Thermal cover:Layout 1 1/18/11 3:56 PM Page 2

TA Instruments
Dynamic Mechanical ANALYSIS

Accurate, Precise,
Versatile DMA
Measurements
 DMA Q800
SPECIFICATIONS

78
 Maximum Force 18 N
Minimum Force 0.0001 N
Force Resolution 0.00001 N
Strain Resolution 1 nanometer
Modulus Range 103 to 3x1012 Pa
Modulus Precision ± 1%
The Q800 is the world’s best-selling DMA, for very Tan δ Sensitivity 0.0001
good reason. It utilizes state-of-the-art, non-contact, Tan δ Resolution 0.00001
linear drive technology to provide precise control Frequency Range 0.01 to 200 Hz
of stress, and air bearings for low friction support. Dynamic Sample Deformation Range ± 0.5 to 10 000 µm
Strain is measured using optical encoder technology Temperature Range -150 to 600°C
Heating Rate 0.1 to 20°C/min
that provides unmatched sensitivity and resolution.
Cooling Rate 0.1 to 10°C/min
With its unique design, the Q800 easily outperforms
Isothermal Stability ± 0.1°C
competitive instruments and is ideal for high-stiffness Time/Temperature Superposition Yes
applications, including composites. RH Control Optional

Output Values
Storage Modulus Complex/Dynamic Viscosity Time
Loss Modulus Creep Compliance Stress/Strain
Storage/Loss Compliance Relaxation Modulus Frequency
Tan Delta (δ) Static/Dynamic Force Sample Stiffness
Complex Modulus Temperature Displacement
Relative Humidity (Optional)

79
 DMA Deformation Modes & Sample Size

Dual/Single Cantilever
8/4* mm (L), Up to 15 mm (W) and 5 mm (T)
20/10* mm (L), Up to 15 mm (W) and 5 mm (T)
35/17.5* mm (L), Up to 15 mm (W) and 5 mm (T)

3-Point Bend
5, 10, or 15 mm (L), Up to 15 mm (W) and 7 mm (T)
20 mm (L), Up to 15 mm (W) and 7 mm (T)
50 mm (L), Up to 15 mm (W) and 7 mm (T)

Tension
Film/Fiber 5 to 30 mm (L), Up to 8 mm (W) and 2 mm (T)
Fiber 5 to 30 mm (L), 5 denier (0.57 tex) to 0.8 mm diameter

Shear 10 mm square, Up to 4 mm (T)

Compression 15 and 40 mm diameter, Up to 10 mm (T)

Submersion
Tension Fixed at 15 mm (L), Up to 8 mm (W) and 2 mm (T)
Compression 25 mm diameter, Up to 10 mm (T)
3-Point Bend 5, 10, or 15 mm (L), Up to 15 mm (W) and 7 mm (T)

*Lengths are for dual/single cantilever

80
 Subambient Operation

Gas Cooling Accessory

The Gas Cooling Accessory (GCA) extends the operating range of the Q800
to -150°C. The GCA uses cold nitrogen gas generated from controlled
evaporation of liquid nitrogen. Automated filling of the GCA tank can be
programmed to occur after the scan is complete.

The GCA will provide ballistic or controlled cooling rates over the entire
operating range of the Q800 DMA (-150 to 600°C). In general, the maximum
cooling rate is a function of the installed clamp and the thermal characteristics
of the sample. The figure below shows the typical range* of controlled cooling
rates available as a function of temperature.

0
10
20

Cooling Rate (˚C/min)

30
40
50
60
70
80
-150˚C -50˚C 50˚C 150˚C 250˚C 350˚C 450˚C 550˚C
Temperature (˚C)

*Actual performance may vary slightly depending on laboratory conditions and

the clamping system installed.

