Imaging and Rheology techniques · Laser diffraction User day and complementary Imaging and...
Transcript of Imaging and Rheology techniques · Laser diffraction User day and complementary Imaging and...
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Laser diffraction User day and complementary Imaging and Rheology techniques
Etten-Leur 2015
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Rheology
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Laser diffraction User day and complementary Imaging and Rheology techniques
Rheology“The science of deformation and flow”
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RheologyIntroduction
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Laser diffraction User day and complementary Imaging and Rheology techniques
RheologyIntroduction
Why- Can my product not be pumped to the next production location?
- Is my paint still wet after 3 hours?
- Does it take an hour to drop some glue on my paper?
For all these questions the answer is;
Rheology helps to understand
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Laser diffraction User day and complementary Imaging and Rheology techniques
RheologyIntroductionRheology Importance to Various Industries
● Pharmaceuticals and personal care products● shelf life, sensory perception, yield point, gel strength, syneresis, consistency
● Foods● texture perception, storage stability, ‘mouth feel’, cooking characteristics, ● processability, extrusion, spreadability
● Ceramics● stability, pouring, pumping, casting performance
● Petrochemicals● lubricant formulation, temperature-viscosity profiles for engine
performance, drilling fluids – suspending capacity and pumpability, ● elevated temperatures and high pressure
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Laser diffraction User day and complementary Imaging and Rheology techniques
RheologyIntroduction
● Plastics and polymers● injection moulding efficiency, extrusion variations, molecular weight determination, dimensional
stability, surface finish, impact strength, glass transition temperature
● Paints, inks and coatings● spatter and fly in roller-coating, spray atomisation, film thickness, colour density, duct flow out,
dot retention and definition, sagging, pigment sedimentation under storage
● Asphalt● binder stiffness, fatigue, rutting, thermal cracking, SHRP specification testing
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RheologyIntroduction
Rheological measurements
Depending on the rheometer a sample is loaded between 2 plates or in a bore barrel.
After loading a sample; stress (force) is applied to the sample.
The sample experiences a strain or shear rate depending on the type of stress applied.
Shear rate is an indication of how fast you are deforming a material.
The sample experiences a shear profile.
Typical material properties can be calculated.
Like; Viscometry, Yield stress, Thixotropy and Viscoelatic behaviour.
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RheologyIntroduction
FLOW● Viscosity (flow) measurements.
● The resistance to flow.
● How thick is a paint sample.● Will the sample be pumped?
● Types of experiment:- Viscometry- Yield stress- Thixotropy
DEFORMATION● Viscoelastic (Oscillation)
measurements● How does a sample behave
before a sample flows…?
● Predicts sample properties.● Toothpaste – deforms and then
flows out of the tube.
● Types of experiment:- Complex modulus - Phase angle- Creep, Relaxation
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Rheology measurements can be divided into:
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Laser diffraction User day and complementary Imaging and Rheology techniques
Viscosity is defined as “resistance to flow”● To measure viscosity; we measure the resistance (i.e.
stress) when a material is flowing at a certain shear rate● A rheometer measures the push (stress) needed to get
the material to move at a certain speed (shear rate)
Viscosity test:1. Apply a constant shear rate (= force (f or p) per area (a))2. Measure the stress the material requires to flow
(=Shear (strain) rate: change in strain with time)
RateShear
StressShearViscosity
Top plate, surface area (a) rotates
with force (f)
RheologyIntroduction (Flow)
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Flow Curves Viscosity is a function of shear rate
Three general flow behaviours
› Most, real, samples are shear thinning with Newtonian regions
RheologyIntroduction (Flow)
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RheologyIntroduction (Flow)
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Yield Stress Measurement
Apply an increasing rotational “squeeze”, i.e. shear stress to a material
● A To measure viscosity; we measure the resistance (i.e. stress) when a material is flowing at a certain shear rate
● A material with yield stress will stretch easily, until the yield point, then flow
● The stress at the peak in viscosity is the force required to go from solid like to liquid like, i.e. the yield stress
● No peak (black line), no force needed
Stre
ss
Time
RheologyIntroduction (Flow)
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Thixotropic Measurement
Viscosity is not only dependent on shear rate it is also time dependent.
