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Rheology Theory and Applications TAINSTRUMENTS.COMTAINSTRUMENTS.COM

Rheology Theory and Applications

Rheology Theory and Applications TAINSTRUMENTS.COMTAINSTRUMENTS.COM
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Course Outline

Course Outline Basics in Rheology Theory Oscillation TA Rheometers Linear Viscoelasticity Setting up Oscillation

Basics in Rheology Theory Oscillation

TA Rheometers

Linear Viscoelasticity Setting up Oscillation Tests

Transient Testing Applications of Rheology

Instrumentation Choosing a Geometry Calibrations

Flow Tests

Viscosity Setting up Flow Tests

Polymers Structured Fluids Advanced Accessories

Setting up Flow Tests Polymers Structured Fluids Advanced Accessories TAINSTRUMENTS.COMTAINSTRUMENTS.COM

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Basics in Rheology Theory

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Rheology: An Introduction

Rheology: The study of Rheology: The study of stress-deformation relationships stress-deformation relationships
Rheology: The study of
Rheology: The study of
stress-deformation relationships
stress-deformation relationships
The study of stress-deformation relationships stress-deformation relationships TAINSTRUMENTS.COMTAINSTRUMENTS.COM
The study of stress-deformation relationships stress-deformation relationships TAINSTRUMENTS.COMTAINSTRUMENTS.COM
The study of stress-deformation relationships stress-deformation relationships TAINSTRUMENTS.COMTAINSTRUMENTS.COM
The study of stress-deformation relationships stress-deformation relationships TAINSTRUMENTS.COMTAINSTRUMENTS.COM
The study of stress-deformation relationships stress-deformation relationships TAINSTRUMENTS.COMTAINSTRUMENTS.COM

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Rheology: An Introduction

Rheology: An Introduction Rheology is the science of flow and deformation of matter The word ‘Rheology’

Rheology is the science of flow and deformation of matter

The word ‘Rheology’ was coined in the 1920s by Professor E C Bingham at Lafayette College in Indiana

Flow is a special case of deformation The relationship between stress and deformation is a property of the material

= Viscosity
= Viscosity
= Modulus
= Modulus
between stress and deformation is a property of the material = Viscosity = Modulus TAINSTRUMENTS.COMTAINSTRUMENTS.COM

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Simple Steady Shear Flow

Simple Steady Shear Flow y Top plate Area = A x(t) y x F Shear Stress,

y

Top plate Area = A x(t) y x F Shear Stress, Pascals σ = A
Top plate Area = A
x(t)
y
x
F
Shear Stress, Pascals
σ =
A
x(t)
γ =
Shear Strain, %
η
=
y
γ
γ& =
Shear Rate, sec -1
t

Velocity = V 0 Force = F

Bottom Plate Velocity = 0

σ

&

γ

Viscosity, Pas

Velocity = V 0 Force = F Bottom Plate Velocity = 0 σ & γ Viscosity,

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Torsion Flow in Parallel Plates

Torsion Flow in Parallel Plates Ω r θ h r = plate radius h = distance
Ω r θ h
r
θ
h

r = plate radius h = distance between plates M = torque (µN.m) θ = Angular motor deflection (radians) = Motor angular velocity (rad/s)

Stress (σσσσ)

Strain (γγγγ)

= × M

=

× θθθθ

Strain rate ( ) =

× ΩΩΩΩ

Strain ( γγγγ ) = × M = × θθθθ Strain rate ( ) = ×

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TA Instruments Rheometers

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Rotational Rheometers at TA

Rotational Rheometers at TA ARES G2 Controlled Strain Dual Head SMT DHR Controlled Stress Single Head

ARES G2

Rotational Rheometers at TA ARES G2 Controlled Strain Dual Head SMT DHR Controlled Stress Single Head

Controlled Strain Dual Head

SMT

DHR

Rheometers at TA ARES G2 Controlled Strain Dual Head SMT DHR Controlled Stress Single Head CMT

Controlled Stress Single Head

CMT

at TA ARES G2 Controlled Strain Dual Head SMT DHR Controlled Stress Single Head CMT TAINSTRUMENTS.COMTAINSTRUMENTS.COM

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Rotational Rheometer Designs

Rotational Rheometer Designs Dual head or SMT Separate motor & transducer Measured Torque (Stress) Applied

Dual head or SMT Separate motor & transducer

Measured

Torque

(Stress)

Applied

Strain or

Rotation

Transducer
Transducer
(Stress) Applied Strain or Rotation Transducer Direct Drive Motor Sample Single head or CMT Combined motor
Direct Drive Motor
Direct Drive
Motor

Sample

Single head or CMT Combined motor & transducer

Displacement

Sensor

Non-Contact Drag Cup Motor Static Plate Static Plate
Non-Contact
Drag Cup
Motor
Static Plate
Static Plate

Measured Strain or Rotation

Applied

Torque

(Stress)

Note: With computer feedback, DHR and AR can work in controlled strain/shear rate, and ARES can work in controlled stress.

AR can work in controlled strain/shear rate, and ARES can work in controlled stress. TAINSTRUMENTS.COMTAINSTRUMENTS.COM

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What does a Rheometer do?

What does a Rheometer do? Rheometer – an instrument that measures both viscosity and viscoelasticity of

Rheometer – an instrument that measures both viscosity and viscoelasticity of fluids, semi-solids and solids

It can provide information about the material’s:

Viscosity - defined as a material’s resistance to deformation and

is a function of shear rate or stress, with time and temperature dependence

Viscoelasticity – is a property of a material that exhibits both viscous and elastic character. Measurements of G’, G”, tan δ with respect to time, temperature, frequency and stress/strain are important for characterization.

A Rheometer works simply by relating a materials property from how hard it’s being pushed, to how far it moves

by commanding torque (stress) and measuring angular displacement (strain) by commanding angular displacement (strain) and measuring torque (stress)

(strain) by commanding angular displacement (strain) and measuring torque (stress) TAINSTRUMENTS.COMTAINSTRUMENTS.COM

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How do Rheometers work?

How do Rheometers work? From the definition of rheology, the science of flow and deformation of

From the definition of rheology,

the science of flow and deformation of matter or the study of stress (Force / Area) – deformation (Strain or Strain rate) relationships.

Fundamentally a rotational rheometer will apply or measure:

1. Torque (Force) 2. Angular Displacement 3. Angular Velocity

will apply or measure: 1. Torque (Force) 2. Angular Displacement 3. Angular Velocity TAINSTRUMENTS.COMTAINSTRUMENTS.COM

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Torque

Shear Stress

Torque Shear Stress In a rheometer, the stress is calculated from the torque. The formula for

In a rheometer, the stress is calculated from the torque.

The formula for stress is: σ = Μ × K σ

Where

σ = Stress (Pa or Dyne/cm 2 )

 

Μ = torque in N . m or gm . cm K σ = Stress Constant

The stress constant, K σ , is a geometry dependent factor

= Stress Constant The stress constant, K σ , is a geometry dependent factor TAINSTRUMENTS.COMTAINSTRUMENTS.COM

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Angular Displacement Shear Strain

Angular Displacement Shear Strain In a SMT Rheometer, the angular displacement is directly applied by a

In a SMT Rheometer, the angular displacement is directly applied by a motor.

The formula for strain is:

%γ = γ × 100

γ = K γ × θ

where γ = Strain K γ = Strain Constant θ = Angular motor deflection (radians)

The strain constant, K γ , is a geometry dependent factor

deflection (radians) The strain constant, K γ , is a geometry dependent factor TAINSTRUMENTS.COMTAINSTRUMENTS.COM

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Equation for Modulus

Equation for Modulus G = Rheological Parameter σ γ Constitutive Equation = Describe In Spec Correctly
Equation for Modulus G = Rheological Parameter σ γ Constitutive Equation = Describe In Spec Correctly

G =

Rheological Parameter
Rheological
Parameter
σ γ Constitutive Equation
σ
γ
Constitutive
Equation

=

Describe In Spec Correctly M ⋅ K σ θ ⋅ K γ
Describe
In Spec
Correctly
M
⋅ K
σ
θ
⋅ K
γ
Raw rheometer Specifications
Raw rheometer
Specifications

Geometric

Shape

Constants

The equation of motion and other relationships have been used to determine the appropriate equations to convert machine parameters (torque, angular velocity, and angular displacement) to rheological parameters.

(torque, angular velocity, and angular displacement) to rheological parameters. TAINSTRUMENTS.COMTAINSTRUMENTS.COM

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Angular Velocity

Shear Rate

Angular Velocity Shear Rate In a SMT rheometer, the angular speed is directly controlled by the

In a SMT rheometer, the angular speed is directly controlled by the motor).

The formula for shear rate is:

= ×

where

= Shear rate

K γ = Strain Constant

= Motor angular velocity in rad/sec

The strain constant, K γ , is a geometry dependent factor

velocity in rad/sec The strain constant, K γ , is a geometry dependent factor TAINSTRUMENTS.COMTAINSTRUMENTS.COM

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Equation for Viscosity

Equation for Viscosity η = Rheological Parameter σ = γ & Constitutive Equation Describe In Spec
η
η

=

Rheological Parameter
Rheological
Parameter
σ = γ & Constitutive Equation
σ
=
γ
&
Constitutive
Equation
Describe In Spec Correctly M ⋅ K σ Ω⋅ K γ
Describe
In Spec
Correctly
M
⋅ K
σ
Ω⋅ K
γ
Raw rheometer Specifications
Raw rheometer
Specifications

Geometric

Shape

Constants

The equation of motion and other relationships have been used to determine the appropriate equations to convert machine parameters (torque, angular velocity, and angular displacement) to rheological parameters.

