2018 E-Basics of Rheology Short

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BASICS OF RHEOLOGY

Markus Nemeth
Business Area Rheometry, Training & Application
1 Rheology and Viscous Behavior

Rheology
to describe
deformation and flow behavior of all kinds of materials
rhei or rheo … to flow

Rheometry
measurement of rheological data
Image: Drugstore (Apotheken) museum
in Heidelberg, Germany

2
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1 Rheology and Viscous Behavior
Each material under load shows viscoelastic behavior as a mixture of
viscous and elastic behavior. Using a simple illustrative picture

The Rheology Road


viscous  viscoelastic  elastic

ideally viscous viscoelastic viscoelastic ideally elastic


liquids liquids solids solids
such as water, oils such as glues, such as pastes, rigid, as a stone, steel
Viscosity Law shampoos gels, rubbers Elasticity Law
 rotational tests  |
 oscillatory tests  3
APXXYYY Ref.: Durou, J.-F.: Cérémonie du Thé, Mauritanie, 1999. Nouvelles Images, Lombreuil.
1 Rheology and Viscous Behavior
What is viscosity ?
Internal friction
between the molecules and particles, when gliding
along each other in a flowing state, or:
flow resistance
(Newton, in 1687: defectus lubricitatus)

comparison of size
molecules of solvents: about 0.5 nm
macro-molecules (polymer coils): about 50 nm . 0,5 nm
particles (minerals): about 5 µm = 5000 nm 0 50 nm

size ratio of molecules and particles


is about 1:100 to 1:10,000 (e.g. 1:1000)

illustrative comparison for 1:1000


a molecule as a 10 cm (0.1m) long fish,
a particle as a 100 m long ship 4
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2 Simple Viscosity Tests

Trowel test
- highly viscous fluids: thick
- low- viscosity fluids: thin
e.g. for dispersions

Finger test
- tacky: long
- less tacky: short
e.g. for adhesives,
offset- printing inks, dough

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2 Simple Viscosity Tests

Flow cups
measurement of the
flow time
of low- viscosity liquids,

determination of the
kinematic viscosity
weight- dependent viscosity

Examples:
oils, solvent- based coatings,
gravure printing inks and flexo printing inks

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2 Simple Viscosity Tests
Rotational viscometers
preset: rotational speed
determination: torque

Relative viscosity values


are measured according to
ISO 2555 and ISO 3219
using typical spindles in the form of
- cylinders
- disks
- T- bars
- pins
Example: ViscoQC of Anton Paar 7
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3 Rheometers and Measuring Geometries
Measuring geometries for rotational and oscillatory rheometers
according to DIN 53019 (for all the 3 geometries) and ISO 3219 (only for CC and CP)
to measure absolute values of viscosity

cone- plate, CP parallel- plates, PP


for liquids; for dispersions
useful for
only with limited particle size,
gels, pastes, soft solids,
recommended:   2°
polymer melt
concentric cylinders, CC Example: For CP 25-1,
recommended:
with 2R = 25 mm and = 1°,
0.50 mm  H  1.00 mm
for low- viscosity liquids, typically a = 50 µm; thus, for a max.
ratio of radii Re/Ri  1.0847 particle size of d  (a/10) = 5 µm 8
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3 Rheometers and Measuring Geometries

rotation oscillation

for for
shear tests shear tests,
and torsional tests
tensile tests and
tensile tests
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4 Definitions: Shear Stress, Shear Rate, Viscosity
The two- plates model