Example: Paint.
● Thick in the can on stock
● Thins when stirred.
● It is thixotropic as it does not rebuild straight away on stopping the stirring.
RheologyIntroduction (Flow)
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Thixotropic Measurement
RheologyIntroduction (Flow)
Store paint
Low shear rate
Appears “thick”
Stir paint
High shear rate
Becomes thinner, shear
thinning.
Apply paint
Low shearrate
Termed thixotropic: it takes time to
become thick again / rebuild
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Laser diffraction User day and complementary Imaging and Rheology techniques
Thixotropic Measurement
RheologyIntroduction
Bad PaintGood Paint
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Thixotropic Measurement
RheologyIntroduction (Flow)
● The longer it takes to rebuild, the more thixotropic the sample is
● Thixotropy also affects how long a sample takes to get to steady flow
● Thixotropy is not only an important material parameter. It is important to understand for reproducible measurements, i.e. repeat when fully rebuilt
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Most materials are not completely solid nor completely liquid like…
They are
viscoelastic
RheologyIntroduction (Deformation)
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Principles – Viscoelastic (Oscillation) testing
● Instead of rotating on a sample, we now oscillate back and forth● We typically apply a sinusoidal signal to the sample● This is non-destructive testing, so can show the properties under
deformation, before flow
RheologyIntroduction (Deformation)
From this we can predict sample properties
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Laser diffraction User day and complementary Imaging and Rheology techniques
Complex Modulus – G*From oscillation we can measure the materials complex modulus, the stiffness of a material
RheologyIntroduction (Deformation)
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Phase AnglePhase Angle can be calculated Different types of materials have a different log / phase angle between the applied and measured sinusoidal signal
RheologyIntroduction (Deformation)
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Phase AngleFor a Purely Elastic Material – Solid-like behaviourThe stress and strain are exactly in phasePhase angle is zero (Yogurt is elastically dominated, behaves solid like)
For a Purely Viscous Material – Liquid-like behaviourStress and strain are 1/4 of a cycle out of phasePhase angle is 90° (Honey is viscously dominated, behaves as a liquid)
RheologyIntroduction (Deformation)
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Rheology language tends to use a combined form of complex modulus and phase angle.
● If G’ > G’’, phase angle less than 45° - SOLID LIKE● If G’’ > G’, phase angle greater than 45° - LIQUID LIKE
● G* - modulus, is still a measure of toughness
RheologyIntroduction (Deformation)
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Oscillation ProceduresThere are fundamentally two parts of the oscillation that we can control:
RheologyIntroduction (Deformation)
1. The oscillation AMPLITUDE,stress or strain:
› Run an amplitude sweep experiment to determine the Linear ViscoElasticRegion
2. The oscillation timescale / FREQUENCY:
› Run an frequency sweep experiment to determine the response for different timescales
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Amplitude SweepThis tests records the:• Linear Viscoelastic Region (LVER) of a material• Indicates the stability of a suspension.
RheologyIntroduction (Deformation)
Small LVR
G’ S
tora
ge M
odul
us
Strain
Large LVR
› Can calculate the “Cohesive Energy” to quantify stability.
› How much energy required to break suspension.
› The larger, the more stable.
