Physical Characterization of

Composites

2003, P. Joyce

Thermal Analysis
Differential scanning calorimetry (DSC) can be used to
provide quantitative information about the physical and
chemical changes which are accompanied by a gain or loss
of heat in a material as its temperature is increased,
decreased, or held constant.
Glass transition temperature
Heat of reaction
Study of cure or decomposition processes

Measures the amount of heat that is involved as a material

undergoes either an endothermic or exothermic transition.
2003, P. Joyce

Thermal Analysis
What is glass transition temperature?
Represents a major transition for many polymers, where
the physical properties change drastically as the
material goes from a hard glassy to a rubbery state.
It defines one end of the temperature range over which the
polymer can be used, it is normally the upper use limit.
Changes in the Tg are often monitored to detect changes
resulting from exposure to environmental solvents or
increased cross-linking from thermal or UV aging.

2003, P. Joyce

Thermal Analysis

2003, P. Joyce

Thermal Analysis

2003, P. Joyce

Thermal Analysis

2003, P. Joyce

Thermal Analysis
Thermogravimetric Analysis (TGA) is used to determine
changes in sample weight, which may result from chemical
or physical transformations, as a function of temperature or
time.
Isothermal TGA measures the weight change as a function of time
at constant temperature.
Dynamic TGA measures the weight change as a function of
changing temperature (at a fixed rate.)
Can scan for volatilization, decomposition behavior.
Limited in that this technique does not provide information as to the
nature of the products evolved.

2003, P. Joyce

Thermal Analysis

2003, P. Joyce

Thermal Analysis

2003, P. Joyce

Dynamic Mechanical Analysis

Provides information on changes in viscoelastic
properties of materials as a function of
temperature, time or frequency at a constant
oscillatory strain.
Pretend I dont know anything about Chemistry
or Physics, just tell me what the Hell is going on.
Ghostbusters
2003, P. Joyce

Dynamic Mechanical Analysis

Definitions
Viscosity the tendency to flow
Elasticity the ability to recover from deformation
Damping the ability to lose energy as heat

Application
The DMA supplies an oscillatory force, causing a sinusoidal stress
in the sample, which generates a sinusoidal strain.
By measuring both the amplitude of the deformation at the peak of
the sine wave and the lag between the stress and strain sine waves,
quantities like the modulus, the viscosity, and the damping can be
calculated.
Can sweep across a temperature or frequency range (calculate a
modulus each time a sine wave is applied.)
2003, P. Joyce

Viscoelasticity
For a range of temperature all polymers will exhibit some
elastic behavior, like a Hookean solid characterized in
DMA by a complex modulus (E*), an elastic or storage
modulus (E), and an imaginary or loss modulus (E)
At elevated temperature polymers will begin to exhibit
some sort of flow behavior.
if you wait long enough everything flows

Like a Newtonian fluid characterized by the complex

viscosity *

2003, P. Joyce

Dynamic Mechanical Analysis

An oscillatory strain is applied to the sample in bending, tension, or
torsion as a function of time or temperature.
The frequency (0.01-200 Hz) and strain (0.03-1.7%) are preselected and
maintained constant throughout the analysis.
The resultant oscillatory stress which lags the applied strain by a phase
angle for a viscoelastic material, is measured.
Can be used to evaluate the cure process in thermosetting resins
Can Estimate

Gel point
Minimum viscosity
When it is stiff enough to bear its own weight
Can even estimate the activation energy

2003, P. Joyce

Thermal Analysis

2003, P. Joyce

Physical Testing

2003, P. Joyce

Physical Testing

2003, P. Joyce

Fiber Volume Fraction

For glass fiber reinforced composite
Calculate the mass of the residue (i.e. fibers)
W2= WTa- Wc
Where WTa is the mass of the crucible and contents after burnout and
cooling
Wc is the mass of the crucible empty

Then calculate the resin loss by ignition as follows

Wm = [(W1- W2)/ W1] x 100
Then, Wf = 100-Wm.
2003, P. Joyce

Fiber Volume Fraction

Likewise for the carbon fiber composite
Calculate the mass of the residue (i.e. fibers)
W2= WTa- Wf
Where WTa is the mass of the crucible and contents after burnout and
cooling
Wf is the mass of the Buchner funnel empty

Then calculate the resin loss by ignition as follows

Wm = [(W1- W2)/ W1] x 100
Then, Wf = 100-Wm.
2003, P. Joyce

Fiber Volume Fraction

Calculate Fiber Volume Fraction (in %)
Vf= [(ceWf)/f]*100
where,
ce= measured density of the composite
f= density of fibers
Wf= fiber weight fraction

2003, P. Joyce

Void Volume Fraction

First calculate the theoretical density of the
composite,

ct = f V f + mVm

Then calculate the void volume

void volume ct ce
Vv =
=
total volume ct

*100

where,
ct= theoretical density of the composite,
ce= measured density of the composite
2003, P. Joyce

Microscopy of Composite
Materials
Article on Surface Prep

2003, P. Joyce

References
1.) A Guide to Materials Characterization and Chemical
Analysis, J. P. Sibilia, 1988 VCH Publishers.
2.) Dynamic Mechanical Analysis, A Practical
Introduction, K. P. Menard, 1999 CRC Press

2003, P. Joyce