shear stress  = F/A


unit: 1 N / m2 = 1 Pa

shear rate ሶ = (D) = v / h


unit: 1 m / (sm) = 1 / s = 1 s-1

Laminar flow with flowing layers


in contrast to turbulent flow showing vortices
ሶ = dv / dh = const / const = const
 e- learning  movie  movie
(laminar, 2-P-M) (peas) (turbulence) 10
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4 Definitions: Shear Stress, Shear Rate, Viscosity
Typical values of shear rates
process shear rates (s-1)
sedimentation < 0.001 to 0.01
surface levelling 0.01 to 0.1
sagging 0.01 to 1
dip coating 1 to 100
extrusion 10 to 1000
pipe flow, pumping, filling into containers 10 to 10,000
mixing, stirring 10 to 10,000
coating, painting, brushing 100 to 10,000
spraying 1000 to 10,000
(high- speed) coating, blade coating 100,000 to 1 mio.
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4 Definitions: Shear Stress, Shear Rate, Viscosity
Practical example
Painting with a brush

brush velocity
(v = 0.5 m/s)

wet layer thickness


(h = 200 µm)

v
ሶ = =
0.5 m
h 0.0002 m·s
= 2500 s-1

Calculation of the shear rate: similar to the two- plates model


coatings 12
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4 Definitions: Shear Stress, Shear Rate, Viscosity
definition of the

(shear) viscosity

 =  / ሶ
unit: 1 Pa / (1/s) = 1 Pas = 1000 mPas
Isaac Newton (1643 to 1727);
he writes about the pascal- seconds,
flow resistance of fluids milli- pascal- seconds
(e.g. of air and water).
Previously used unit:
However, this laterly so- called
1 cP = 1 mPas
Viscosity Law “of Newton“ (centi- poises)
was formulated not before However, this is not an SI- unit.
the 19. century (e.g. by G.G. Stokes in 1845). 13
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6 Flow Behavior

Overview
Viscosity curves

1 ideally viscous (Newtonian)


2 shear- thinning (pseudoplastic)
3 shear- thickening (dilatant)

14
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6 Flow Behavior

Mineral oil
CC 27
constant viscosity concentric cylinders
T = +50°C

viscosity shear stress

shear rate mineral oils 15


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6 Flow Behavior
Silicone oil
constant viscosity
CP 50-2
cone- plate

T = +23°C

diagrams
on a logarithmic scale
Advantage: Here, also
the range of very low values
can be presented clearly.

silicone oils 16
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6 Flow Behavior

 sense of the double- tube experiment,


with decreasing shear stress 1 polymer solution
viscosity is velocity- dependent
shear- thinning

2 mineral oil
constant viscosity
ideally viscous

polymers, mineral oils 17


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6 Flow Behavior
at rest when shearing

Polymers
with chain- like
macro- molecules

molecules are coiled, deformation in shear direction,


entanglements disentanglements

Consequence: shear- thinning flow behavior, decreasing viscosity

Typical size: molecule coil, hydrodynamic diameter 5 nm to 50 nm


Example: polyethylene PE, molar mass M = 100 kg/mol,
molecules with L = 1 m = 1000 nm (stretched), d = 0.5 nm, ratio L/d = 2000:1
Comparison: spaghetti noodles, 1 mm thick and 2 m long polymers 18
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6 Flow Behavior
at rest when shearing

Suspensions
with particles
showing the shape
of needles or platelets

particles are particles are


suspended randomly orientated in
(when without flow direction.
interaction forces)
Consequence: shear- thinning flow behavior, decreasing viscosity
Typical size:
1) metallic- effect pigments, aluminum flakes,
diameters d = 7µm to 30 m, thickness h = 0.2 µm to 1 m, ratio d/h = 30:1
2) ceramics, such as Bentonite: length/ width/ thickness, L x b x h = 800 x 800 x 1 (in nm) dispersions 19
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6 Flow Behavior
at rest when shearing

Suspensions
with agglomerated
particles

The agglomerates are The agglomerates


including and immobilizing also are disintegrated.
a part of the dispersion liquid.

Consequence: shear- thinning flow behavior, decreasing viscosity

Typical size: Primary particles 1 nm to 10 nm,


aggregates up to 100 nm, agglomerates up to 100 m = 0.1 mm dispersions 20
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6 Flow Behavior
at rest when shearing

Emulsions
with dispersed droplets

The droplets show The doplets are deformed


the shape of and show the shape of
spheres. ellipsoids.