(torque, angular velocity, and angular displacement) to rheological parameters. TAINSTRUMENTS.COMTAINSTRUMENTS.COM

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Discovery Hybrid Rheometer Specifications

Discovery Hybrid Rheometer Specifications Specification HR-3 HR-2 HR-1 Bearing Type, Thrust Magnetic

Specification

HR-3

HR-2

HR-1

Bearing Type, Thrust

Magnetic

Magnetic

Magnetic

Bearing Type, Radial

Porous Carbon

Porous Carbon

Porous Carbon

Motor Design

Drag Cup

Drag Cup

Drag Cup

Minimum Torque (nN.m) Oscillation

0.5

2

10

Minimum Torque (nN.m) Steady Shear

5

10

20

Maximum Torque (mN.m)

200

200

150

Torque Resolution (nN.m)

0.05

0.1

0.1

Minimum Frequency (Hz)

1.0E-07

1.0E-07

1.0E-07

Maximum Frequency (Hz)

100

100

100

Minimum Angular Velocity (rad/s)

0

0

0

Maximum Angular Velocity (rad/s)

300

300

300

Displacement Transducer

Optical

Optical

Optical

encoder

encoder

encoder

Optical Encoder Dual Reader

Standard

N/A

N/A

Displacement Resolution (nrad)

2

10

10

Step Time, Strain (ms)

15

15

15

Step Time, Rate (ms)

5

5

5

Normal/Axial Force Transducer

FRT

FRT

FRT

Maximum Normal Force (N)

50

50

50

Normal Force Sensitivity (N)

0.005

0.005

0.01

Normal Force Resolution (mN)

0.5

0.5

1

HR-3

HR-2

HR-1

DHR - DMA mode (optional)

Motor Control

FRT

Minimum Force (N) Oscillation

0.1

Maximum Axial Force (N)

50

Minimum Displacement (µm) Oscillation

1.0

Maximum Displacement (µm) Oscillation

100

Displacement Resolution (nm)

10

Axial Frequency Range (Hz)

1 x 10 -5 to 16

Resolution (nm) 10 Axial Frequency Range (Hz) 1 x 10 - 5 to 16 TAINSTRUMENTS.COMTAINSTRUMENTS.COM

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ARES-G2 Rheometer Specifications

ARES-G2 Rheometer Specifications Force/Torque Rebalance Transducer (Sample Stress) Transducer Type Force/Torque

Force/Torque Rebalance Transducer (Sample Stress)

Transducer Type

Force/Torque

Rebalance

Transducer Torque Motor

Brushless DC

Transducer Normal/Axial Motor

Brushless DC

Minimum Torque (µN.m) Oscillation

0.05

Minimum Torque (µN.m) Steady Shear

0.1

Maximum Torque (mN.m)

200

Torque Resolution (nN.m)

1

Transducer Normal/Axial Force Range (N)

0.001 to 20

Transducer Bearing

Groove Compensated Air

Driver Motor (Sample

Deformation)

Maximum Motor Torque (mN.m)

800

Motor Design

Brushless DC

Motor Bearing

Jeweled Air, Sapphire

Displacement Control/ Sensing

Optical Encoder

Strain Resolution (µrad)

0.04

Minimum Angular Displacement (µrad) Oscillation

1

Maximum Angular Displacement (µrad) Steady Shear

Unlimited

Angular Velocity Range (rad/s)

1x 10 -6 to 300

Angular Frequency Range (rad/s)

1x 10 -7 to 628

Step Change, Velocity (ms)

5

Step Change, Strain (ms)

10

Velocity (ms) 5 Step Change, Strain (ms) 10 Orthogonal Superposition (OSP) and DMA modes Motor

Orthogonal Superposition (OSP) and DMA modes

Motor Control

FRT

Minimum Transducer Force (N) Oscillation

0.001

Maximum Transducer Force

20

(N)

Minimum Displacement (µm) Oscillation

0.5

Maximum Displacement (µm) Oscillation

50

Displacement Resolution (nm)

10

Axial Frequency Range (Hz)

1 x 10 -5 to 16

Resolution (nm) 10 Axial Frequency Range (Hz) 1 x 10 - 5 to 16 TAINSTRUMENTS.COMTAINSTRUMENTS.COM

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Geometry Options

Geometry Options Concentric Cylinders Cone and Plate Parallel Plate Very Low Very Low to Medium Viscosity

Concentric

Cylinders

Cone and Plate

Parallel

Plate

Very Low Very Low
Very Low
Very Low

to Medium

Viscosity

to High

Viscosity

Very Low Viscosity to Soft Solids

Torsion

Rectangular

Viscosity Very Low Viscosity to Soft Solids Torsion Rectangular Solids Water to Steel TAINSTRUMENTS.COMTAINSTRUMENTS.COM

Solids

Water

Viscosity Very Low Viscosity to Soft Solids Torsion Rectangular Solids Water to Steel TAINSTRUMENTS.COMTAINSTRUMENTS.COM

to

Viscosity Very Low Viscosity to Soft Solids Torsion Rectangular Solids Water to Steel TAINSTRUMENTS.COMTAINSTRUMENTS.COM

Steel

Viscosity Very Low Viscosity to Soft Solids Torsion Rectangular Solids Water to Steel TAINSTRUMENTS.COMTAINSTRUMENTS.COM

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Choosing a Geometry Size

Choosing a Geometry Size Assess the ‘viscosity’ of your sample When a variety of cones and
Choosing a Geometry Size Assess the ‘viscosity’ of your sample When a variety of cones and

Assess the ‘viscosity’ of your sample

When a variety of cones and plates are available, select diameter appropriate for viscosity of sample

Low viscosity (milk) - 60mm geometry Medium viscosity (honey) - 40mm geometry High viscosity (caramel) – 20 or 25mm geometry

Examine data in terms of absolute instrument variables torque/displacement/speed and modify geometry choice to move into optimum working range

You may need to reconsider your selection after the first run!

optimum working range You may need to reconsider your selection after the first run! TAINSTRUMENTS.COMTAINSTRUMENTS.COM

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Parallel Plate

Parallel Plate Diameter (2 ⋅⋅⋅⋅ r) Gap (h) Strain Constant: = (to convert angular velocity, rad/sec,
Parallel Plate Diameter (2 ⋅⋅⋅⋅ r) Gap (h) Strain Constant: = (to convert angular velocity, rad/sec,
Parallel Plate Diameter (2 ⋅⋅⋅⋅ r) Gap (h) Strain Constant: = (to convert angular velocity, rad/sec,

Diameter (2⋅⋅⋅⋅r)

Gap (h)

Strain Constant:

=

(to convert angular velocity, rad/sec, to shear rate, 1/sec, at the edge or angular displacement, radians, to shear strain (unitless) at the edge. The radius, r, and the gap, h, are expressed in meters)

Stress Constant:

=

(to convert torque, Nm, to shear stress at the edge, Pa, for Newtonian fluids. The radius, r, is expressed in meters)

stress at the edge, Pa, for Newtonian fluids. The radius, r, is expressed in meters) TAINSTRUMENTS.COMTAINSTRUMENTS.COM

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When to use Parallel Plates

When to use Parallel Plates Low/Medium/High Viscosity Liquids Soft Solids/Gels Thermosetting materials Samples

Low/Medium/High Viscosity Liquids Soft Solids/Gels Thermosetting materials Samples with large particles

Samples with long relaxation time Temperature Ramps/ Sweeps Materials that may slip

Crosshatched or Sandblasted plates

Small sample volume

Materials that may slip Crosshatched or Sandblasted plates Small sample volume TAINSTRUMENTS.COMTAINSTRUMENTS.COM
Materials that may slip Crosshatched or Sandblasted plates Small sample volume TAINSTRUMENTS.COMTAINSTRUMENTS.COM

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Plate Diameters

Plate Diameters Shear Stress 20 mm 40 mm 60 mm As diameter decreases, shear stress increases
Shear Stress 20 mm 40 mm 60 mm
Shear Stress
20 mm
40 mm
60 mm

As diameter decreases, shear stress increases

=

2

Shear Stress 20 mm 40 mm 60 mm As diameter decreases, shear stress increases = 2

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Plate Gaps

Plate Gaps Shear Rate 2 mm Increases 1 mm 0.5 mm As gap height decreases, shear
Shear Rate 2 mm Increases 1 mm 0.5 mm
Shear
Rate
2 mm
Increases
1 mm
0.5 mm

As gap height decreases, shear rate increases

2 mm Increases 1 mm 0.5 mm As gap height decreases, shear rate increases =Ω ℎ

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Effective Shear Rate varies across a Parallel Plate

Effective Shear Rate varies across a Parallel Plate For a given angle of deformation, there is

For a given angle of deformation, there is a greater arc of deformation at the edge of the plate than at the center

of deformation at the edge of the plate than at the center dx increases further from
dx increases further from the center,
dx increases further from the center,

=

h stays constant

plate than at the center dx increases further from the center, = ℎ h stays constant

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Shear Rate is Normalized across a Cone

Shear Rate is Normalized across a Cone The cone shape produces a smaller gap height closer

The cone shape produces a smaller gap height closer to inside, so the shear on the sample is constant

closer to inside, so the shear on the sample is constant = ℎ h increases proportionally

=

h increases proportionally to dx, γ is uniform

on the sample is constant = ℎ h increases proportionally to dx , γ is uniform

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Cone and Plate

Cone and Plate Diameter (2⋅⋅⋅⋅r) Truncation (gap) Strain Constant: = (to convert angular velocity, rad/sec, to
Cone and Plate Diameter (2⋅⋅⋅⋅r) Truncation (gap) Strain Constant: = (to convert angular velocity, rad/sec, to
Diameter (2⋅⋅⋅⋅r)
Diameter (2⋅⋅⋅⋅r)

Truncation (gap)

Strain Constant:

=

(to convert angular velocity, rad/sec, to shear rate. 1/sec, or angular displacement, radians, to shear strain, which is unit less. The angle, β, is expressed in radians)

Stress Constant:

=

(to convert torque, Nm, to shear stress, Pa. The radius, r, is expressed in meters)

convert torque, N ⋅ m, to shear stress, Pa. The radius, r, is expressed in meters)

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When to use Cone and Plate

When to use Cone and Plate Very Low to High Viscosity Liquids High Shear Rate measurements

Very Low to High Viscosity Liquids High Shear Rate measurements Normal Stress Growth Unfilled Samples Isothermal Tests Small Sample Volume

Normal Stress Growth Unfilled Samples Isothermal Tests Small Sample Volume TAINSTRUMENTS.COMTAINSTRUMENTS.COM
Normal Stress Growth Unfilled Samples Isothermal Tests Small Sample Volume TAINSTRUMENTS.COMTAINSTRUMENTS.COM

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Cone Diameters

Cone Diameters Shear Stress 20 mm 40 mm 60 mm As diameter decreases, shear stress increases
Shear Stress 20 mm 40 mm 60 mm
Shear Stress
20
mm
40
mm
60
mm

As diameter decreases, shear stress increases

=

3

2

Stress 20 mm 40 mm 60 mm As diameter decreases, shear stress increases = 3 2

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Cone Angles

Cone Angles Shear Rate Increases 2 ° 1 ° 0.5 ° As cone angle decreases, shear
Shear Rate Increases 2 ° 1 ° 0.5 °
Shear Rate
Increases
2 °
1 °
0.5 °

As cone angle decreases, shear rate increases

1

Rate Increases 2 ° 1 ° 0.5 ° As cone angle decreases, shear rate increases =Ω

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Limitations of Cone and Plate

Limitations of Cone and Plate Typical Truncation Heights: 1 ° degree ~ 20 - 30 microns
Limitations of Cone and Plate Typical Truncation Heights: 1 ° degree ~ 20 - 30 microns

Typical Truncation Heights:

1 ° degree ~ 20 - 30 microns 2 ° degrees ~ 60 microns 4 ° degrees ~ 120 microns

Truncation Height = Gap

Cone & Plate

Truncation Height = Gap C o n e & P l a t e Gap must

Gap must be > or = 10 [particle size]!!

