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Users Training Course Rheometric Scientific One Possumtown Rd. Piscataway NJ 08854

Rheology - the study of flow of materials DMTA is Rheology on solids Also called Dynamic Mechanical Spectroscopy - it gives a spectrum of behavior of materials which are subjected to a dynamic or steady deformation.

DMTA looks at how materials respond to an imposed stress. The stress deforms the materials. The DMTA measures the strain - how far the material moves, and calculates how much energy is stored or dissipated during the process.

Mechanical Testing

Dynamic (Oscillatory) - Deformation is applied as a sinusoidal function. Steady - Deformation is applied as a constant over a time period.

Review of terms

Stress- Force deforming the sample per unit area (or) = F/A

Strain- the distance sample moves in response relative to the sample length in shear: = X/ Y in tensile = L/Lo

Hookes Law

Describes the behavior of an ideal elastic solid. Relates the applied strain to the resultant stress (or visa versa). The proportionality factor is called the modulus of the material. Denoted as E or G

Review of terms

Youngs Modulus is the ratio of dynamic stress to strain, E* (measured in tensile or bending mode) E= / Shear Modulus is the ratio of dynamic shear stress to strain, G* G= / for most rubbery polymers: E=3G

assuming a Poisson ratio of 1/2 (Poissons ratio is the linear contraction relative to the extension in tensile)

Review of terms

Viscosity - the resistance of a material to flow. High viscosity materials need more force to make them flow than low viscosity materials. Shear thinning - materials that become thinner, lower viscosity, as you increase the stress deforming them.

Newtons Law

Describes the behavior of ideal fluids according to the stress and shear Proportionality factor is viscosity, . Ideal viscous fluids are linear with shear rate, no shear thinning = d/dt =

+ o + o

Strain

Strain Rate

Elastic Response Viscous Response (t) Time

*(t)

Time (t)

*(t)

(t)

(t)

'

(t)

''

Review of terms

Storage Modulus, E - component in phase with the applied sinusoidal deformation; relates to stiffness of materials This is the elastic behavior of a materialthe solid-like properties it displays The storage modulus is a measure of how a material stores the energy of deformation, and allows material to regain shape after deformation

Review of terms

Loss Modulus, E- component out of phase with the applied sinusoidal deformation; relates to damping ability of material This is the viscous nature of the material its liquid-like behavior The loss modulus is an indication of how the material dissipates the energy used to deform it.

Modulus relationships

Loss (viscous) Modulus = E Liquid like behavior

Complex Modulus Phase angle tan = E/E Storage (Elastic) Modulus = E solid like behavior

Review of terms

tangent delta- E/E dimensionless, related to the damping characteristic. This is also called the loss tangent. A high tan delta means a greater ability to dissipates stress and behave more like a liquid.

Complex Modulus

Storage Modulus

G" = " = Gsin 0

Or E* = / Or E = / = (/)cos

Loss Modulus

Or E = / = (/)sin

Complex Viscosity

= G

tan = G/G or E/E

Loss tangent

V isco sity

= &

G ( t) = ( t)

( t) J(t) =

DMTA is a Controlled Stress Instrument

It generates data via a feedback loop: Strain is asked for in the method for stress is applied to the sample. Actual strain is measured, as is the applied stress to allow rheological data (E,E, tan delta) to be calculated.

A current to the motor moves the drive shaft. Motion of the drive shaft is detected by a position sensor consisting of a static probe and a target attatched tot he drive shaft. Change in magnitude of gap between probe and target produces a current in the position sensor, which is converted into a distance measurement. All are thermally isolated from the furnace.

The User defines the geometry; accurate measurements of the sample are CRUCIAL! Strain is multiplied by a geometrical constant to give an actual displacement that the DMTA will try to achieve. At the first data point 5% of the full scale allowable dynamic force is applied to the sample. Displacement is measured and the feed back loop takes over to control the force needed for the next data point.

Note: this initial 5% dynamic force can be changed in software with version 6.4.1 and higher via the measurement options section.

Chosen strain is divided by actual strain and if ratio is between 0.85 and 1.15 (+/15% window,user selectable defaults) the measurement can be taken. If this ration is outside the window, the applied force is multiplied by this ration and again applied to the sample.

Once strain falls within the window the standard measurement process begins: 2048 points are taken for strain and force from 1 to >64 cycles depending on frequency. Strain and force are cross correlated to models of a Sine and Cosine representing a perfect solid and fluid. This yields two phasors representing normalized strain and force amplitudes and their respective phase angles. Effects of mass of drive shaft and tools are taken into account to give correct applied force.

For the next data point the previous force is applied and if necessary modified to achieve the chosen displacement. Movement of the drive shaft due to sample growth does not affect the measurement of displacement in dynamic motion.

Controlling temperature

Temp. is measured by a PRT in the radiant oven. PID loops adjust the line voltage to power the furnace to heat. If using LN2, a solenoid (with 3 user selectable control features in ver. 6.4.1 and higher) allows LN2 into a cooling container surround the furnace, no LN2 ever touches the sample! Oven and LN2 can only operate if oven lid is fully closed- for safety reasons.