Consequence: shear- thinning flow behavior, decreasing viscosity

 movie
Typical size: droplets in milk, fat particles: 0.1 m to 10 m emulsions (emulsion 1) 21
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6 Flow Behavior
Rheo- microscopy: Emulsion of water in silicone oil

at
rest

Size and shape of the droplets


are dependent on sample
preparation and shear rate.
after
shearing
Viscosity may increase
due to droplet size division,
hence an increase in the
lg ሶ volume specific surface.
emulsions 22
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6 1 Flow Behavior300
Pa
Pa∙s
250
0.8 O/W emulsion
200 O/W Emulsion
0.7
 Viscosity
 0.6 150  E1 undiluted
 Shear Stress
0.5
100 O/W Emulsion with 10% water
0.4  Viscosity
50 E2 with 10% additional water
0.3  Shear Stress
0.2 0
0 200 400 600 1/s 1,000
.
Shear Rate 
Typical behavior of
dispersions
initially strongly, and then less
shear- thinning

emulsions 23
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6 1 Flow Behavior300
Pa
Pa∙s
250
0.8 Gravure printing inks
These 200
3 samplesO/Wwith the
Emulsion
diluted
0.7
same pigment concentration
 Viscosity
 0.6 showed the same flow time
150 S1 binder
 Shear Stress
0.5 when testing with a flow cup the useful one
100 O/W Emulsion with 10% water
0.4 
50
Viscosity
S3 binder
0.3  Shear Stress spattering
0.2 0
0 200 400 600 1/s 1,000
.
S2 binder
Shear Rate  50/50 mix of 1 & 3
measuring range Summary:
of the flow cup
flow cup tests
cover only a
limited shear rate range.
printing inks 24
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6 1 Flow BehaviorPa
300
Pa∙s
250
0.8
200 O/W Emulsion
0.7
 Viscosity Wall paper paste
 0.6 150 
 Shear Stress
0.5 aqueous methylcellulose solution
100 O/W Emulsion with 10% water
0.4  Viscosity
50 T = +23°C
0.3  Shear Stress
0.2 0
0 200 400 600 1/s 1,000
. typical behavior of
Shear Rate 
polymer solutions
continued shear- thinning

polymers, adhesives 25
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6 1 Flow Behavior300
Pa
Pa∙s
250
0.8 Wall paper paste
200 O/W Emulsion
0.7
 Viscosity aqueous solution of methylcellulose,
 0.6 150  uncrosslinked polymer
 Shear Stress
0.5
100 T = +23°C
O/W Emulsion with 10% water
0.4 
ሶ < 0.1 s-1
Viscosity
50 for
0.3  Shear Stress
0.2 0
0 200 400 600 1/s 1,000 plateau of the
.
Shear Rate  zero- shear viscosity

Presentation on a
logarithmic scale
to illustrate the behavior
in the low- shear range.
polymers 26
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6 1 Flow Behavior300
Pa
Pa∙s
Uncrosslinked
250 polymers in the low- shear range,
0.8
and
200 theO/W
zero- shear viscosity
Emulsion
0.7
 Viscosity
0.6 Superposition
150 of two processes
   Shear Stress
0.5 1)100Orientation of the
O/W Emulsion withmacro-
10% watermolecules under shear load
0.4  disentanglements
 Viscosity
0.3
50
 here, the viscosity
Shear Stress is decreasing
0.2
0
2)0
200 400 600 1/s 1,000
Re - coiling due to visco- elastic behavior
.  re- entanglements
Shear Rate 
 here, the viscosity is increasing