= Gap C o n e & P l a t e Gap must be >

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Correct Sample Loading

Correct Sample Loading × × × Under Filled sample: Under Filled sample: Under Filled sample: Lower
× × × Under Filled sample: Under Filled sample: Under Filled sample: Lower torque contribution
×
×
×
Under Filled sample:
Under Filled sample:
Under Filled sample:
Lower torque contribution
Lower torque contribution
Lower torque contribution
×
×
×
Over Filled sample:
Over Filled sample:
Over Filled sample:
Additional stress from
Additional stress from
Additional stress from
drag along the edges
drag along the edges
drag along the edges
CorrectCorrect FillingFilling
Correct Filling
along the edges drag along the edges CorrectCorrect FillingFilling Correct Filling TAINSTRUMENTS.COMTAINSTRUMENTS.COM

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Concentric Cylinder

Concentric Cylinder Strain Constant: = 1 + 2 2 1 (to convert angular velocity, rad/sec, to
Concentric Cylinder Strain Constant: = 1 + 2 2 1 (to convert angular velocity, rad/sec, to

Strain Constant:

= 1 + 2 2 1

(to convert angular velocity, rad/sec, to shear rate, 1/sec, or angular displacement, radians, to shear strain (unit less). The radii, r 1 (inner) and r 2 (outer), are expressed in meters)

Stress Constant:

=

1 + 2

2 1

*

(to convert torque, Nm, to shear stress, Pa. The bob length, l, and the radius, r, are expressed in meters)

*Note including end correction factor. See TRIOS Help

r, are expressed in meters) *Note including end correction factor. See TRIOS Help TAINSTRUMENTS.COMTAINSTRUMENTS.COM

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Double Wall

Double Wall Use for very low viscosity systems (<1 mPas) Strain Constant: = 1 + 2

Use for very low viscosity systems (<1 mPas)

Double Wall Use for very low viscosity systems (<1 mPas) Strain Constant: = 1 + 2

Strain Constant:

= 1 + 2 2 1

Strain Constant: = 1 + 2 2 − 1 Stress Constant: r 1 r 2 h

Stress Constant:

r 1 r 2 h r 3 r 4 = ∙
r
1
r
2
h
r
3
r
4
=

ARES Gap Settings: standard operating gap DW = 3.4 mm narrow operating gap DW = 2.0 mm Use equation Gap > 3 × (R 2 –R 1 )

mm narrow operating gap DW = 2.0 mm Use equation Gap > 3 × (R 2

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When to Use Concentric Cylinders

When to Use Concentric Cylinders Low to Medium Viscosity Liquids Unstable Dispersions and Slurries Minimize Effects
When to Use Concentric Cylinders Low to Medium Viscosity Liquids Unstable Dispersions and Slurries Minimize Effects

Low to Medium Viscosity Liquids Unstable Dispersions and Slurries Minimize Effects of Evaporation Weakly Structured Samples (Vane) High Shear Rates

Minimize Effects of Evaporation Weakly Structured Samples (Vane) High Shear Rates TAINSTRUMENTS.COMTAINSTRUMENTS.COM

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Peltier Concentric Cylinders

Peltier Concentric Cylinders TAINSTRUMENTS.COMTAINSTRUMENTS.COM
Peltier Concentric Cylinders TAINSTRUMENTS.COMTAINSTRUMENTS.COM
Peltier Concentric Cylinders TAINSTRUMENTS.COMTAINSTRUMENTS.COM
Peltier Concentric Cylinders TAINSTRUMENTS.COMTAINSTRUMENTS.COM

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Torsion Rectangular

Torsion Rectangular = 1 − 0.378 = 3 + . ∙ Advantages: H igh modulus samples
Torsion Rectangular = 1 − 0.378 = 3 + . ∙ Advantages: H igh modulus samples

=

1 − 0.378

Torsion Rectangular = 1 − 0.378 = 3 + . ∙ Advantages: H igh modulus samples

=

3+ .

Advantages:

High modulus samples Small temperature gradient Simple to prepare

w = Width

l = Length

t

= Thickness

Disadvantages:

No pure Torsion mode for high strains

Torsion cylindrical also available

N o pure Torsion mode for high strains Torsion cylindrical also available TAINSTRUMENTS.COMTAINSTRUMENTS.COM

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Torsion and DMA Measurements

Torsion and DMA geometries allow solid samples to be characterized in a temperature controlled environment
Torsion and DMA geometries allow solid samples to be
characterized in a temperature controlled environment
Torsion measures G’, G”, and Tan δ
DMA measures E’, E”, and Tan δ
ARES G2 DMA is standard function (50 µm amplitude)
DMA is an optional DHR function (100 µm amplitude)
Rectangular and
cylindrical torsion
DMA 3-point bending and tension
(cantilever not shown)
and cylindrical torsion DMA 3-point bending and tension (cantilever not shown) TAINSTRUMENTS.COMTAINSTRUMENTS.COM
and cylindrical torsion DMA 3-point bending and tension (cantilever not shown) TAINSTRUMENTS.COMTAINSTRUMENTS.COM

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Geometry Overview

Geometry Overview Geometry Application Advantage Disadvantage Cone/plate fluids, melts viscosity >

Geometry

Application

Advantage

Disadvantage

Cone/plate

fluids, melts viscosity > 10mPas

true viscosities

temperature ramp difficult

Parallel Plate

fluids, melts viscosity > 10mPas

easy handling, temperature ramp

shear gradient across sample

Couette

low viscosity samples < 10 mPas

high shear rate

large sample volume

Double Wall Couette

very low viscosity samples < 1mPas

high shear rate

cleaning difficult

Torsion Rectangular

solid polymers,

glassy to rubbery state

Limited by sample stiffness

composites

DMA

Solid polymers, films, Composites

Glassy to rubbery state

Limited by sample stiffness (Oscillation and stress/strain)

Glassy to rubbery state Limited by sample stiffness (Oscillation and stress/strain) TAINSTRUMENTS.COMTAINSTRUMENTS.COM

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Rheometer Calibrations and Performance Verification

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DHR – Calibration Options

DHR – Calibration Options Instrument Calibrations   Inertia (Service) Rotational Mapping Geometry

Instrument Calibrations

 

Inertia (Service)

Rotational Mapping

Geometry Calibrations:

 

Inertia

Friction

Gap Temperature

Compensation Rotational Mapping

Details in Appendix #4

Gap Temperature Compensation Rotational Mapping Details in Appendix #4 TAINSTRUMENTS.COMTAINSTRUMENTS.COM
Gap Temperature Compensation Rotational Mapping Details in Appendix #4 TAINSTRUMENTS.COMTAINSTRUMENTS.COM

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ARES-G2 – Calibration Options

ARES-G2 – Calibration Options Instrument Calibrations Transducer Temperature Offsets Phase Angle (Service)

Instrument Calibrations

Transducer Temperature Offsets Phase Angle (Service) Measure Gap Temperature Compensation

Geometry Calibrations:

Compliance and Inertia (from table) Gap Temperature Compensation

Details in Appendix #4

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Verify Rheometer Performance

Verify Rheometer Performance Rheometers are calibrated from the factory and again at installation. TA recommends

Rheometers are calibrated from the factory and again at installation. TA recommends routine validation or confidence checks using standard oils or Polydimethylsiloxane (PDMS).

PDMS is verified using a 25 mm parallel plate.

Oscillation - Frequency Sweep: 1 to 100 rad/s with 5% strain at 30 ° C Verify modulus and frequency values at crossover

Standard silicone oils can be verified using cone, plate or concentric cylinder configurations.

Flow – Ramp: 0 to 88 Pa at 25 ° C using a 60 mm 2 ° cone

Service performs this test at installation

at 25 ° C using a 60 mm 2 ° cone Service performs this test at

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PDMS Frequency Sweep Results

PDMS Frequency Sweep Results TAINSTRUMENTS.COMTAINSTRUMENTS.COM
PDMS Frequency Sweep Results TAINSTRUMENTS.COMTAINSTRUMENTS.COM
PDMS Frequency Sweep Results TAINSTRUMENTS.COMTAINSTRUMENTS.COM

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Load Standard Oil

Set Peltier temperature to 25°C and equilibrate. Zero the geometry gap Load sample Be careful
Set Peltier temperature to 25°C and
equilibrate.
Zero the geometry gap
Load sample
Be careful not to introduce air bubbles!
Set the gap to the trim gap
Lock the head and trim with non-absorbent
tool
Important to allow time for temperature equilibration.
Go to geometry gap and initiate the
experiment.
time for temperature equilibration. Go to geometry gap and initiate the experiment. TAINSTRUMENTS.COMTAINSTRUMENTS.COM

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Flow Ramp – Standard Oil (Service Test)

Flow Ramp – Standard Oil (Service Test) TAINSTRUMENTS.COMTAINSTRUMENTS.COM
Flow Ramp – Standard Oil (Service Test) TAINSTRUMENTS.COMTAINSTRUMENTS.COM
Flow Ramp – Standard Oil (Service Test) TAINSTRUMENTS.COMTAINSTRUMENTS.COM

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Setting up Rheological Experiments Flow Tests