Review of terms

Viscoelastic- Polymers display the behavior of both elastic solids and viscous liquids. Linear Viscoelasticity- Region where the modulus is independent of the applied deformation

Linear Region Nonlinear Region

10

7

0.5

E'

b A b B b C Test 1 of 3 Test 2 of 3 Test 3 of 3

0.4

tan_delta (b A []

E' (b A [Pa]

tan delta

0.1

Length = 5.0 mm Width = 10.42 mm Thickness = 2.45 mm Frequency = 1 Hz

10 -2 10

10

-1

10

0.0 1 10

strain [%]

Materials that are stiff have a high storage modulus, E Soft materials have a high E tan delta gives the ratio of the two: E/E Materials change properties at the glass transition, stiffness (E),and ability to dissipate stress (E) change rapidly, thus the ratio (tan delta) gives a peak.

E = Storage Modulus = Elastic response tan = E/E

log Modulus

Temperature

Test Set up

Testing Options

Dynamic

Single point - to set parameters Time sweep at constant freq. Dynamic strain sweep Frequency dependence Temperature dependence Combinations of freq./temp. dependence

Transient

Static load - creep and TMA mode Constant strain - stress relaxation Strain rate testing- Stress vs. Strain Curves

Testing Conditions

Variables Deformation % strain Rate/Frequency in Hz or Rad/s Temperature ramp or step isothermal Time

or E

9x108 0.16

8x108 0.14 7x108

6x108

5x108

4x10

E Storage Modulus increase with frequency. 0.12 Material will be stiffer at higher frequency.

0.1

tan_delta (b K []

E' (b I [Pa]

E" (b J [Pa]

3x108

2x10

0.08

1x108

0.0 10-2

H idden Information

10

-1

10

10

0.06 20.0

Freq [H z]

10

5

10

Modulus, G', G" [Pa]

10

Eta* [Pa.s]

104

103

10 -1 10

100

Rheometric Scientific

Frequency, rad/s

101

10 2 10

or E Step testing or E Ramp

Frequency/Temperature testing

Frequency Temperature Ramp: Temperature ramps while frequencies are swept, two variables changing. Long frequencies or fast ramp rates will cause temperature to change before frequency sweep is complete Used only as a screening tool

Frequency/Temperature testing

Frequency Temperature Sweep: Isothermal Temperature steps at which frequencies are swept only one variable changes at a time Soak time used to allow thermal equilibration These are long runs, but clearly better data Used for Time Temperature Superpositioning (TTS)

Short Time / High Frequency(Rate) / Low Temperature Long Time / Low Frequency(Rate) / High Temperature

Data taken at higher temperatures represents data taken at lower frequencies (long times) Data taken at lower temperatures represents the behavior at high frequencies (short times) Data can be shifted horizontally to create a Master Curve TTS Software package uses WLF, (Williams Landel Ferry) equations

107

10

105

104

10

102

101 -1 10

G' b J b E b F b G b H b I b D

10

0

c c c c c c c 10

2

Frequency [Hz]

10

10

7

10

10

6

105

101

104

103

100

102

10 -3 10

10-2

10-1

10 0

10 1

10 2

10 3

Frequency [Hz]

10-1 4 10

tan delta

Stress Elastic Response

Time 2

Time 2

Stress Viscous Response

Time

Time 2

8.0

DMTA IV

6.0

Zone 1

Zone 2

Strain(t) (b Q [%]

4.0

2.0

0.0 0.0

60.0 120.0 180.0

240.0

time [s]

TMA mode

Tensile or compression geometry Sample of a measured length is subjected to a temperature ramp A load may be placed on the sample, either in tension or compression Change in length of the specimen is measured Coefficient of thermal expansion can be calculated

0.2

Sample in Compression

0.0

-0.2

Displacement (A ) [mm]

Linear Expansion

-0.4

-0.6

-0.8

-1.0

-1.2 0.0

50.0

100.0

150.0

200.0

250.0

300.0

Temp [C ]

Elastic Response Viscous Response

t1 Time

t1 Time

Strain Strain Rate

t1

t2 Time

t1

t2 Time

Elastic Response Viscous Response

t1

t 2 Time

t1

t 2 Time

Viscoelastic Response

t1

t2

Time

Strain Rate Test at -125C

6x105

5x105

4x105

stress(t) (b A [dyn/cm2]

3x10

2x105

1x105

0.0 0.0

0.5

1.0

1.5

2.0

2.5

3.0

strain(t) [%]

.

Dual cantilever bending Single cantilever bending Three point bending Tensile Compression Shear sandwich

Bending modes pull samples downward by a chosen amplitude then push up past zero to the same amplitude:

Clamp Zero position Zero position Clamp

Negative Strain amplitude Positive Strain amplitude

Sample moves X microns in negative direction, then X microns in the positive direction

Adjustable lengths Three frame sizes For solid bars Coatings on substrates Layered materials For specimens >1 mm in thickness

Three frame sizes For solid samples Best geometry for very high modulus (rigid) samples Eliminates edge effects from clamping For samples that grow with temp.