Result:
In the low-shear range there is no change in the total viscosity value,
which is referred to as the 0 - value.
This low- shear range mostly occurs for ሶ < 1 s-1
polymers 27
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6 1 Flow Behavior300
Pa
Pa∙s
250
0.8 Polymer solutions
200 O/W Emulsion uncrosslinked polymers
0.7
 Viscosity and zero- shear viscosity
 0.6 150 
 Shear Stress
0.5
100 P1 compared to P2
O/W Emulsion with 10% water
0.4  Viscosity shows a higher plateau value of the
50
0.3  Shear Stresszero- shear viscosity and therefore a
0.2 0
0 200 400 600 1/s 1,000 a higher average molar mass M
.
Shear Rate 
with P1 and P2 having the same
chemical structure and polymer concentration

polymers 28
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7 Yield Point (via Flow Curves)

flow curves on a linear scale

Yield point
as the limiting value of the shear stress
Break of the structure-at-rest.
There is a super- structure due to a
chemical- physical network of interactive forces.

1 without a yield point


2 showing the yield point 0
as an interception
on the  - axis 29
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7 Yield Point (via Flow Curves)
Yield point determination
via
mathematical curve fitting
B for flow curves on a linear scale
C (approximation, "regression")

HB regression models

Yield points
1) Bingham model  = B + B  ሶ are not material constants
with “Bingham yield point“ and “Bingham viscosity“
as they depend as well on the
2) Casson model  = 𝐂 +  · ሶ measuring method
with “Casson yield point“ and “Casson viscosity“ as well as on the
3) Herschel / Bulkley model  = HB + HB  ሶ p analysis method
with “HB yield point“, “HB viscosity“ and exponent p used.
30
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9 Time- dependent Behavior (Rotation)

Sometimes Sometimes
cats are cats are very
very curious stupid

Requirements for coatings: structure recovery just in the right time


1) not too fast, and thus, good levelling
2) not too slow, and thus, not too much sagging,
desired wet- layer thickness
31
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9 Time- dependent Behavior (Rotation)

Structure recovery,
step test
(3ITT, 3 intervals thixotropy test)
Here as a rotational test,
to determine „thixotropic behavior“.
Preset
1 low- shear conditions
2 high- shear conditions
3 low- shear conditions
Measuring result
1 state at rest
2 structural decomposition
3 structural regeneration
coatings 32
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9 Time- dependent Behavior (Rotation)
Coatings
step tests

1 with the gellant


fast structural recovery
 • less sagging
structure • high wet- layer thickness
recovery • maybe poor levelling

2 with the viscosifier


slow structural recovery
• good levelling
• maybe too much sagging
coatings 33
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11 Viscoelastic Behavior

Tack and stringiness,


e.g. of adhesives, printing inks,
or food (mouth sensation)

Stirring process: rod climbing


Weissenberg effect , poor mixing result
(Karl Weissenberg, 1893 to 1976, rheologist)

Extrusion: extrudate swelling


e.g. dimension stability

Result: In many cases,


viscosity values only are not sufficient
since elastic effects are occurring,
resulting in viscoelastic behavior.
34
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12 Definitions: Deformation, Strain

two- plates model

shear stress
 = F/A
unit: 1 N / m2 = 1 Pa (Pascal)

shear deformation or shear strain


 = s/h
unit: 1 m / m = 1 = 100 %
35
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14 Definition: Shear Modulus

law of springs: F/s=C


spring force F
deflection path s
spring constant C (stiffness)

Definition
shear modulus G=/
Robert Hooke (1635 to 1703),
unit: (1 Pa / 1 = ) 1 Pa
in 1676 he states for solids
proportionality of force and deformation.
further units:
However, the laterly so-called
1 GPa = 1000 MPa = 106 kPa = 109 Pa
“Elasticity Law of Hooke“
was formulated not before the 19. century Giga- pascals, Mega- pascals, kilo- pascals
(e.g. by T. Young in 1807,
or A.L. Cauchy in 1827).  movie (bouncing balls) 36
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15 Oscillatory Tests

Two- plates model, equipped with two sensors,


on top: preset of deflection path (strain or deformation)
bottom: measurement of resulting force (shear stress)

sinusoidal preset

For ideally elastic behavior


of a totally stiff sample (e.g. a stone, or steel):
There is no time shift between the sine curves of
preset strain and resulting shear stress:
the curves of  and  are “in phase“  movie (2-plates-model, ideal elastic behavior) 37
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15 Oscillatory Tests

Preset: constant frequency and constant amplitude

Result: Most samples show


viscoelastic behavior with the
phase shift  between the sine curves of the
test preset (here: strain) and the measuring result (then: stress), as the
retardation of the measuring response compared to the preset.

 movie (2-plates-model, viscoelastic behavior) 38


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15 Oscillatory Tests
Vector diagram

G* complex shear modulus,


viscoelastic behavior in total.