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Viscosity: Definition

Viscosity: Definition Viscosity is… “lack of slipperiness” synonymous with internal friction resistance to

Viscosity is…

“lack of slipperiness”

synonymous with internal friction

resistance to flow

The Units of Viscosity are …

SI unit is the Pascal . second (Pa . s) cgs unit is the Poise 10 Poise = 1 Pa . s 1 cP (centipoise) = 1 mPa . s (millipascal second)

. second (Pa . s) cgs unit is the Poise 10 Poise = 1 Pa .
. second (Pa . s) cgs unit is the Poise 10 Poise = 1 Pa .
Poise 10 Poise = 1 Pa . s 1 cP (centipoise) = 1 mPa . s

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Equation for Viscosity

Equation for Viscosity η = Rheological Parameter σ γ & Constitutive Equation Describe In Spec Correctly
η
η

=

Rheological Parameter
Rheological
Parameter
σ γ & Constitutive Equation
σ
γ
&
Constitutive
Equation
Describe In Spec Correctly M ⋅ K σ = Ω⋅ K γ Geometric Raw rheometer
Describe
In Spec
Correctly
M
⋅ K
σ
=
Ω⋅ K
γ
Geometric
Raw rheometer
Specifications
Shape
Constants
⋅ K σ = Ω⋅ K γ Geometric Raw rheometer Specifications Shape Constants TAINSTRUMENTS.COMTAINSTRUMENTS.COM

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Typical Viscosity Values (Pa-s)

Typical Viscosity Values (Pa-s) Asphalt Binder -------------- Polymer Melt ---------------- Molasses

Asphalt Binder -------------- Polymer Melt ---------------- Molasses --------------------- Liquid Honey ---------------- Glycerol ---------------------- Olive Oil ---------------------- Water ------------------------- Air -----------------------------

100,000

 

1,000

100

10

Need for

1

Log scale

0.01

0.001

0.00001

1,000 100 10 Need for 1 Log scale 0.01 0.001 0.00001 TAINSTRUMENTS.COMTAINSTRUMENTS.COM

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Newtonian and Non-Newtonian Fluids

Newtonian and Non-Newtonian Fluids Newtonian Fluids - constant proportionality between shear stress and shear-rate

Newtonian Fluids - constant proportionality between shear stress and shear-rate

Non-Newtonian Fluids - Viscosity is time or shear rate dependent

Time:

 

At constant shear-rate, if viscosity

Decreases with time – Thixotropy

Increases with time - Rheopexy

Shear-rate:

 

Shear - thinning

Shear - thickening

with time - Rheopexy Shear-rate:   Shear - thinning Shear - thickening TAINSTRUMENTS.COMTAINSTRUMENTS.COM

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Characteristic Diagrams for Newtonian Fluids

Characteristic Diagrams for Newtonian Fluids Ideal Yield Stress (Bingham Yield) γ ,1/s σ, Pa γ ,1/s
Ideal Yield Stress (Bingham Yield) γ ,1/s σ, Pa
Ideal Yield Stress
(Bingham Yield)
γ ,1/s
σ, Pa
γ ,1/s or σ, Pa η, Pa.s
γ ,1/s or σ, Pa
η, Pa.s
Fluids Ideal Yield Stress (Bingham Yield) γ ,1/s σ, Pa γ ,1/s or σ, Pa η,

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Characteristic Diagrams for Shear Thinning Fluids

Characteristic Diagrams for Shear Thinning Fluids 10 5 10 3 10 1 10 -1 10 -6
10 5 10 3 10 1 10 -1 10 -6 10 -4 10 -2 10
10
5
10
3
10
1
10
-1
10 -6
10 -4
10 -2 10 0
10 2
10 4
,1/s
η, Pa.s
10 5 Ideal Yield Stress 10 3 (Bingham plastic) 10 1 10 -1 10 -6
10
5
Ideal Yield Stress
10
3
(Bingham plastic)
10
1
10
-1
10 -6
10 -4
10 -2 10 0
10 2
10 4
γ ,1/s
σ, Pa
10 5 10 3 10 1 10 -1 10 -1 10 -0 10 -1 10
10
5
10
3
10
1
10
-1
10 -1
10 -0
10 -1
10 2
10 3
σ, Pa
η, Pa.s

Another name for a shear thinning fluid is a pseudo-plastic

2 10 3 σ, Pa η, Pa.s Another name for a shear thinning fluid is a

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Characteristic Diagrams for Shear Thickening Fluids

Characteristic Diagrams for Shear Thickening Fluids Log , 1/s Log η, Pa.s Dilatant material resists deformation
Log , 1/s Log η, Pa.s
Log , 1/s
Log η, Pa.s

Dilatant material resists deformation more than in proportion to the applied force (shear-thickening)

Cornstarch in water or sand on the beach are actually dilatant fluids, since they do not show the time- dependent, shear-induced change required in order to be labeled rheopectic

the time- dependent, shear-induced change required in order to be labeled rheopectic TAINSTRUMENTS.COMTAINSTRUMENTS.COM

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Non-Newtonian, Time Dependent Fluids

Non-Newtonian, Time Dependent Fluids Rheopectic Shear Rate = Constant Thixotropic time Viscosity Rheopectic materials
Rheopectic Shear Rate = Constant Thixotropic time Viscosity
Rheopectic
Shear Rate = Constant
Thixotropic
time
Viscosity

Rheopectic materials become more viscous with increasing time of applied force Higher concentration latex dispersions and plastisol paste materials exhibit rheopectic behavior Thixotropic materials become more fluid with increasing time of applied force Coatings and inks can display thixotropy when sheared due to structure breakdown

with increasing time of applied force Coatings and inks can display thixotropy when sheared due to
with increasing time of applied force Coatings and inks can display thixotropy when sheared due to
with increasing time of applied force Coatings and inks can display thixotropy when sheared due to
force Coatings and inks can display thixotropy when sheared due to structure breakdown TAINSTRUMENTS.COMTAINSTRUMENTS.COM

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Flow Experiments

Flow Experiments Flow Experiments Constant shear rate/stress (or Peak hold) Continuous stress/rate ramp and down

Flow Experiments

Constant shear rate/stress (or Peak hold) Continuous stress/rate ramp and down Stepped flow (or Flow sweep) Steady state flow Flow temperature ramp

and down Stepped flow (or Flow sweep) Steady state flow Flow temperature ramp TAINSTRUMENTS.COMTAINSTRUMENTS.COM
and down Stepped flow (or Flow sweep) Steady state flow Flow temperature ramp TAINSTRUMENTS.COMTAINSTRUMENTS.COM
and down Stepped flow (or Flow sweep) Steady state flow Flow temperature ramp TAINSTRUMENTS.COMTAINSTRUMENTS.COM

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Constant Shear Rate/Stress

Constant Shear Rate/Stress Stress /Rate Constant rate vs. time Constant stress vs. time USES Single point
Stress /Rate
Stress /Rate
Constant Shear Rate/Stress Stress /Rate Constant rate vs. time Constant stress vs. time USES Single point
Constant Shear Rate/Stress Stress /Rate Constant rate vs. time Constant stress vs. time USES Single point

Constant rate vs. time

Constant stress vs. time

USES Single point testing Scope the time for steady state under certain rate

vs. time USES Single point testing Scope the time for steady state under certain rate TAINSTRUMENTS.COMTAINSTRUMENTS.COM

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Constant Shear Rate/Stress

Constant Shear Rate/Stress viscosity (Pa.s) 3.500 4.000 Hand Wash Rate 1/s 3.500 3.000 3.000 2.500 2.500
viscosity (Pa.s) 3.500 4.000 Hand Wash Rate 1/s 3.500 3.000 3.000 2.500 2.500 2.000 2.000
viscosity (Pa.s)
3.500
4.000
Hand Wash Rate 1/s
3.500
3.000
3.000
2.500
2.500
2.000
2.000
1.500
Viscosity at 1 1/s is 2.8 Pa⋅s
1.500
1.000
1.000
0.5000
0.5000
0
0
shear stress (Pa)

0

5.0000

10.000

15.000

20.000

25.000

30.000

 

time (s)

(Pa) 0 5.0000 10.000 15.000 20.000 25.000 30.000   time (s) TAINSTRUMENTS.COMTAINSTRUMENTS.COM

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Continuous Ramp

Continuous Ramp Deformation m =Stress rate (Pa/min) time (min) Stress is applied to material at a
Continuous Ramp Deformation m =Stress rate (Pa/min) time (min) Stress is applied to material at a

Deformation

m =Stress rate (Pa/min)
m =Stress rate
(Pa/min)

time (min)

Stress is applied to material at a constant rate. Resultant strain is monitored with time.

USES Yield stress Scouting Viscosity Run

Resultant strain is monitored with time. USES Yield stress Scouting Viscosity Run TAINSTRUMENTS.COMTAINSTRUMENTS.COM

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Stress Ramp: Flow Media Dispersion

Stress Ramp: Flow Media Dispersion TAINSTRUMENTS.COMTAINSTRUMENTS.COM
Stress Ramp: Flow Media Dispersion TAINSTRUMENTS.COMTAINSTRUMENTS.COM
Stress Ramp: Flow Media Dispersion TAINSTRUMENTS.COMTAINSTRUMENTS.COM

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Thixotropic Loop - Continuous Ramp Up and Down

Thixotropic Loop - Continuous Ramp Up and Down σσσσ Deformation time Stress is first increased, then

σσσσ

Deformation

Loop - Continuous Ramp Up and Down σσσσ Deformation time Stress is first increased, then decreased,

time

Stress is first increased, then decreased, at a constant rate. Resultant strain is monitored with time.