In a dynamic run tensile force pulls downward then returns towards the starting position but not past the zero point

Area = w * t Stress = = F/A Lo Strain= = L/Lo Strain Amplitude L Stationary clamp Mobile clamp

Zero position

Tensile Geometry

Films and Fibers Elastomers TMA mode Auto-gap sets sample length reproducibly Pretension and autotension keeps sample taut during testing

Compression Geometry

Foams Gels Determines the resilience of foam structures Auto gap sets thickness

Stress: Force per unit area Strain: Magnitude of deformation relative to sample geometry

A: Area y

Shear Sandwich

Pastes and gels Elastomers Best in horizontal orientation Useful for melts and viscous fluids

Sample types

Thermoplastic - can melt and reform into a solid without significant change Thermoset - heating will not melt it, material will cure/cross link and harden Elastomer - lightly cross linked, pliable, will not melt Polymer blend, Copolymer or Alloy

Material may be a solid rectangular bar A solid film A fiber or bundles of fibers A polymer coating on a substrate Thick melts or viscous liquids Foams, wet or dry, soft or rigid Pastes or gels

Clamping torque is important! Too much torque on the sample will create stresses radiating into the sample and distorting the data Too light clamping torque can cause sample to slip Re-clamping at lower temp. after contraction may be necessary

Keep clamp tension reproducible -even if stress patterns affect absolute results, the run to run variations will be minimal Thicker specimens fare better Use of rubber grips between steel clamps and films improve results

sections of rubber bands can be used, without introducing creep effect

When measurements on samples are inexact, the moduli values are affected. Specimens with uneven surfaces or geometries will not give consistent moduli. Bear in mind that moduli are usually plotted in log form, a slight change visually on the graph is a large change in data. Transition temperatures will not be affected.

Films and fibers are often more fragile requiring a gentle treatment in loading and testing Production often involves tremendous stresses on the material: drawing, orienting, annealing, extruding Internal stress causes rapid changes during and after Tg, measuring system must compensate rapidly

Uneven thickness are more problematic since aspect ratio is extreme Measuring the thickness of films and fibers can be imprecise Because of difficulty in loading, good lighting is important over work area

Deformation is in tensile, bending and compression generally not practical Sample length is more variable than bending modes: clamp geometry doesnt interfere with size. Autogap keeps sample length constant.

In many cases, the testing needs to use bundled fibers to represent real life Evenly distribute or wind the bundles Avoid kinking that would make some fibers longer than others Approximate sample dimensions and do not use absolute modulus values: run to run variations may be large

Curling of films

Electrostatic effects on thin films can cause static attractions that make loading frustrating Small residual stresses in the film from processing can cause curling Thin brittle films are subject to cracking while trying to flatten for loading

Buckling during loading causes serious errors

Effective sample length is the shortest line of contact by clamps, so by measuring the whole width you will have large errors, the buckled areas will not feel the force or deformation Difficult to evenly smooth sample as you load You can stretch the sample while doing so, causing stresses in the material

Sample buckling

Smooth sample distributes stress evenly across sample width Even sample width Clamps Buckled sample has an effective width narrowed to only the region that is taut between the clamps, modulus values depend on correctly measured geometry Sample width is taut region only

Wider samples are harder to load- buckling is more of a problem Thin film samples are more difficult to keep smooth Load the stationary grips first- this will give you a third hand as you align and smooth the sample, in case the mobile grips move during loading. Glance across the sample at an angle when loaded- do you see ripples?

The force needed to keep a specimen taut during a dynamic run can change Dimensional changes

as load remains on the sample it can creep as a sample softens during heating it will elongate, or shrinkage can occur as stress relaxation takes place

Stiffness changes

modulus values change dramatically at Tg

This additional tensile force is additive to the dynamic force, one must take care not to exceed linear viscoelastic regions Dynamic +

Pre-tension Dynamic Force alone Linear region exceeded Strain

Stress

a static pre-tension will not keep specimen taut, buckling will occur if sample elongates static pretension alone can exceed plastic deformation if sample shrinks static pre-tension can exceed linear region as sample softens need to have tracking with autotension which can change the force with changing sample modulus

In tensile geometry where a sample is long:

care must be taken to avoid temperature gradients: heat rises run DMTA in horizontal orientation. Or you will see: these temperature gradients can cause a broadening or doublet in Tg Failure can occur at the top edge, necking

Many materials contain residual solvent This acts as a plasticizer, lowering modulus and Tg Measuring systems must avoid changing the sample:

forced air convection furnaces dry-out specimens slow heating rates can also dry out and embrittle the sample

Loss of moisture or residual solvent can raise the modulus of the material Without the plasticizer (or solvent) Tg is raised Embrittlement Draw ratio decreases Lower elongation at break

Elastomer solvent swell Medical applications Leaching of plasticizers Destructive fluid interactions Fluid effects on creep

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