dr. Khaled Mezghani Lecture 12, Slide 28

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Temperature Step & Hold/Single

Frequency/Multi-Frequency
¾A step and hold
temperature
profile is applied.
The material

Temperatur
response is Soak Time Step
monitored at one, Size
or over a range
of frequencies, at
e
Denotes Oscillatory
constant Measurement
amplitude of Time
deformation.

ME-578. Mechanical Prop. of Eng. Polym. Dr. Khaled Mezghani Lecture 12, Slide 29

Dynamic Temperature Ramp or Step and Hold:

Material Response

Glassy Region Transition

Region Rubbery Plateau
Region Terminal Region
log E' (G') and E" (G")

Storage Modulus (E' or G')

Loss Modulus (E" or G")

ME-578. Mechanical Prop. of Eng. Polym. Temperature

Dr. Khaled Mezghani Lecture 12, Slide 30

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 Lecture_16_chapter 5

The Viscoelastic Spectrum

log E' (G') and E" (G")

log E' (G') and E" (G")

(E' or G') (E' or G')

(E" or G") (E" or G")

log Frequency Temperature

log E (t) or G (t)

log Jc

log Time log Time

ME-578. Mechanical Prop. of Eng. Polym. Dr. Khaled Mezghani Lecture 12, Slide 31

Example 2

Establish and plot the variation with frequency of the

storage and loss moduli for materials which can have
their viscoelastic behavior described by the following
models:

(i) A Maxwell model with E = 1 GPa and η = 0.1 GPa.s

(ii) A Standard Linear Solid with E1 = 2 GPa, E2 = 0.1
GPa, η = 1 GPa.s

ME-578. Mechanical Prop. of Eng. Polym. Dr. Khaled Mezghani Lecture 12, Slide 32

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Maxwell Model
dε 1 dσ σ
The governing equation

= +
for this model is:

dt E dt η
E

Assume that:

ε = ε 0e i (ωt ) and σ = σ 0e i (ωt +δ )

Then:
1
i (ωt ) i (ωt +δ ) 1
ε 0i ωe = σ 0i ωe + σ 0e i (ωt +δ )
E η
i (ωt +δ )
i ω σ 0e 1 σ 0e i (ωt +δ )
iω = ⋅ + ⋅
E ε 0e i (ωt )
η ε 0e i (ωt )
ME-578. Mechanical Prop. of Eng. Polym. Dr. Khaled Mezghani Lecture 12, Slide 33

Maxwell Model
Therefore:
iω σ 1 σ iω * 1 *
iω = ⋅ + ⋅ = ⋅G + ⋅G
E ε η ε E η
Where E* is the complex modulus:
i ωη E
Rearranging gives:
G* =
E + i ωη
Using the fact that (a + ib)x(a - ib) = a2 – i2b2 = a2 + b2
i ωη E E − i ωη i ωη E 2 + ω 2η 2 E
G =
*
⋅ =
E + i ωη E − i ωη E 2 + ω 2η 2
ω 2η 2 E ωη E 2
G = 2
*
+i 2 = G1 + iG 2
E +ω η 2 2
E +ω η2 2

ME-578. Mechanical Prop. of Eng. Polym. Dr. Khaled Mezghani Lecture 12, Slide 34

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Maxwell Model
ω 2η 2 E ωη E 2
G = 2
*
+i 2 = G1 + iG 2
E +ω η 2 2
E +ω η2 2

Therefore:

E η 2ω 2 E 2ηω
G1 = 2 G2 = 2
E + η 2ω 2 E + η 2ω 2
G2 E
tan(δ ) = =
G1 ηω

ME-578. Mechanical Prop. of Eng. Polym. Dr. Khaled Mezghani Lecture 12, Slide 35

1.0 Maxwell Model

0.9 E Loss tangent Storage Modulus
0.8 E
η tan(δ ) =
ηω
E η 2ω 2
0.7 G1 = 2
0.6
E + η 2ω 2
G1, G2, tan (δ)

0.5 Loss Modulus

0.4 E 2ηω
G2 = 2
0.3 E + η 2ω 2
0.2
0.1

0.1 1 10 100 1000

Log (ω)
ME-578. Mechanical Prop. of Eng. Polym. Dr. Khaled Mezghani Lecture 12, Slide 36

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Standard Linear Solid Model

The governing equation
for this model is:
σ1
ε1
E1 σ2
σ3 ε2
ε3 E2
η

dσ dε
η + E1σ = η (E1 + E2 ) + E1 E2ε
dt dt
ME-578. Mechanical Prop. of Eng. Polym. Dr. Khaled Mezghani Lecture 12, Slide 37