G' storage modulus, elastic portion


G'' loss modulus, viscous portion
For scientists: of the viscoelastic behavior,
G' (G - prime) for the stored,
unit: Pa, for all G- values.
G'' (G - double prime) for the lost (dissipated)
deformation energy
due to internal friction when flowing left- hand side:
freely movable, unlinked molecules
right- hand side:
crosslinked molecules 39
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16 Amplitude Sweeps

Preset:

constant frequency
(e.g. angular frequency  = 10 rad/s)
and

variable strain (deformation)


strain sweep
or alternatively, with variable stress, as
stress sweep

Frequency Conversion:  = 2  f
with angular frequency  in rad /s (or in s-1) and frequency f in Hz
Please note: Hz is not an SI unit.
 movie (amplitude sweep) 40
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16 Amplitude Sweeps
limiting value
of the LVE- range

Result:
storage modulus G' (elastic behavior), loss modulus G'' (viscous behavior)
limiting value of the linear viscoelastic (LVE- ) range when reaching L
(linearity limit of strain), at the given test conditions, i.e., at the preset (angular) frequency

left hand side: G' > G'' (gel- like, solid structure) in the LVE- range
right hand side: G'' > G' (liquid, fluid structure) in the LVE- range 41
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16 Amplitude Sweeps

Polymer melt
liquid state
because G'' > G'
viscoelastic fluid

limit of the LVE range at


L = 10% = 0.1

ω = 10rad/s
T = +180°C

polymers 42
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16 Amplitude Sweeps

Sealant
in the LVE range
gel- like or pasty state
because G' > G''

Limit of the LVE- range at


L = 0.026% = 2.6  10-4

ω = 10rad/s
T = +25°C

dispersions, polymers 43
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16 Amplitude Sweeps

Dispersions
water- based

additive 1, gellant
e.g. clay (silicate)
yield stress y = 6.9Pa
flow stress f = 42Pa
additive 2, viscosifier
e.g. associative thickener
yield stress y = 1.5Pa

Summary, in the LVE range: but no flow stress !


with the gellant G' > G'' (gel- like state, solid),
with the viscosifier G'' > G' (liquid), hence no physical stability)
dispersions, coatings 44
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17 Frequency Sweeps

Preset:

constant amplitude
as shear strain within the LVE- range
(or alternatively, as shear stress)
and

variable frequency

Precondition: Firstly, the LVE- range has to be checked


by an amplitude sweep.

 movie (frequency sweep) 45


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17 Frequency Sweeps

PDMS
poly- di- methyl siloxane

typical behavior of
uncrosslinked polymers
showing a crossover point G' = G''

 = 10%
T = +23°C

uncrosslinked polymers 46
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17 Frequency Sweeps

Uncrosslinked polymers: analysis

average molar mass M

position of the crossover point G' = G''


depends on M (here: M1 > M2 )

relaxation time  = 1 / co

uncrosslinked polymers 47
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17 Frequency Sweeps

Polyethylene
melts, uncrosslinked polymers,
with a different molar mass
PE 1
PE 2

PE 1 has a higher average molar mass


since the crossover point G‘ = G‘‘
occurs at a lower frequency value

 = 10%
T = +180°C
uncrosslinked polymers 48
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17 Frequency Sweeps

Polyethylene
with functional groups
uncrosslinked
crosslinked

At low frequencies:
a higher G'- value indicates a higher
degree of crosslinking

 = 1%
T = +170°C

polymers 49
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17 Frequency Sweeps