USES “Pseudo-thixotropy” from Hysteresis loop

strain is monitored with time. USES “Pseudo-thixotropy” from Hysteresis loop TAINSTRUMENTS.COMTAINSTRUMENTS.COM

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Up & Down Flow Curves - 2 Repeats

Up & Down Flow Curves - 2 Repeats Run in Stress Control TA Instruments 500.0 400.0

Run in Stress Control

TA Instruments

500.0 400.0 300.0 Red: First cycle Blue: Second cycle 200.0 100.0 FORDB3.04F-Up step FORDB3.04F-Down step
500.0
400.0
300.0
Red: First cycle
Blue: Second cycle
200.0
100.0
FORDB3.04F-Up step
FORDB3.04F-Down step
FORDB3.05F-Up step
FORDB3.05F-Down step
0
0
0.1000
0.2000
0.3000
0.4000
0.5000
shear stress (Pa)

shear rate (1/s)

step 0 0 0.1000 0.2000 0.3000 0.4000 0.5000 shear stress (Pa) shear rate (1/s) TAINSTRUMENTS.COMTAINSTRUMENTS.COM

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Stepped or Steady-State Flow

Stepped or Steady-State Flow σ or σ or Deformation Data point saved time Delay time γ

σ

or

σ

or

Deformation

or Steady-State Flow σ or σ or Deformation Data point saved time Delay time γ or
Data point saved time
Data point saved
time

Delay time

Delay time
Delay time
Delay time
Delay time
Delay time
Delay time
Delay time
Delay time
Delay time

γ or σ = Constant

Steady State Flow

time

Stress is applied to sample. Viscosity measurement is taken when material has reached steady state flow. The stress is increased(logarithmically) and the process is repeated yielding a viscosity flow curve.

USES

Viscosity Flow Curves Yield Stress Measurements

Viscosity Flow Curves Yield Stress Measurements
yielding a viscosity flow curve. USES Viscosity Flow Curves Yield Stress Measurements TAINSTRUMENTS.COMTAINSTRUMENTS.COM

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Stepped or Steady-State Flow

Stepped or Steady-State Flow A series of logarithmic stress steps allowed to reach steady state, each

A series of logarithmic stress steps allowed to reach steady state, each one giving a single viscosity data point:

Data at each Shear Rate

a single viscosity data point: Data at each Shear Rate Shear Thinning Region Viscosity Time Shear
Shear Thinning Region Viscosity
Shear
Thinning
Region
Viscosity
Time
Time

Shear Rate, 1/s

η = σ /(dγ/dt)

Shear Rate Shear Thinning Region Viscosity Time Shear Rate, 1/s η = σ / (d γ/

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DHR and ARES G2: Steady State Flow

DHR and ARES G2: Steady State Flow Control variables: Shear rate Velocity Torque Shear stress Steady
DHR and ARES G2: Steady State Flow Control variables: Shear rate Velocity Torque Shear stress Steady

Control variables:

Shear rate Velocity Torque Shear stress

Shear rate Velocity Torque Shear stress
Shear rate Velocity Torque Shear stress
Shear rate Velocity Torque Shear stress

Steady state algorithm

Flow Control variables: Shear rate Velocity Torque Shear stress Steady state algorithm TAINSTRUMENTS.COMTAINSTRUMENTS.COM

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Flow Sweeps- Water-Based Paint with Solvent Trap

Flow Sweeps- Water-Based Paint with Solvent Trap TAINSTRUMENTS.COMTAINSTRUMENTS.COM
Flow Sweeps- Water-Based Paint with Solvent Trap TAINSTRUMENTS.COMTAINSTRUMENTS.COM
Flow Sweeps- Water-Based Paint with Solvent Trap TAINSTRUMENTS.COMTAINSTRUMENTS.COM

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Comparison of Cough Syrups

Comparison of Cough Syrups 0.8000 Sample 1-Flow step Sample 2-Flow step 0.7000 0.6000 Which material would
0.8000 Sample 1-Flow step Sample 2-Flow step 0.7000 0.6000 Which material would do a better
0.8000
Sample 1-Flow step
Sample 2-Flow step
0.7000
0.6000
Which material would do a better job
coating your throat?
0.5000
0.4000
0.3000
0.2000
0.1000
0
0.1000
1.000
10.00
100.0
1000
viscosity (Pa.s)

shear rate (1/s)

0.2000 0.1000 0 0.1000 1.000 10.00 100.0 1000 viscosity (Pa.s) shear rate (1/s) TAINSTRUMENTS.COMTAINSTRUMENTS.COM

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Comparison of Two Latex Paints

Comparison of Two Latex Paints 10000 A.01F-Flow step B.01F-Flow step Low shear rates B>A 1000 100.0
10000 A.01F-Flow step B.01F-Flow step Low shear rates B>A 1000 100.0 10.00 Medium shear rates
10000
A.01F-Flow step
B.01F-Flow step
Low shear rates B>A
1000
100.0
10.00
Medium shear rates A>B
1.000
High shear rates B>A
0.1000
1.000E-4
1.000E-3
0.01000
0.1000
1.000
10.00
100.0
1000
viscosity (Pa.s)

shear rate (1/s)

1.000E-3 0.01000 0.1000 1.000 10.00 100.0 1000 viscosity (Pa.s) shear rate (1/s) TAINSTRUMENTS.COMTAINSTRUMENTS.COM
1.000E-3 0.01000 0.1000 1.000 10.00 100.0 1000 viscosity (Pa.s) shear rate (1/s) TAINSTRUMENTS.COMTAINSTRUMENTS.COM

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Flow Temperature Ramp

Flow Temperature Ramp X X X X time (min) Hold the rate or stress constant whilst
Flow Temperature Ramp X X X X time (min) Hold the rate or stress constant whilst
X X X X time (min)
X
X
X
X
time (min)
Flow Temperature Ramp X X X X time (min) Hold the rate or stress constant whilst

Hold the rate or stress constant whilst ramping the temperature.

USES Measure the viscosity change vs. temperature

whilst ramping the temperature. USES Measure the viscosity change vs. temperature TAINSTRUMENTS.COMTAINSTRUMENTS.COM

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Viscosity: Temperature Dependence

Viscosity: Temperature Dependence Notice a nearly 2 decade decrease in viscosity. thermal equilibration of the sample
Viscosity: Temperature Dependence Notice a nearly 2 decade decrease in viscosity. thermal equilibration of the sample

Notice a nearly 2 decade decrease in viscosity.

thermal equilibration of the sample prior to testing. i.e. Conditioning Step or equilibration time for 3 to 5 min

This displays the importance of

Conditioning Step or equilibration time for 3 to 5 min This displays the importance of TAINSTRUMENTS.COMTAINSTRUMENTS.COM

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Flow Testing Considerations

Flow Testing Considerations Small gaps give high shear rates Be careful with small gaps: Gap errors

Small gaps give high shear rates

Be careful with small gaps:

Gap errors (gap temperature compensation) and shear heating can cause large errors in data. Recommended gap is between 0.5 to 2.0 mm. Secondary flows can cause increase in viscosity curve

Be careful with data interpretation at low shear rates

Surface tension can affect measured viscosity, especially with aqueous materials

rates Surface tension can affect measured viscosity, especially with aqueous materials TAINSTRUMENTS.COMTAINSTRUMENTS.COM

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Water at 25°C – Secondary Flow

Surface tension at low torques Secondary flows at high shear rates
Surface tension at low torques
Secondary flows at high shear rates
– Secondary Flow Surface tension at low torques Secondary flows at high shear rates TAINSTRUMENTS.COMTAINSTRUMENTS.COM

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Wall Slip

Wall Slip Wall slip can manifest as “apparent double yielding” Can be tested by running the
Wall Slip Wall slip can manifest as “apparent double yielding” Can be tested by running the
Wall Slip Wall slip can manifest as “apparent double yielding” Can be tested by running the
Wall Slip Wall slip can manifest as “apparent double yielding” Can be tested by running the

Wall slip can manifest as “apparent double yielding” Can be tested by running the same test at different gaps For samples that don’t slip, the results will be independent of the gap

gaps For samples that don’t slip, the results will be independent of the gap TAINSTRUMENTS.COMTAINSTRUMENTS.COM

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Shear Thinning or Sample Instability?

When Stress Decreases with Shear Rate, it indicates that sample is leaving the gap TAINSTRUMENTS.COMTAINSTRUMENTS.COM
When Stress Decreases with
Shear Rate, it indicates that
sample is leaving the gap
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Flow Testing Considerations

Flow Testing Considerations Edge Failure – Sample leaves gap because of normal forces Look at stress

Edge Failure – Sample leaves gap because of normal forces

Look at stress vs. shear rate curve – stress should not decrease with increasing shear rate – this indicates sample is leaving gap

Possible Solutions:

use a smaller gap or smaller angle so that you get the same shear rate at a lower angular velocity if appropriate (i.e. Polymer melts) make use of Cox Merz Rule

η(γ )

&

η

*

(ω)

(i.e. Polymer melts) make use of Cox Merz Rule η ( γ ) & ≡ η

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Viscoelasticity

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Elastic Behavior of an Ideal Solid

Hooke’s Law of Elasticity: Stress = Modulus ⋅ Strain γ 1 γ 2 γ 3
Hooke’s Law of Elasticity: Stress = Modulus ⋅ Strain
γ 1
γ 2
γ 3
3
E
2
1
Stress (σ)

1

2

Strain (ɣ)

3

= Modulus ⋅ Strain γ 1 γ 2 γ 3 3 E 2 1 Stress (σ)

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Elastic Behavior of an Ideal Solid Hooke’s Law of Elasticity: Stress = Modulus ⋅ Strain
Elastic Behavior of an Ideal Solid
Hooke’s Law of Elasticity: Stress = Modulus ⋅ Strain
E
>
E
>
E

=

Elasticity: Stress = Modulus ⋅ Strain E > E > E = γ 1 γ 2

γ 1

Elasticity: Stress = Modulus ⋅ Strain E > E > E = γ 1 γ 2

γ 2

Elasticity: Stress = Modulus ⋅ Strain E > E > E = γ 1 γ 2
Elasticity: Stress = Modulus ⋅ Strain E > E > E = γ 1 γ 2

γ 3

Elasticity: Stress = Modulus ⋅ Strain E > E > E = γ 1 γ 2

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Viscous Behavior of an Ideal Liquid

Viscous Behavior of an Ideal Liquid Newton’s Law: stress = coefficient of viscosity ⋅ shear rate
Newton’s Law: stress = coefficient of viscosity ⋅ shear rate η =η ∙ Shear Rate
Newton’s Law: stress
= coefficient of viscosity ⋅ shear rate
η
=η ∙
Shear Rate (ɣ)
Stress (σ)
= coefficient of viscosity ⋅ shear rate η =η ∙ Shear Rate (ɣ) Stress (σ) TAINSTRUMENTS.COMTAINSTRUMENTS.COM

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Viscous Behavior of an Ideal Liquid

Viscous Behavior of an Ideal Liquid Newton’s Law: stress= coefficient of viscosity ⋅ shear rate η