81
 Q800 Technology

Drive Motor Optical Encoder

The Q800 uses a non-contact, direct drive motor to provide the oscillatory A high-resolution linear optical encoder is used to measure displacement
or static force required. The motor is constructed of high performance on the Q800 DMA. Based on diffraction patterns of light through gratings
composites that ensure low compliance and is thermostated to eliminate (one moveable and one stationary), optical encoders provide exceptional
heat build-up even when using large oscillation amplitudes and high resolution compared to typical LVDT technology. Due to the excellent
deformation forces. Sophisticated electronics enable the motor current to 1 nanometer resolution of the optical encoder, very small amplitudes can
be rapidly adjusted in small increments. The motor can deliver reproducible be measured precisely. This, combined with the non-contact drive motor
forces over a wide range and the force can be changed rapidly, enabling and air bearing technology, provides excellent modulus precision and high
a broad spectrum of material properties to be measured. tan δ sensitivity allowing the Q800 DMA to characterize a broad range of
materials.
Air Bearings
Low Mass, High Stiffness Sample Clamps
The non-contact drive motor transmits force directly to a rectangular
air bearing slide. The slide is guided by eight porous carbon air The Q800 features a variety of sample clamps that provide for multiple
bearings grouped into two sets of four near the top and bottom of the modes of deformation. The clamps are optimized using finite element
slide. Pressurized air or nitrogen flows to the bearings forming a frictionless analysis to provide high stiffness, with low mass, and attach to the drive
surface that permits the slide to “float.” The slide, which connects to shaft with a simple dovetail connection. The clamps are easy to use and
the drive shaft and sample clamp, can move vertically 25 mm and its adjust, and each is individually calibrated to ensure data accuracy. A broad
rectangular shape eliminates any twisting of the sample. Very weak range of samples can be analyzed. The high stiffness minimizes clamp
materials like films and fibers can be characterized with ease. compliance, and the low mass ensures rapid temperature equilibration.
These simple, yet elegant designs reduce the time necessary to change
Furnace clamps and load samples.

The Q800 features a bifilar wound furnace with automated movement.

The furnace design, combined with the Gas Cooling Accessory, provides Rigid Aluminum Casting
for efficient and precise temperature control over the entire temperature The Q800 drive motor, air bearing slide assembly with optical encoder
range, both in heating, cooling, and isothermal operation. The automatic and air bearings are all mounted within a rigid aluminum casting that is
furnace movement simplifies experimental setup. temperature controlled. The rigid aluminum housing minimizes system
compliance and the temperature-controlled housing ensures precise data.

82
 Furnace

Low Mass, High Stiffness Sample Clamps Air Bearings

Rigid Aluminum Casting

Drive motor Optical Encoder

83
 Modes of Deformation

Dual/Single Cantilever
In this mode, the sample is clamped at both ends and either flexed in the middle (dual
cantilever) or at one end (single cantilever). Cantilever bending is a good general-purpose
mode for evaluating thermoplastics and highly damped materials (e.g., elastomers). Dual
cantilever mode is ideal for studying the cure of supported thermosets. A powder clamp is
also available for characterizing transitions in powder materials.

3-Point Bend
In this mode, the sample is supported at both ends and force is applied in the middle.
3-point bend is considered a “pure” mode of deformation since clamping effects are
eliminated. The 50 and 20 mm clamps on the Q800 utilize unique low-friction, roller
bearing supports that improve accuracy.

Shear Sandwich
In this mode, two equal-size pieces of the same material are sheared between a fixed and
moveable plate. This mode is ideal for gels, adhesives, high viscosity resins, and other
highly damped materials.

84
Compression
In this mode, the sample is placed on a fixed flat surface and an oscillating plate
applies force. Compression is suitable for low to moderate modulus materials
(e.g., foams and elastomers). This mode can also be used to make measurements of
expansion or contraction, and tack testing for adhesives.

Tension
In this mode, the sample is placed in tension between a fixed and moveable clamp.
In oscillation experiments, the instruments use a variety of methods for applying a
static load to prevent buckling and unnecessary creep. The clamps are suitable for
both films and fibers.

Submersible Clamps
Film tension, compression, and 3-point bend clamps are available in submersible
configurations for the Q800. These clamps allow samples to be analyzed in a fluid
environment up to 80°C.

