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TMA 402 F1/F3 Hyperion® - Thermomechanical Analyzer
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Meaningful Material Characterization
in the Low-Temperature Fields
Tension Test on a Polymer Film
Orientation effects, stretch conditions and shrinkage are measured under load for films. In this example, the expansion and contraction behavior of a 40-μm thick polycarbonate film was tested under tensile load. The results varied considerably depending on the load. Under low amounts of force (5 mN), the film contracted at higher temperatures; however, it expanded if greater force (50 mN) was applied.

Behavior of Polymers under Pressure
The extent to which the elastic properties of a seal remain intact after being subjected to a constant load of longer duration is very important. To test this, an elastomer seal was loaded with a force of 3 N and then relieved to 5 mN. Following a 40-hour load time, 21% compression was observed. After a 30-minute relief period, the compression had reversed by 16.2%; after 60 min, by 16.8%. The visco-elastic properties of the elastomer were such that the sample did not return to its original length even after 30 hours.

Visco-Elastic Properties of Polytetrafluoroethylene
The combination of a 3-point bending sample holder and a modulated sample force allows the visco-elastic properties of a material to be determined. A PTFE bar was measured between -150°C and 150°C under (rectangular) modulated force (fixed static force of 0.2 N and three different dynamic forces). Based on the expansion data and the sample geometry, the storage
modulus E´ can be calculated as a function of temperature. The three typical PTFE transformations are clearly visible at around -100°C (ß-transition), between 0°C and 50°C (crystal to condis-crystal transformation) and above 100°C (glass transition).

Meaningful Material Characterization in the High-Temperature Field
Sintering of Aluminum Titanate
One use of aluminum titanate is as a carrier material for catalytic converters in the automobile industry. Shown here is the measurement of an aluminum titanate green body in the temperature range from RT to 1450°C with a subsequent isothermal line at 1450°C of 7 hours. During the heating, shrinkage of 12.7% is observed. The sintering takes place in 2 steps with a maximum sintering rate of 0.31%/min. In the subsequent isothermal phase, further shrinkage of 0.6% occurs. To optimize the sintering process, an RCS measurement (rate controlled sintering; optionally available) can additionally be carried out.

Measurement with EGA (Evolved Gas Analysis)
A clay sample (powder) was tested in air using a TMA-MS (Aëolos®) coupling in the temperature range from RT to 800°C. At the beginning of the measurement, the adsorptively bound water and the interlayer water are released (shrinkage of 0.01%). Above 300°C, the sample’s organic constituents burn up (maxima in the curves for m18, water, and m44, CO2). There is no visible influence on the expansion curve here, due to the very low proportion. Between 487°C and 536°C, dehydroxylation of the sample’s clay mineral content takes place. Associated with that is a sample shrinkage of 0.05%.
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