Newton’s Law: stress= coefficient of viscosity shear rate

η

<

η

<

η=

η

Law: stress= coefficient of viscosity ⋅ shear rate η < η < η= η TAINSTRUMENTS.COMTAINSTRUMENTS.COM
Law: stress= coefficient of viscosity ⋅ shear rate η < η < η= η TAINSTRUMENTS.COMTAINSTRUMENTS.COM
Law: stress= coefficient of viscosity ⋅ shear rate η < η < η= η TAINSTRUMENTS.COMTAINSTRUMENTS.COM
Law: stress= coefficient of viscosity ⋅ shear rate η < η < η= η TAINSTRUMENTS.COMTAINSTRUMENTS.COM
Law: stress= coefficient of viscosity ⋅ shear rate η < η < η= η TAINSTRUMENTS.COMTAINSTRUMENTS.COM
Law: stress= coefficient of viscosity ⋅ shear rate η < η < η= η TAINSTRUMENTS.COMTAINSTRUMENTS.COM
Law: stress= coefficient of viscosity ⋅ shear rate η < η < η= η TAINSTRUMENTS.COMTAINSTRUMENTS.COM
Law: stress= coefficient of viscosity ⋅ shear rate η < η < η= η TAINSTRUMENTS.COMTAINSTRUMENTS.COM
Law: stress= coefficient of viscosity ⋅ shear rate η < η < η= η TAINSTRUMENTS.COMTAINSTRUMENTS.COM
Law: stress= coefficient of viscosity ⋅ shear rate η < η < η= η TAINSTRUMENTS.COMTAINSTRUMENTS.COM
Law: stress= coefficient of viscosity ⋅ shear rate η < η < η= η TAINSTRUMENTS.COMTAINSTRUMENTS.COM
Law: stress= coefficient of viscosity ⋅ shear rate η < η < η= η TAINSTRUMENTS.COMTAINSTRUMENTS.COM
Law: stress= coefficient of viscosity ⋅ shear rate η < η < η= η TAINSTRUMENTS.COMTAINSTRUMENTS.COM
Law: stress= coefficient of viscosity ⋅ shear rate η < η < η= η TAINSTRUMENTS.COMTAINSTRUMENTS.COM
Law: stress= coefficient of viscosity ⋅ shear rate η < η < η= η TAINSTRUMENTS.COMTAINSTRUMENTS.COM
Law: stress= coefficient of viscosity ⋅ shear rate η < η < η= η TAINSTRUMENTS.COMTAINSTRUMENTS.COM
Law: stress= coefficient of viscosity ⋅ shear rate η < η < η= η TAINSTRUMENTS.COMTAINSTRUMENTS.COM
Law: stress= coefficient of viscosity ⋅ shear rate η < η < η= η TAINSTRUMENTS.COMTAINSTRUMENTS.COM
Law: stress= coefficient of viscosity ⋅ shear rate η < η < η= η TAINSTRUMENTS.COMTAINSTRUMENTS.COM
Law: stress= coefficient of viscosity ⋅ shear rate η < η < η= η TAINSTRUMENTS.COMTAINSTRUMENTS.COM
Law: stress= coefficient of viscosity ⋅ shear rate η < η < η= η TAINSTRUMENTS.COMTAINSTRUMENTS.COM
Law: stress= coefficient of viscosity ⋅ shear rate η < η < η= η TAINSTRUMENTS.COMTAINSTRUMENTS.COM
Law: stress= coefficient of viscosity ⋅ shear rate η < η < η= η TAINSTRUMENTS.COMTAINSTRUMENTS.COM
Law: stress= coefficient of viscosity ⋅ shear rate η < η < η= η TAINSTRUMENTS.COMTAINSTRUMENTS.COM
Law: stress= coefficient of viscosity ⋅ shear rate η < η < η= η TAINSTRUMENTS.COMTAINSTRUMENTS.COM
Law: stress= coefficient of viscosity ⋅ shear rate η < η < η= η TAINSTRUMENTS.COMTAINSTRUMENTS.COM
Law: stress= coefficient of viscosity ⋅ shear rate η < η < η= η TAINSTRUMENTS.COMTAINSTRUMENTS.COM

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Viscoelastic Behavior

σ = E*ε + η*dε/dt Kelvin-Voigt Model (Creep) Maxwell Model (Stress Relaxation) L 1 L
σ = E*ε + η*dε/dt
Kelvin-Voigt Model (Creep)
Maxwell Model (Stress Relaxation)
L
1
L
2

Viscoelastic Materials: Force depends on both Deformation and Rate of Deformation and vice versa.

Relaxation) L 1 L 2 Viscoelastic Materials: Force depends on both Deformation and Rate of Deformation
Relaxation) L 1 L 2 Viscoelastic Materials: Force depends on both Deformation and Rate of Deformation
Relaxation) L 1 L 2 Viscoelastic Materials: Force depends on both Deformation and Rate of Deformation

Viscoelasticity Defined

Viscoelasticity Defined Range of Material Behavior Liquid Like ---------- Solid Like Ideal Fluid ----- Most Materials

Range of Material Behavior Liquid Like---------- Solid Like Ideal Fluid ----- Most Materials -----Ideal Solid Purely Viscous ----- Viscoelastic ----- Purely Elastic

Viscoelasticity: Having both viscous and elastic properties

Materials behave in the linear manner, as described by Hooke and Newton, only on a small scale in stress or deformation.

as described by Hooke and Newton, only on a small scale in stress or deformation. TAINSTRUMENTS.COMTAINSTRUMENTS.COM

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Pitch Drop Experiment

Pitch Drop Experiment Long deformation time: pitch behaves like a highly viscous liquid 9 t h
Pitch Drop Experiment Long deformation time: pitch behaves like a highly viscous liquid 9 t h

Long deformation time: pitch behaves like a highly viscous liquid

9 th drop fell July 2013

Short deformation time: pitch behaves like a solid

July 2013 Short deformation time: pitch behaves like a solid Started in 1927 by Thomas Parnell

Started in 1927 by Thomas Parnell in Queensland, Australia

http://www.theatlantic.com/technology/archive/2013/07/the-3-most-exciting-words-in-science-right-now-the-pitch-dropped/277919/

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Time-Dependent Viscoelastic Behavior

Time-Dependent Viscoelastic Behavior T is short [< 1s] T is long [24 hours] TAINSTRUMENTS.COMTAINSTRUMENTS.COM
Time-Dependent Viscoelastic Behavior T is short [< 1s] T is long [24 hours] TAINSTRUMENTS.COMTAINSTRUMENTS.COM
Time-Dependent Viscoelastic Behavior T is short [< 1s] T is long [24 hours] TAINSTRUMENTS.COMTAINSTRUMENTS.COM
Time-Dependent Viscoelastic Behavior T is short [< 1s] T is long [24 hours] TAINSTRUMENTS.COMTAINSTRUMENTS.COM
Time-Dependent Viscoelastic Behavior T is short [< 1s] T is long [24 hours] TAINSTRUMENTS.COMTAINSTRUMENTS.COM
Time-Dependent Viscoelastic Behavior T is short [< 1s] T is long [24 hours] TAINSTRUMENTS.COMTAINSTRUMENTS.COM
Time-Dependent Viscoelastic Behavior T is short [< 1s] T is long [24 hours] TAINSTRUMENTS.COMTAINSTRUMENTS.COM

T is short [< 1s]

Time-Dependent Viscoelastic Behavior T is short [< 1s] T is long [24 hours] TAINSTRUMENTS.COMTAINSTRUMENTS.COM
Time-Dependent Viscoelastic Behavior T is short [< 1s] T is long [24 hours] TAINSTRUMENTS.COMTAINSTRUMENTS.COM
Time-Dependent Viscoelastic Behavior T is short [< 1s] T is long [24 hours] TAINSTRUMENTS.COMTAINSTRUMENTS.COM
Time-Dependent Viscoelastic Behavior T is short [< 1s] T is long [24 hours] TAINSTRUMENTS.COMTAINSTRUMENTS.COM

T is long [24 hours]

Time-Dependent Viscoelastic Behavior T is short [< 1s] T is long [24 hours] TAINSTRUMENTS.COMTAINSTRUMENTS.COM

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Time-Dependent Viscoelastic Behavior

Time-Dependent Viscoelastic Behavior Silly Putties have different characteristic relaxation times Dynamic (oscillatory)
Time-Dependent Viscoelastic Behavior Silly Putties have different characteristic relaxation times Dynamic (oscillatory)

Silly Putties have different characteristic relaxation times Dynamic (oscillatory) testing can measure time-dependent viscoelastic properties more efficiently by varying frequency (deformation time)

testing can measure time-dependent viscoelastic properties more efficiently by varying frequency (deformation time)
viscoelastic properties more efficiently by varying frequency (deformation time) TAINSTRUMENTS.COMTAINSTRUMENTS.COM

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Viscoelasticity, Deborah Number

Viscoelasticity, Deborah Number Old Testament Prophetess who said (Judges 5:5): "The Mountains ‘Flowed’ before the

Old Testament Prophetess who said (Judges 5:5):

"The Mountains ‘Flowed’ before the Lord"

Everything Flows if you wait long enough!

Deborah Number, De - The ratio of a characteristic relaxation time of a material ) to a characteristic time of the relevant deformation process (T).

De = τ/T

(τ ) to a characteristic time of the relevant deformation process (T). De = τ /T

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Deborah Number

Deborah Number Hookean elastic solid - τ is infinite Newtonian Viscous Liquid - τ is zero

Hookean elastic solid - τ is infinite

Newtonian Viscous Liquid - τ is zero

Polymer melts processing - τ may be a few seconds

High De Low De Solid-like behavior Liquid-like behavior
High De
Low De
Solid-like behavior
Liquid-like behavior

IMPLICATION: Material can appear solid-like because 1) it has a very long characteristic relaxation time or 2) the relevant deformation process is very fast

characteristic relaxation time or 2) the relevant deformation process is very fast TAINSTRUMENTS.COMTAINSTRUMENTS.COM

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Time and Temperature Relationship

Time and Temperature Relationship (E' or G') (E" or G") log Frequency log Time (E' or
(E' or G') (E" or G")
(E' or G')
(E" or G")

log Frequency

(E' or G') (E" or G") log Frequency log Time (E' or G') (E" or G")

log Time

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

Temperature

Time (E' or G') (E" or G") T e m p e r a t u

log Time

Time (E' or G') (E" or G") T e m p e r a t u

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Linear Viscoelasticity Region (LVR) Defined

Linear Viscoelasticity Region (LVR) Defined " If the deformation is small, or applied sufficiently slowly, the

"If the deformation is small, or applied sufficiently slowly, the molecular arrangements are never far from equilibrium.