Standard Linear Solid Model

E 12 E 2 + ( E 1 + E 2 )η 2ω 2 E 12ηω
G =
*
+i 2
E1 +η ω
2 2 2
E 1 + η 2ω 2
Therefore: E 12 E 2 + ( E 1 + E 2 )η 2ω 2
G1 =
E 12 + η 2ω 2
E 12ηω
G2 = 2
E 1 + η 2ω 2
G E 12ηω
tan(δ ) = 2 = 2
G1 E 1 E 2 + ( E 1 + E 2 )η 2ω 2
ME-578. Mechanical Prop. of Eng. Polym. Dr. Khaled Mezghani Lecture 12, Slide 38

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2.5 Standard Linear Solid Model

E 12ηω E 12 E 2 + ( E 1 + E 2 )η 2ω 2
tan(δ ) =
E 12 E 2 + ( E 1 + E 2 )η 2ω 2 G1 =
E 12 + η 2ω 2
2.0 Loss tangent
Storage Modulus
1.5
ε = ε 0e i (ωt )
G1, G2, tan (δ)

1.0 σ = σ 0e i (ωt +δ ) Loss Modulus

E 12ηω
G2 = 2
E 1 + η 2ω 2
0.5

0.0
0.01 0.1 1 10 100
Log (ω)
ME-578. Mechanical Prop. of Eng. Polym. Dr. Khaled Mezghani Lecture 12, Slide 39

Standard Linear Solid Model

However, the predicted relaxation is narrower than that of the experimental PE.
ME-578. Mechanical Prop. of Eng. Polym. Dr. Khaled Mezghani Lecture 12, Slide 40

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DMA Modes Of Operation

• DMA Multi-frequency Stress/Strain
– Time, temperature & Frequency dependence of
Storage & Loss Modulus, Tan Delta.
– To Compare materials (Modulus & Transition
temperatures).
– Thermoset Curing Behaviour.
– Projection of Long term performance under Load
using TTS
• DMA Multi-strain
– Evaluation of Linear Viscoelastic Region (LVR).
– “Mullens”-effect in elastomers.
• DMA Multi-stress
– Stress fatigue
– Stress-dependent LVR

ME-578. Mechanical Prop. of Eng. Polym. Dr. Khaled Mezghani Lecture 12, Slide 41

DMA - Single & Dual Cantilever Clamp

Clamped Bending

ME-578. Mechanical Prop. of Eng. Polym. Dr. Khaled Mezghani Lecture 12, Slide 42

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Measure principles of DMA

Sample

Movable Stationary
clamp Clamp

¿ Good general purpose mode (thermoplastics, elastomers)

¿ Highly damped materials can be measured
¿ Best mode for evaluating the cure of supported materials

ME-578. Mechanical Prop. of Eng. Polym. Dr. Khaled Mezghani Lecture 12, Slide 43

DMA - Single Cantilever Clamp

Sample

Stationary
Clamp

Movable
clamp

 Best general purpose mode (thermoplastics)

 Same deformation mode as DMA 983
 Preferred mode over dual cantilever for most neat
thermoplastics (unreinforced) except elastomers
 Clamping torque is important
ME-578. Mechanical Prop. of Eng. Polym. Dr. Khaled Mezghani Lecture 12, Slide 44

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DMA
3 POINT
BENDING

3 Point Bending

ME-578. Mechanical Prop. of Eng. Polym. Dr. Khaled Mezghani Lecture 12, Slide 45

DMA 3 POINT BENDING

Sample

Stationary Fulcrum

Moveable Force
Clamp

 Best mode for measuring medium to high modulus materials

 Conforms with ASTM standard test method for bending
 Purest deformation mode since clamping effects are
eliminated

ME-578. Mechanical Prop. of Eng. Polym. Dr. Khaled Mezghani Lecture 12, Slide 46

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DMA Tension : Thin Film

Tension

ME-578. Mechanical Prop. of Eng. Polym. Dr. Khaled Mezghani Lecture 12, Slide 47

DMA Tension : Fiber

Tension

ME-578. Mechanical Prop. of Eng. Polym. Dr. Khaled Mezghani Lecture 12, Slide 48

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DMA : Tension Mode

Stationary
Clamp

Sample
(film, fiber,or thin sheet)

Movable clamp

 Best mode for evaluation of thin films and fibers (bundle or single
filaments)
 Small samples of high modulus materials can be measured
 TMA constant force & force ramp measurements (mini-tensile tester)
 Force Track & constant force control

ME-578. Mechanical Prop. of Eng. Polym. Dr. Khaled Mezghani Lecture 12, Slide 49

DMA
Shear Sandwich

Simple Shear

ME-578. Mechanical Prop. of Eng. Polym. Dr. Khaled Mezghani Lecture 12, Slide 50

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DMA Shear Sandwich

Movable Sample
Clamp
Stationary
Clamp

z Square sample configuration provides pure shear deformation

z Provides Shear Moduli: G*, G', G" & G(t)
z Good for evaluating highly damped soft solids such as gels and
adhesives & elastomers > Tg
z Can be used for high viscosity melts and resins

ME-578. Mechanical Prop. of Eng. Polym. Dr. Khaled Mezghani Lecture 12, Slide 51

DMA - Compression

Compression

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