85
 DMA Accessories
DMA-RH
The new DMA-RH Accessory allows mechanical properties of a sample to be analyzed under controlled and/or varying conditions of both relative humidity and
temperature. It is designed for use with the Q800 Dynamic Mechanical Analyzer.

The DMA-RH Accessory is a fully integrated unit and includes the following hardware components:

1. The sample chamber mounts to the DMA in place of the standard furnace. Peltier elements in the chamber precisely control the temperature to +/-0.1°C.
The sample chamber accommodates standard DMA clamps (tension, cantilever, and 3-point bending). It is quickly removed for conversion back to the standard
DMA furnace.

2. A heated vapor-transfer line is maintained at a temperature above the dew point temperature of the humidified gas in order to avoid condensation and
provide accurate results.

3. The DMA-RH Accessory contains the humidifier and electronics which continuously monitor and control temperature and humidity of the sample chamber.

100
The DMA-RH accessory offers the
widest range of temperature and relative humidity. 90
80

Relative Humidity (%)

Temperature Range 5 to 120°C 70
Temperature Accuracy ±0.5°C 60
Heating/Cooling Rate Maximum ±1°C/min 50
Humidity Range See humidity range chart.
40
Humidity Accuracy 5-90% RH: ±3% RH
30
>90% RH: ±5% RH
20
Humidity Ramp Rate 2% RH/min (fixed)
10
(both increasing and decreasing)
0
0 10 20 30 40 50 60 70 80 90 100 110 120
Temperature (˚C)

86
 1

87
 DMA-RH Applications

4000 0.28
Effect of Relative Humidity on the Glass 80% RH
0.24
Transition of Nylon 6 50% RH
2000 20% RH

Storage Mdulus (MPa)

0.20

[ – – – –] Tan Delta
Nylon 6 is strongly plasticized by water; as such the mechanical 50% RH
properties will be dependent on the surrounding relative humidity. 
0.16
The data in this figure demonstrate the effect of relative humidity 0
on the glass transition of Nylon 6 as measured on the Q800 DMA 61.08˚C 67.49˚C
31.99˚C 49.44˚C 0.12
equipped with the DMA-RH accessory. The sample was analyzed
in single cantilever mode at a frequency of 1 Hz at a variety of 0.08
-2000
constant RH conditions. Note how the mechanical properties and
glass transition are significantly influenced by the imposed relative 0.04
humidity. -4000 0.00
0 20 40 60 80 100
Temperature (˚C)

Measurement of the Coefficient of

Hygroscopic Expansion (CHE)
1500
Hygroscopy is defined as the ability of a substance to attract water
molecules from the surrounding environment through either absorption
or adsorption. The effect of moisture sorption on the mechanical
characteristics of a material can be quantified by the Coefficient 1000
of Hygroscopic Expansion (CHE), the constant which relates the
dimensional change of a material to a change in the surrounding
relative humidity. The data in this figure show the effect of imposed 500
relative humidity on the Nylon 6 sample as measured by the
Q800 DMA with the DMA-RH Accessory. As the relative humidity
is increased the sample expands. The resulting slope of the line
is equivalent to the CHE for the material. 0

0 20 40 60 80 100
Relative Humidity (%)

88
 1000
Stress Relaxation of Nafion® 112 Under 0.5% Strain
Varying Temperature/RH Conditions

Relaxation Modulus (MPa)

25˚C/50% RH
Recent research has focused on alternative fuel technologies
including Proton Exchange Membrane Fuel Cells (PEMFC) which
contain polymeric membranes such as Nafion* 112.  PEM 100
properties can significantly change as functions of time and
85˚C/85% RH
exposure to elevated temperatures and humidity, as water is the
primary by-product of the electrochemical reaction of the fuel
cell.  The Q800 DMA equipped with the DMA-RH accessory is
the ideal platform to study the effect of temperature and humidity
on the time-dependent processes of the PEM. In this example, the
0
stress relaxation behavior of a Nafion 112 membrane is analyzed 1 10 100 1000 10000
in tension mode under two discrete conditions; 25°C/50% RH Decay Time (sec)
(controlled ambient) and under elevated temperature and RH
conditions of 85°C/85% RH.
*Nafion is a registered trademark of DuPont Co.