The mechanical response is then just a reflection of dynamic processes at the molecular level which go on constantly, even for a system at equilibrium.

This is the domain of LINEAR VISCOELASTICITY.

The magnitudes of stress and strain are related linearly, and the behavior for any liquid is completely described by a single function of time."

Mark, J., et. al., Physical Properties of Polymers, American Chemical Society, 1984, p. 102.

J., et. al., Physical Properties of Polymers, American Chemical Society, 1984, p. 102. TAINSTRUMENTS.COMTAINSTRUMENTS.COM

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Importance of LVR

Importance of LVR E’ (or G’), E” (or G”), tan δ , η * Measuring linear
Importance of LVR E’ (or G’), E” (or G”), tan δ , η * Measuring linear
Importance of LVR E’ (or G’), E” (or G”), tan δ , η * Measuring linear
Importance of LVR E’ (or G’), E” (or G”), tan δ , η * Measuring linear
Importance of LVR E’ (or G’), E” (or G”), tan δ , η * Measuring linear
Importance of LVR E’ (or G’), E” (or G”), tan δ , η * Measuring linear

E’ (or G’), E” (or G”), tan δ, η *

Measuring linear viscoelastic properties helps us bridge the gap between molecular structure and product performance

properties helps us bridge the gap between molecular structure and product performance TAINSTRUMENTS.COMTAINSTRUMENTS.COM

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Setting up Rheological Experiments Oscillatory Tests

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Understanding Oscillation Experiments

Understanding Oscillation Experiments Define Oscillation Testing Approach to Oscillation Experimentation Stress and Strain
Define Oscillation Testing
Define Oscillation Testing

Approach to Oscillation Experimentation

Stress and Strain Sweep Time Sweep Frequency Sweep Temperature Ramp Temperature Sweep (TTS)

Sweep Time Sweep Frequency Sweep Temperature Ramp Temperature Sweep (TTS) TAINSTRUMENTS.COMTAINSTRUMENTS.COM

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What is Oscillation?

What is Oscillation? Phase angle δ Strain, ε Stress, σ * Dynamic stress applied sinusoidally User-defined
What is Oscillation? Phase angle δ Strain, ε Stress, σ * Dynamic stress applied sinusoidally User-defined
What is Oscillation? Phase angle δ Strain, ε Stress, σ * Dynamic stress applied sinusoidally User-defined
What is Oscillation? Phase angle δ Strain, ε Stress, σ * Dynamic stress applied sinusoidally User-defined
What is Oscillation? Phase angle δ Strain, ε Stress, σ * Dynamic stress applied sinusoidally User-defined
What is Oscillation? Phase angle δ Strain, ε Stress, σ * Dynamic stress applied sinusoidally User-defined
What is Oscillation? Phase angle δ Strain, ε Stress, σ * Dynamic stress applied sinusoidally User-defined
What is Oscillation? Phase angle δ Strain, ε Stress, σ * Dynamic stress applied sinusoidally User-defined
What is Oscillation? Phase angle δ Strain, ε Stress, σ * Dynamic stress applied sinusoidally User-defined
What is Oscillation? Phase angle δ Strain, ε Stress, σ * Dynamic stress applied sinusoidally User-defined
What is Oscillation? Phase angle δ Strain, ε Stress, σ * Dynamic stress applied sinusoidally User-defined
What is Oscillation? Phase angle δ Strain, ε Stress, σ * Dynamic stress applied sinusoidally User-defined
What is Oscillation? Phase angle δ Strain, ε Stress, σ * Dynamic stress applied sinusoidally User-defined
What is Oscillation? Phase angle δ Strain, ε Stress, σ * Dynamic stress applied sinusoidally User-defined
What is Oscillation? Phase angle δ Strain, ε Stress, σ * Dynamic stress applied sinusoidally User-defined
What is Oscillation? Phase angle δ Strain, ε Stress, σ * Dynamic stress applied sinusoidally User-defined
What is Oscillation? Phase angle δ Strain, ε Stress, σ * Dynamic stress applied sinusoidally User-defined
What is Oscillation? Phase angle δ Strain, ε Stress, σ * Dynamic stress applied sinusoidally User-defined
What is Oscillation? Phase angle δ Strain, ε Stress, σ * Dynamic stress applied sinusoidally User-defined
What is Oscillation? Phase angle δ Strain, ε Stress, σ * Dynamic stress applied sinusoidally User-defined
What is Oscillation? Phase angle δ Strain, ε Stress, σ * Dynamic stress applied sinusoidally User-defined
What is Oscillation? Phase angle δ Strain, ε Stress, σ * Dynamic stress applied sinusoidally User-defined
What is Oscillation? Phase angle δ Strain, ε Stress, σ * Dynamic stress applied sinusoidally User-defined
What is Oscillation? Phase angle δ Strain, ε Stress, σ * Dynamic stress applied sinusoidally User-defined
What is Oscillation? Phase angle δ Strain, ε Stress, σ * Dynamic stress applied sinusoidally User-defined
What is Oscillation? Phase angle δ Strain, ε Stress, σ * Dynamic stress applied sinusoidally User-defined
What is Oscillation? Phase angle δ Strain, ε Stress, σ * Dynamic stress applied sinusoidally User-defined
What is Oscillation? Phase angle δ Strain, ε Stress, σ * Dynamic stress applied sinusoidally User-defined
What is Oscillation? Phase angle δ Strain, ε Stress, σ * Dynamic stress applied sinusoidally User-defined
What is Oscillation? Phase angle δ Strain, ε Stress, σ * Dynamic stress applied sinusoidally User-defined
What is Oscillation? Phase angle δ Strain, ε Stress, σ * Dynamic stress applied sinusoidally User-defined
What is Oscillation? Phase angle δ Strain, ε Stress, σ * Dynamic stress applied sinusoidally User-defined
What is Oscillation? Phase angle δ Strain, ε Stress, σ * Dynamic stress applied sinusoidally User-defined
What is Oscillation? Phase angle δ Strain, ε Stress, σ * Dynamic stress applied sinusoidally User-defined
What is Oscillation? Phase angle δ Strain, ε Stress, σ * Dynamic stress applied sinusoidally User-defined
What is Oscillation? Phase angle δ Strain, ε Stress, σ * Dynamic stress applied sinusoidally User-defined
What is Oscillation? Phase angle δ Strain, ε Stress, σ * Dynamic stress applied sinusoidally User-defined
What is Oscillation? Phase angle δ Strain, ε Stress, σ * Dynamic stress applied sinusoidally User-defined
What is Oscillation? Phase angle δ Strain, ε Stress, σ * Dynamic stress applied sinusoidally User-defined
What is Oscillation? Phase angle δ Strain, ε Stress, σ * Dynamic stress applied sinusoidally User-defined
What is Oscillation? Phase angle δ Strain, ε Stress, σ * Dynamic stress applied sinusoidally User-defined
What is Oscillation? Phase angle δ Strain, ε Stress, σ * Dynamic stress applied sinusoidally User-defined
What is Oscillation? Phase angle δ Strain, ε Stress, σ * Dynamic stress applied sinusoidally User-defined
What is Oscillation? Phase angle δ Strain, ε Stress, σ * Dynamic stress applied sinusoidally User-defined
What is Oscillation? Phase angle δ Strain, ε Stress, σ * Dynamic stress applied sinusoidally User-defined
What is Oscillation? Phase angle δ Strain, ε Stress, σ * Dynamic stress applied sinusoidally User-defined
What is Oscillation? Phase angle δ Strain, ε Stress, σ * Dynamic stress applied sinusoidally User-defined
What is Oscillation? Phase angle δ Strain, ε Stress, σ * Dynamic stress applied sinusoidally User-defined
What is Oscillation? Phase angle δ Strain, ε Stress, σ * Dynamic stress applied sinusoidally User-defined
What is Oscillation? Phase angle δ Strain, ε Stress, σ * Dynamic stress applied sinusoidally User-defined
What is Oscillation? Phase angle δ Strain, ε Stress, σ * Dynamic stress applied sinusoidally User-defined
What is Oscillation? Phase angle δ Strain, ε Stress, σ * Dynamic stress applied sinusoidally User-defined
What is Oscillation? Phase angle δ Strain, ε Stress, σ * Dynamic stress applied sinusoidally User-defined

Phase angle δ Strain, ε

Stress, σ *

is Oscillation? Phase angle δ Strain, ε Stress, σ * Dynamic stress applied sinusoidally User-defined Stress
is Oscillation? Phase angle δ Strain, ε Stress, σ * Dynamic stress applied sinusoidally User-defined Stress

Dynamic stress applied sinusoidally User-defined Stress or Strain amplitude and frequency

stress applied sinusoidally User-defined Stress or Strain amplitude and frequency TAINSTRUMENTS.COMTAINSTRUMENTS.COM

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Frequency Defined

Frequency Defined Time to complete one oscillation Frequency is the inverse of time Units Angular Frequency

Time to complete one oscillation Frequency is the inverse of time Units

Angular Frequency = radians/second Frequency = cycles/second (Hz)

Rheologist must think in terms of rad/s.

1 Hz

=

6.28 rad/s

= cycles/second (Hz) Rheologist must think in terms of rad/s. 1 Hz = 6.28 rad/s TAINSTRUMENTS.COMTAINSTRUMENTS.COM

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Frequency

Frequency ωωωω = 6.28 rad/s ωωωω = 12.560rad/s 0 0 0 0 Time = 1sec ωωωω
ωωωω = 6.28 rad/s ωωωω = 12.560rad/s 0 0 0 0 Time = 1sec ωωωω
ωωωω = 6.28 rad/s
ωωωω = 12.560rad/s
0
0
0
0
Time = 1sec
ωωωω = 50 rad/s
= 6.28 rad/s ωωωω = 12.560rad/s 0 0 0 0 Time = 1sec ωωωω = 50

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Amplitude: Strain or Stress

Amplitude: Strain or Stress Strain and stress are calculated from peak amplitude in the displacement and
Strain and stress are calculated from peak amplitude in the displacement and torque waves, respectively.
Strain and stress are calculated from peak amplitude in the
displacement and torque waves, respectively.
0
0
0
0
Time = 1sec
amplitude in the displacement and torque waves, respectively. 0 0 0 0 Time = 1sec TAINSTRUMENTS.COMTAINSTRUMENTS.COM

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Dynamic Mechanical Testing

Dynamic Mechanical Testing An oscillatory (sinusoidal) deformation (stress or strain) is applied to a sample. The

An oscillatory (sinusoidal)

deformation (stress or strain) is applied to a sample.