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Frequency Sweep● A frequency sweep records a
fingerprint spectrum of the material● It can also classify a material into
three general behaviours● The material property at rest (0Hz) classifies behaviour
RheologyIntroduction (Deformation)
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Frequency Sweep
On studying the phase angle…VISCOELASTIC SOLID: phase angle 0° at 0Hz
(45° 0°) SOLID LIKEVISCOELASTIC LIQUID: phase angle 90° at 0Hz
(45° 90°) LIQUID LIKEGEL : phase angle independent of frequency
RheologyIntroduction (Deformation)
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Kinexus
RheologyKinexus
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Kinexus series rheometers
RheologyKinexus
● Liquids to soft solids● Processability to product performance● Temperature to time dependence● From simple viscosity to complex
viscoelastic parameters
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Kinexus series rheometers
RheologyKinexus
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Interaction with hardware
● Auto-detection of accessoriesEnvironmental controllers and geometries
● Calibration and configuration data is stored on the instrument Auto-initialization of instrument on accessory change Always know what environmental cartridge is loaded and system
sets up accordingly Changing cartridge or geometry will prompt a re-zero of geometry
– best rheological practice
● System is always ready to measure
● Intelligent, automatic……and simple
RheologyKinexus
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Interchangeable lower cartrige system
Self-contained cartridges with unique functionality
● Provide lower geometry interchange and temperature and environmental control for sample
● Fully-integrated into Kinexus chassis● ‘Plug and play’
– all connections made/automatic recognition● Life-tested – repeatable mechanical alignment
(over 12000 operations)
RheologyKinexus
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Interchangeable lower plate● Interchangeable lower plates
Match upper and lower geometries for different sample types
Interchange between types of finish to optimize for different sample types
Easy cleaning● Consistent, repeatable and accurate mechanical alignment
● Thermal performance controlled
Stability, ramp performance, minimal thermal gradients Resolution 0.01°C
RheologyKinexus
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Temperature control
Plate Cartridge -40C to 200C●Peltier heating and cooling●Additional boost heater design● Improves heating performance●Minimises thermal gradient across Peltier
element lengthening life time●Dedicated protection thermocouples to
prevent overdriving Peltier element●Thermally-modelled – stability, ramp performance, gradient-free
RheologyKinexus
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Temperature controlActive Hood Cartridge (-40°C to 200°C)
● Minimized thermal gradients for plate measuring systems● Highly thermally-sensitive samples ● Proprietary design to control radial and vertical thermal losses from
local sample environment● Inlet for inert gas feed
Peltier Cylinder Cartridge (-30°C to 200°C)
● For concentric cylinder-type measuring systems● Highly fluid-like samples through to high concentration yield stress
dispersions
RheologyKinexus
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Geometry
Interchange: Quick-connect & releaseNew chuck mechanism for upper geometry
● Easy, quick, positive, reliable‘Plug and play’ configuration for quick start-up
● Auto-recognition● Set up into working state (zeroed and ready for sample loading) in
<30secs
RheologyKinexus
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Geometry
Viscometry: Cone (real viscosity)
Oscillation: Cone or plate (gap normally 0.5 – 1mm).
Size of geometry (guidelines):
● Viscosity ca. 1Pa.s: 40mm plates● Viscosity >> 1 Pa.s: 20mm plates● Viscosity << 1 Pa.s: 50-60mm plates
No grip on the sample/slippage:
● Serrated: 700um pyramids● Sand blasted: ca. 30um roughness
RheologyKinexus
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GeometryBob systems● Low viscosity samples
● Cup and Bob etc.
● Avoid breaking structure, avoid wall slib (yoghurt)
● Vane Tool
● Slippery samples:
● Sandblasted, Splined, Groved cup and bob
● Very low viscous samples
● Double gap (couette)
RheologyKinexus
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Solvent Trap Systems – minimize evaporation
Kinexus Active solvent trap cover (SS) (KNX2514)
● For Active Hood Cartridge ONLY ● Stainless Steel (SS)
Kinexus Passive solvent trap cover (SS) (KNX2513)
● For Standard Plate and Cylinder Cartridges ONLY ● Includes thermal cover to 200°C
and purge gas option
RheologyKinexus
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The Kinexus software:
r-Space
RheologyKinexus