Analysis of a Pharmaceutical Gelatin Capsule 10000 0.5

83.46% 93.63%
Gelatin capsules are widely used in the pharmaceutical and 0.4

Storage Modulus (MPa)

dietary supplement market. When stored in an ambient, low- 1000
0.25% RH/min

[ – – – –] Tan Delta
humidity environment gelatin is remarkably stable. However, when
0.3
combined with water, gelatin forms a semi-solid colloid gel which
can profoundly affect its mechanical properties. The data in this 100
example illustrate the effect of increasing relative humidity on a 0.2
gelatin sample cut from the side wall of a two-piece capsule at
25°C and 40°C. As the relative humidity is increased, the material 10 25˚C
0.1
undergoes a multi-step transition resulting in a significant decrease
in modulus near 80% RH.  The transition is resolved in both the 40˚C
storage modulus and tan d signals. 1 0.0
0 20 40 60 80 100
Relative Humidity (%)

89
 DMA Theory
Range of Material Behavior
Dynamic Mechanical Analysis (DMA) is a technique used to measure the
mechanical properties of a wide range of materials. Many materials, including Solid Like Liquid Like
polymers, behave both like an elastic solid and a viscous fluid, thus the term
viscoelastic. DMA differs from other mechanical testing devices in two important Ideal Solid Most Materials Ideal Fluid
ways. First, typical tensile test devices focus only on the elastic component. In
many applications, the inelastic, or viscous component, is critical. It is the viscous Purely Elastic Viscoelastic Purely Viscous
component that determines properties such as impact resistance. Second, tensile
test devices work primarily outside the linear viscoelastic range. DMA works Viscoelasticity: Having both viscous and elastic properties
primarily in the linear viscoelastic range and is therefore more sensitive to structure.

DMA measures the viscoelastic properties using either transient or dynamic

oscillatory tests. The most common test is the dynamic oscillatory test, where a Figure 1
sinusoidal stress (or strain) is applied to the material and a resultant sinusoidal δ = 0˚ δ = 90˚
strain (or stress) is measured. Also measured is the phase difference, δ, between
the two sine waves. The phase lag will be 0° for purely elastic materials and
90° for purely viscous materials (Figure 1). However, viscoelastic materials Stress
(e.g. polymers) will exhibit an intermediate phase difference (Figure 2a).

Since modulus equals stress/strain, the complex modulus, E*, can be calculated. Strain
From E* and the measurement of δ, the storage modulus, E’, and loss modulus,
E’’, can be calculated as illustrated in Figure 2b. The storage modulus (E’) is the
elastic component and related to the sample’s stiffness. The loss modulus (E’’) 100% Elastic Behavior 100% Viscous Behavior
is the viscous component and is related to the sample’s ability to dissipate
mechanical energy through molecular motion. The tangent of phase difference, or
tan δ, is another common parameter that provides information on the relationship Figure 2a Figure 2b
between the elastic and inelastic components. 0˚ < δ < 90˚
E*
Transient tests include creep and stress relaxation. In creep, a stress is applied to Ell
the sample and held constant while deformation is measured vs. time. After some
time, the stress is removed and the recovery is measured. In stress relaxation, δ
a deformation is applied to the sample and held constant, and the degradation of El
the stress required to maintain the deformation is measured versus time. E* = stress/strain
El = E*cosδ
Ell = E*sinδ
Viscoelastic Behavior tan δ = Ell/El

90
 Multi-Frequency
Modes of Operation

% Strain/Stress

Time
Multi-Frequency
Multi-Stress/Strain The multi-frequency mode can assess viscoelastic properties as a function of frequency,
while oscillation amplitude is held constant. These tests can be run at single or
% Strain/Stress

multiple frequencies, in time sweep, temperature ramp, or temperature step/hold

experiments.