The material response (strain or stress) is measured.

The phase angle δ, or phase shift, between the deformation and response is measured.

Deformation

between the deformation and response is measured. Deformation Response Phase angle δ TAINSTRUMENTS.COMTAINSTRUMENTS.COM

Response

between the deformation and response is measured. Deformation Response Phase angle δ TAINSTRUMENTS.COMTAINSTRUMENTS.COM
Phase angle δ
Phase angle δ
between the deformation and response is measured. Deformation Response Phase angle δ TAINSTRUMENTS.COMTAINSTRUMENTS.COM
between the deformation and response is measured. Deformation Response Phase angle δ TAINSTRUMENTS.COMTAINSTRUMENTS.COM

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Dynamic Testing: Response for Classical Extremes

Dynamic Testing: Response for Classical Extremes Purely Elastic Response (Hookean Solid) Purely Viscous Response

Purely Elastic Response (Hookean Solid)

Purely Viscous Response (Newtonian Liquid)

Strain

Stress

δ = 0°
δ = 0°

δ = 90°

Viscous Response (Newtonian Liquid) Strain Stress δ = 0° δ = 90 ° Strain Stress TAINSTRUMENTS.COMTAINSTRUMENTS.COM

Strain

Stress
Stress
Viscous Response (Newtonian Liquid) Strain Stress δ = 0° δ = 90 ° Strain Stress TAINSTRUMENTS.COMTAINSTRUMENTS.COM

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Dynamic Testing: Viscoelastic Material Response

Dynamic Testing: Viscoelastic Material Response Phase angle 0°< δ < 90° Strain Stress

Phase angle 0°< δ < 90°

Viscoelastic Material Response Phase angle 0°< δ < 90° Strain Stress TAINSTRUMENTS.COMTAINSTRUMENTS.COM
Viscoelastic Material Response Phase angle 0°< δ < 90° Strain Stress TAINSTRUMENTS.COMTAINSTRUMENTS.COM
Viscoelastic Material Response Phase angle 0°< δ < 90° Strain Stress TAINSTRUMENTS.COMTAINSTRUMENTS.COM

Strain

Stress

Viscoelastic Material Response Phase angle 0°< δ < 90° Strain Stress TAINSTRUMENTS.COMTAINSTRUMENTS.COM

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Viscoelastic Parameters: Complex, Elastic, & Viscous Stress

Parameters: Complex, Elastic, & Viscous Stress The stress in a dynamic experiment is referred to as

The stress in a dynamic experiment is referred to as the complex stress σ* The complex stress can be separated into two components:

a dynamic experiment is referred to as the complex stress σ * The complex stress can

An elastic stress in phase with the strain. σσσσ' = σσσσ*cosδδδδ

σ' is the degree to which material behaves like an elastic solid.

A viscous stress in phase with the strain rate. σσσσ" = σσσσ*sinδδδδ

2)

σ" is the degree to which material behaves like an ideal liquid.

1)

degree to which material behaves like an ideal liquid. 1) Strain, ε ε ε ε Phase
degree to which material behaves like an ideal liquid. 1) Strain, ε ε ε ε Phase

Strain, εεεε

Phase angle δδδδ Complex Stress, σσσσ*

σσσσ* = σσσσ' + iσσσσ"

=

+
+
σ * σσσσ * = σσσσ ' + i σσσσ " = + Complex number: +
σ * σσσσ * = σσσσ ' + i σσσσ " = + Complex number: +

Complex number:

+
+

The material functions can be described in terms of complex variables having both real and imaginary parts. Thus, using the relationship:

complex variables having both real and imaginary parts. Thus, using the relationship: TAINSTRUMENTS.COMTAINSTRUMENTS.COM

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Viscoelastic Parameters

Viscoelastic Parameters The Modulus: Measure of materials overall resistance to deformation. The Elastic (Storage)

The Modulus: Measure of materials overall resistance to deformation. The Elastic (Storage) Modulus:

Measure of elasticity of material. The ability of the material to store energy. The Viscous (loss) Modulus:

The ability of the material to dissipate energy. Energy lost as heat.

Tan Delta:

Measure of material damping - such as vibration or sound damping.

G =

G =

G " =

cos δ

sin δ

tan δ = "

G = G " = ∗ ∗ c o s δ ∗ s i n δ

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Storage and Loss of a Viscoelastic Material

Storage and Loss of a Viscoelastic Material RUBBER BALL X TENNIS BALL X LOSS (G”) STORAGE
RUBBER BALL X TENNIS BALL X
RUBBER BALL
X
TENNIS
BALL
X

LOSS

(G”)

STORAGE

(G’)

G* Phase angle δ
G*
Phase angle δ

Dynamic measurement represented as a vector

(G’) G* Phase angle δ Dynamic measurement represented as a vector G' G" TAINSTRUMENTS.COMTAINSTRUMENTS.COM

G'

G"

(G’) G* Phase angle δ Dynamic measurement represented as a vector G' G" TAINSTRUMENTS.COMTAINSTRUMENTS.COM

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Complex Viscosity

Complex Viscosity The viscosity measured in an oscillatory experiment is a Complex Viscosity much the way

The viscosity measured in an oscillatory experiment is a Complex Viscosity much the way the modulus can be expressed as the complex modulus. The complex viscosity contains an elastic component and a term similar to the steady state viscosity.

The Complex viscosity is defined as:

η* = η’ + i η” or η* = G*/ω

Note: frequency must be in rad/sec!

as: η * = η ’ + i η ” or η * = G*/ ω

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Dynamic Rheological Parameters

Dynamic Rheological Parameters Parameter Shear Elongation Units Strain γ = γ 0 sin(ωt) ε = ε

Parameter

Shear

Elongation

Units

Strain

γ = γ 0 sin(ωt)

ε = ε 0 sin(ωt)

---

Stress

σ = σ 0 sin(ωt + δ)

τ = τ 0 sin(ωt + δ)

Pa

Storage Modulus (Elasticity)

G’ = (σ 0 0 )cosδ

E’ = (τ 0 0 )cosδ

Pa

Loss Modulus (Viscous Nature)

G” = (σ 0 0 )sinδ

E” = (τ 0 0 )sinδ

Pa

Tan δ

G”/G’

E”/E’

---

Complex Modulus

G * = (G’ 2 +G” 2 ) 0.5

E * = (E’ 2 +E” 2 ) 0.5

Pa

Complex Viscosity

η * = G*/ω

η E * = E *

Pa·sec

Cox-Merz Rule for Linear Polymers: η * (ω) = η( ) @ = ω

Pa·sec Cox-Merz Rule for Linear Polymers: η * ( ω ) = η ( ) @

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Understanding Oscillation Experiments

Understanding Oscillation Experiments Define Oscillation Testing Approach to Oscillation Experimentation 1. Stress and

Define Oscillation Testing

Approach to Oscillation Experimentation 1. Stress and Strain Sweep 2. Time Sweep 3. Frequency Sweep
Approach to Oscillation Experimentation
1. Stress and Strain Sweep
2. Time Sweep
3. Frequency Sweep
4. Temperature Ramp
5. Temperature Sweep (TTS)
2. Time Sweep 3. Frequency Sweep 4. Temperature Ramp 5. Temperature Sweep (TTS) TAINSTRUMENTS.COMTAINSTRUMENTS.COM

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Dynamic Strain or Stress Sweep

Dynamic Strain or Stress Sweep Stress or strain Time The material response to increasing deformation amplitude
Stress or strain
Stress or strain

Time

The material response to increasing deformation amplitude (strain or stress) is monitored at a constant frequency and temperature.

Main use is to determine LVR All subsequent tests require an amplitude found in the LVR Tests assumes sample is stable If not stable use Time Sweep to determine stability

LVR Tests assumes sample is stable If not stable use Time Sweep to determine stability TAINSTRUMENTS.COMTAINSTRUMENTS.COM

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Dynamic Strain Sweep: Material Response

Dynamic Strain Sweep: Material Response Linear Region: Modulus independent of strain Non-linear Region: Modulus is a
Linear Region: Modulus independent of strain Non-linear Region: Modulus is a function of strain G'
Linear Region:
Modulus
independent
of strain
Non-linear Region:
Modulus is a function of strain
G'
Stress
Constant
γ c = Critical Strain
Slope
Strain (amplitude)
of strain G' Stress Constant γ c = Critical Strain Slope Strain (amplitude) TAINSTRUMENTS.COMTAINSTRUMENTS.COM

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G’

Temperature Dependence of LVR

G’ Temperature Dependence of LVR In general, the LVR is shortest when the sample is in

In general, the LVR is shortest when the sample is in its most solid form.

Solid Liquid % strain
Solid
Liquid
% strain
the LVR is shortest when the sample is in its most solid form. Solid Liquid %

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Frequency Dependence of LVR

Frequency Dependence of LVR LVR decreases with increasing frequency Modulus increases with increasing frequency
LVR decreases with increasing frequency Modulus increases with increasing frequency
LVR decreases with increasing frequency
Modulus increases with increasing frequency
LVR decreases with increasing frequency Modulus increases with increasing frequency TAINSTRUMENTS.COMTAINSTRUMENTS.COM

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SAOS versus LAOS Waveforms

SAOS versus LAOS Waveforms Linear response to a sinusoidal excitation is sinusoidal and represented by the
Linear response to a sinusoidal excitation is sinusoidal and represented by the fundamental in the
Linear response to a sinusoidal excitation
is sinusoidal and represented by the
fundamental in the frequency domain
Nonlinear response to a sinusoidal
excitation is not sinusoidal and
represented in the frequency domain by
the fundamental and the harmonics