Dispersions
water- based
long- term behavior,
sedimentation stability
at low frequencies
additive 1, gellant
e.g. clay (silicate)
G' > G'' hence gel- like solid,
stable
additive 2, viscosifier
e.g. an associative thickener
G'' > G' hence liquid,
unstable
dispersions, coatings 50
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18 Time- dependent Behavior (Oscillation)

Coatings: leveling and sagging

1 fast structure recovery 2 slow structure recovery


high wet- layer thickness, small wet- layer
good film stability thickness, good leveling

51
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18 Time- dependent Behavior (Oscillation)

Printing inks
structure recovery

requirements:
• fixing on the substrate
halftone printing
• dot sharpness
area printing
• sufficient leveling
Ref.: Teschner, H., Offsetdrucktechnik, Fachschriftenverlag, Fellbach

printink inks 52
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18 Time- dependent Behavior (Oscillation)
Structure recovery, step test,
3 intervals thixotropy test (3ITT),
here as an ORO Test:
Oscillation / Rotation / Oscillation
to determine “thixotropic behavior“
Preset
1 low- shear conditions (strain in the LVE- range, osc.)
2 high- shear conditions (rotation)
3 low- shear conditions (strain in the LVE- range, osc.)
Test result
1 state of rest
2 structure decomposition
3 structure regeneration
- in the 2nd interval: liquid
- in the 1st & 3rd interval: solid structure (at rest),
when reaching G' > G'' 53
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18 Time- dependent Behavior (Oscillation)

Dispersion

step test,
as an ORO test

 structure 1 = 3 = 1%
recovery ω = 10rad/s
ሶ = 100s-1
T = +23°C

dispersions 54
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18 Time- dependent Behavior (Oscillation)

Practical example:
Automotive coatings
electrostatically supported spray process,
using high- speed rotational atomizers

Ref.:
Problem with spray coatings: - Daimler- Museum
in Stuttgart, Germany;
sagging - Evonik

coatings 55
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18 Time- dependent Behavior (Oscillation)

Automotive spray coatings


ORO- Tests
AC1:
AC2:
AC3:

(a) as long as G'' > G'


liquid state, flowing, leveling, sagging
(b) when finally G' > G''
solid state, sagging is stopped

time point of crossover G' = G''


can be controlled using rheology additives:
sag control
coatings 56
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18 Time- dependent Behavior (Oscillation)
Gelation or curing processes
isothermal curing at constant dynamic- mechanical shear conditions
Preset:
- constant measuring temperature
- constant amplitude (strain or stress) in the LVE- region
- constant (angular) frequency (usually with ω = 10rad/s)

Result: time- dependent G' and G'' curves

tCR point in time at the start of gelation


or chemical reaction

tSG time when reaching the


crossover point G' = G'' or the point of
sol / gel transition
resins, powder coatings 57
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18 Time- dependent Behavior (Oscillation)

G', G''

104 10
Two- component adhesive
Pa
lg G' Pa

t-SWP Kleber 5
curing reaction
lg G'' PP25; [d=1 mm]

G' Storage Modulus


isothermal, at T = +23°C

G' G'' Loss Modulus

10310
G''
3

curing t-SWP Kleber 5 [tsg,Tsg]

t = 35.16 s; G' = 1360 Pa


crossover G' = G''
G' Storage Modulus

G'' Loss Modulus


after t = 35s
with G' = 1360Pa

MS PP 25, disposable measuring system


102
 = 0.1%
2
10
0 50 100 150 200 250 300 350 400 450 s 500
0 100 200 300
Time t 400 500
Anton Paar GmbH
s ω = 10rad/s
time t

adhesives, resins 58
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19 Temperature- dependent Behavior (Oscillation)

melting 
Polymer- modified bitumen
(PMB) with 5 w-% polymer
uncrosslinked, amorphous polymer

preset in 2 intervals, as the


G'- values are spreading over 7 decades
1) 1 = 0.1% (for T < 35°C)
2) 2 = 1% (for T > 35°C)