Multi-Stress/Strain
Creep/Stress Relaxation In this mode, frequency and temperature are held constant, and the viscoelastic
properties are monitored as strain or stress is varied. This mode is primarily used to
identify the Linear Viscoelastic Range (LVR).
Strain/Stress

Creep/Stress Relaxation
With creep, the stress is held constant and deformation is monitored as a function of
T1 T1 time. In stress relaxation, the strain is held constant and the stress is monitored vs. time.
Time
Controlled Force/Strain Rate
Controlled Force/Strain Rate
Strain/Stress

In this mode, the temperature is held constant while stress or strain is ramped at a
constant rate. This mode is used to generate stress/strain plots to obtain Young’s
Modulus. Alternatively, stress can be held constant with a temperature ramp while
strain is monitored.

Time
Isostrain Isostrain
In isostrain mode, available on the Q800, strain is held constant during a temperature
ramp. Isostrain can be used to assess shrinkage force in films and fibers.
Strain

Temperature

91
 Applications

10000 10000
Tg by E’ Onset
Tg by Tan Delta Peak
-30.60˚C
1000 -2.04˚C 1000
2.0
Measurement of Tg of Polymeric Materials

Storage Modulus (MPa)

Loss Modulus (MPa)

100 100
A common measurement on polymers is the glass transition 1.5

Tan Delta
Tg by E’’ Peak
temperature, Tg. It can be measured with various techniques, but 10 10
-28.58˚C
DMA is by far the most sensitive. The figure to the right shows a 1.0
scan of a pressure sensitive adhesive run in the tension clamps at a 1 1
frequency of 1 Hz. Tg can be measured by the E’ onset point,
0.5
by the E’’ peak, or the peak of Tan δ. In addition to the Tg, the 0.1 0.1
absolute value of the various viscoelastic parameters is also useful.
0.01 0.01
-100 -75 -50 -25 0 25 50 75 100 125
Temperature (˚C)

5000 0.20
E’ at 10 HZ Tg at 0.1 HZ 103.00˚C
Frequency Effect on Modulus and Glass 4000 Tg at 10 HZ 113.25˚C

Storage Modulus (MPa)

0.15
Transition of Polyethylene Terephthalate (PET)
Because the Tg has a kinetic component, it is strongly influenced 3000 E’ at 0.1 HZ

Tan Delta
by the frequency (rate) of deformation. As the frequency of the test 0.10
increases, the molecular relaxations can only occur at higher 2000 Tan Delta at 0.1 HZ
temperatures and, as a consequence, the Tg will increase with
increasing frequency as illustrated to the right. In addition, the shape 0.05
and intensity of the Tan δ peak as well as the slope of the storage 1000
modulus in the transition region will be affected. Based on end- Tan Delta at 10 Hz
use conditions, it is important to understand the temperature and 0 0.00
frequency dependence of transitions. 20 40 60 80 100 120 140 160
Temperature (˚C)

92
 100000
Tg 0.09
200.72˚C

Storage Modulus (MPa)

0.08
The Measurement of Secondary Transitions 10000
0.07
in Vinyl Ester

Tan Delta
β Relaxation 0.06
DMA is one of the few techniques sensitive to β and γ second- 101.27˚C
ary transitions. Secondary transitions arise from side group motion 0.05
1000 γ Relaxation
with some cooperative vibrations from the main chain as well as 0.04
-89.55˚C
internal rotation within a side group. The transitions are below the
Tg and typically subambient. They are very important as they af- 0.03
fect impact resistance and other end-use properties. This data was
100
generated using 3-point bending and also illustrates the ability to -150 -100 -50 0 50 100 150 200 250 300
run stiff composites.
Temperature (˚C)

1010 102

Measuring Effect of Adhesive Coatings 109 E' 101

E' Storage Modulus (Pa)