ω = 10 rad/s

polymers, bitumen 59
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19 Temperature- dependent Behavior (Oscillation)

melting 
Hotmelt adhesive
uncrosslinked,
partially crystalline polymer
with a pronounced rubber- elastic region

Tg = -18°C (G'' max)


Tg = 0°C (tan max)
finally as a melt, since
G'' > G' for T > Tm = +78°C
tan = G'' / G'

polymers, adhesives 60
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19 Temperature- dependent Behavior (Oscillation)

heating, softening 
Rubber
crosslinked polymer
Tg = -22°C (G'' max),
Tg = -16°C (tan max)
no melting, since G' > G''
also at high temperatures

 = 0.25%
ω = 10rad/s
tan = G'' / G'

elastomers, rubber 61
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19 Temperature-dependent Behavior (Oscillation)

4
10 48
°C
Pa 36 Handcream
G' 3
30 T emulsion
10 24
18 temperature
12 freeze-thaw
6 cycle test
2
10 0
0 10 20 30 40 50 60 70 80 90 100 min 120
Time t

62
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19 Temperature- dependent Behavior (Oscillation)

Gel formation or curing


when heating
Preset: constant shear conditions
(amplitude and frequency)
Result:
temperature- dependent functions
of G' and G''

Tm ... melting temperature (when G' = G'')


TCR ... onset of gel formation or curing (chemical reaction)
TSG ... sol /gel transition (when again G' = G'')

63
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19 Temperature- dependent Behavior (Oscillation)

softening  swelling  thickening  fusion  gelation


PVC plastisol
fusion and gelation process
from plastisol paste to elastomer

onset of gelation: T = +65°C


end of fusion: T = +96°C

 = 0.2%
ω = 10rad/s

dispersions  movies (plastisol fusion 1 & 2) 64


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20 Torsional Tests on Solid Specimens

Torsion bars

typical dimensions
of solid specimens

40 x 10 x 1 (in mm)

with 40mm
of the free length,
outside of the clamps

measuring system SRF (solid rectangular fixture),


for solid specimens, having a rectangular cross- section
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20 Torsional Tests on Solid Specimens

Laminates
DMTA
dynamic mechanical thermo- analysis

reinforced laminate
unmodified laminate

increase of G' from 3 GPa to 8 GPa


softening 
ω = 10rad/s
 = 0.01%
torsion bar (SRF)
50 x 10 x 1 (in mm)
polymers 66
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21 Tensile Tests
Measuring systems
SER - Sentmanat Extensional Rheology (rotation), and
UXF - Universal Extensional Fixture (rotation and oscillation)
for films, foils and fibers (e.g. 50µm thickness)
 movies
(sample preparation
& loading,
tensile & relaxation
tests of
adhesives, rubbers,
polymer melts & films;
in normal light
& polarized light)

Typical examples: Oscillation (DMA, DMTA):


Preset: extension (strain, deformation),
Rotation:
 (in %), & angular frequency (in s-1)
Preset: extensional rate ሶ (in s-1)
Result: extensional viscosity E (in Pas) Result: storage modulus E'
and loss modulus E'' (in Pa) 67
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21 Tensile Tests

measuring system UXF 12


Comparison of three coating films films: 19 x 10 x 0.044 (mm)
test program:
1) 30s pre- stress, T = +20°C, M = 0 to 1mNm
2) 30s pre- strain, T = +20°C,  = 0 to 1°
3) measurement:
a) rotation (ramp):  = 1000 kPa to 10 kPa
b) oscillation (superposed):
 = 400 kPa to 4 kPa, and  = 10 s-1
c) heating: T = +20 to 120°C, with 5K/min
Tg values via the E'' maximas
film 1 (blue): Tg= 57°C
film 2 (green): Tg= 69°C
film 3 (red): Tg= 76°C
coatings 68
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End of the Rheo- Seminar

Never
give up !

Have a
nice evening …

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