Frequency = 6.28 1 Hz
on Films
108 100
This figure shows a comparison among three PET samples in tension

Tan Delta
Uncoated
on the DMA; one with a uniform adhesive layer that performs well, Good Coating Tan Delta
one with a non-uniform layer that performs poorly, and one that is 107 Poor Coating 10-1
uncoated. A transition peak due to the adhesive is seen in Tan δ
around 40°C in the “good” sample, whereas the “poor” sample
106 10-2
shows a much smaller peak. Knowing the characteristics of good
and poor samples enables quality control of the coating process
and the finished product. 105 10-3
-90 -60 -30 0 30 60 90 120 150 180 210
Temperature (˚C)

93
 Applications

12000 2000
10401 MPa 142.70˚C
10000
Characterizing Printed Circuit Boards 141.84˚C 15000

Storage Modulus (MPa)

9589 MPa

Loss Modulus (MPa)

8000
Printed Circuit Boards (PCB) are typically comprised of fiberglass
braid impregnated with a thermosetting resin. Characterizing 1000
6000 PCB “As Received”
the Tg of PCB’s is often difficult due to the very low amount of
resin used. This figure shows a typical PCB run in single cantilever PCB “Post Baked”
4000
bending. The Tg is clearly discernible and the difference between
500
the sample “as received” and “post baked” clearly shows the effect
2000
that further crosslinking has on both the Tg and the absolute value
of modulus. 0
0
40 60 80 100 120 140 160 180 200
Temperature (˚C)

1010 10
Effect of Carbon Black in Elastomers
Another very common application is the effect of fillers and 109
additives on viscoelastic properties. The figure to the right illustrates 1
the effect on storage modulus (E’) and Tan δ when adding carbon

Modulus E' (Pa)

108

Tan Delta
black to an SBR rubber. This test, performed in dual cantilever on
the DMA, shows that adding carbon black increases the absolute 0.1
value of the storage modulus and significantly increases the Tg 107
temperature. Understanding how fillers and additives affect
material properties is crucial in many industrial applications. 0.01
106 SBR
SBR + Carbon Black
105 0.001
-80 -65 -50 -35 -20
Temperature (˚C)

94
 10
8.944% Good (PTFE/PP)
Poor (PTFE/PP)
8 Excellent (PTFE/PP/PE)
Characterizing Packaging Films
Jer=2.89 E-8 Pa-1
Using Creep 6 5.520%

Strain (%)
In a thermoforming process, a film is pulled down into a heated mold
to form a desired shape. The ability to produce a stable product 4 3.466% Jer=2.43 E-8 Pa-1
can be predicted by using a creep-recovery experiment. This figure
illustrates data on a packaging film using the tension mode. In the
2
recovery phase, the equilibrium recoverable compliance, (Jer) can Jer=8.86 E-9 Pa-1
be calculated. If the sample compliance is too high, as observed by
a high Jer, then the elasticity may be too low at the forming 0
temperature to maintain the desired shape. 0 5 10 15 20 25 30 35
Time (min)

Predicting Material Performance Using Time/ 1010

Temperature Superpositioning (TTS)
The TTS technique, well-grounded in theory, is used to predict
material performance at frequencies or time scales outside the range
E' Master Curve
of the instrument. Data is usually generated by scanning multiple

E' (Pa)
Tr=75˚C
frequencies during a series of isothermal step-hold experiments 109
over a temperature range. A reference temperature is selected and
the data shifted. A shift factor plot is generated and fit to either a
Williams-Landel-Ferry (WLF) or Arrhenius model. Finally, a master
curve at a specific temperature is generated as illustrated to the right
for a PET film sample. Using this technique, properties at very high
frequencies (short time scales) or very low frequencies (long time 108
scales) can be assessed. 10-15 10-8 10-1 106 1013 1020
Frequency (Hz)

95
Thermal cover:Layout 1 1/18/11 3:56 PM Page 1

tainstruments.com

© 2010 TA Instruments. All rights reserved. L90010.001