TA INSTRUMENTS 2940 THERMOMECHANICAL

ANALYZER (TMA)

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Operating
Instructions

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Table of Contents
1

INTRODUCTION

Safety

Samples

BACKG ROUND

Background Information

References

INSTR UMENT

O PERATIO N

Startup

Sample Loading

Test Conditions

Running the Test

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Cleanup

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Hardware Shutdown

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Introduction

he TA Instruments 2940 Thermomechanical Analyzer (TMA) is a powerful and

versatile analyzer that provides mechanical property measurements on a broad variety
of materials from -150 to 1,000C. The TMA is a useful tool for applications
involving dimension change as a function of temperature, time, or force. TMA is
usually used to precisely measure thermal expansion coefficients, but it can also be used to
determine creep and stress relaxation behavior, heat deflection, melting temperatures, and glass
transition temperatures. The TMA instrument works in conjunction with a controller and
associated software to allow for easy data acquisition and analysis.

Safety
The following labels are displayed on the TMA instrument for your protection:

Hot Stuff. The TMA is capable of heating samples to 1000C. During testing, the furnace
assembly becomes noticeably hot. After testing, the furnace assembly, sample, probe, and stage
may remain hot for some time. Do not touch the furnace assembly or sample stage area
during heating or while the sample is cooling from an elevated temperature.

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Cold Stuff. The TMA is capable of cooling samples to -196C through the use of liquid
nitrogen. Because of its low temperature (-196C), liquid nitrogen will cause tissue damage upon
contact with your skin. When you work with liquid nitrogen, use the following precautions:
Liquid nitrogen boils rapidly when exposed to room temperature. Only use liquid
nitrogen in a well ventilated area to prevent displacement of oxygen in the air.
Wear goggles or a face shield, cryogenic gloves, long pants, and closed-toed shoes.
Transfer the liquid slowly to prevent thermal shock to the equipment. Use containers
that have satisfactory low-temperature properties. Ensure that closed containers have
vents to relieve pressure.
Sample Decomposition. The TMA is capable of heating samples to 1000C. Many materials
may decompose during the heating, which can generate hazardous byproducts. WARNING: If
you are using samples that may emit harmful gases, vent the gases in an appropriate manner. In
general, samples should not be heated above their decomposition temperatures to prevent the
release of hazardous materials or contamination of the TMA.
Sample Melting. Since the TMA is capable of heating samples to 1000C, it is very possible that
your sample will melt. WARNING: A melted sample can easily stick to the stage, probe, or
furnace upon solidification. This will likely break or damage the instrument. Thus DO NOT
HEAT AN UNENCAPSULATED SAMPLE TO ANY HIGHER THAN 75% OF ITS
MELTING TEMPERATURE. For polymers, it cant hurt to encapsulate your sample even if
you are reaching temperatures at or above 50% of the sample melting point.

Samples
TMA samples should be smaller than a cylinder 10 mm in diameter and 25 mm tall.

Samples for thermal expansion and glass transition measurements should have parallel and
flat top and bottom surfaces.
Samples for melting temperature measurements may be any shape. NOTE: To avoid
making a mess with molten thermoplastics, you should encapsulate thermoplastic polymer
samples in aluminum foil or a DSC aluminum pan (ask your instructor or TA, or see the
Sample Preparation section of the DSC operating instructions, for information on specimen
encapsulation). To avoid reactions between molten metals and the quartz probe and stage,
you should sandwich your metallic sample between two plates of aluminum oxide.

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Background Information

Thermomechanical analyzers (TMAs) are used to measure a variety of material properties,

including coefficients of thermal expansion (CTE), melting temperatures, glass transition
temperatures, heat deflection, and elevated temperature creep or stress relaxation behavior. One
convenient aspect of the thermomechanical analyzer is that the same test can be used to find all of
these material properties!
In the typical operation of a TMA, a small sample with parallel and flat top and bottom surfaces is
placed on a quartz stage near a thermocouple. A quartz probe is lowered against the specimen
with a constant applied force, and a heating/cooling unit is placed around the sample stage
assembly. As the sample is heated or cooled, changes in dimension are measured by monitoring
the motion of the quartz probe. The schematic figure below shows the typical setup for thermal
expansion measurements.

While the specimen size does not need to fit any pre-set specification, there are some guidelines
for its size and shape. Specimens should also be no larger than 10 mm diameter (or 8 mm square
cross section) and 15 mm long, so that they will fit safely within the furnace and avoid
overloading of the extension sensor. If you plan to analyze the specimens for thermal expansion
or glass transition, they should have parallel top and bottom surfaces so that that TMA can better
gauge changes in size.
The coefficient of thermal expansion (CTE) is a normalized number that describes the
mechanical expansion or contraction of a material at different temperatures. It is an important
property of a material, and failure to take into account the effect temperature has on the physical

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size of materials has been known to cause many famous disasters, including the Challenger
explosion. The mean coefficient of thermal expansion (CTE) is calculated as

Ls
Lo T

where is the mean coefficient of thermal expansion in C-1, Ls is the expansion of the
specimen in mm, Lo is the initial specimen length in mm, and T is the temperature change in C
through the test. The CTE of a material is temperature dependent, and is a reported mean for a
particular temperature range. More information on the CTE can be found in chapter 21 of your textbook.
The glass transition temperature (Tg) is also an important characteristic of noncrystalline and
semicrystalline materials, but Tg is a particularly significant property of many common polymers.
At a temperature below Tg, amorphous and semicrystalline polymers tend to be hard and brittle
because the polymer chains are locked in a tangled, coiled position. Above Tg, the polymeric
chains are able to more easily rotate and slip past each other, and the polymer becomes softer and
more ductile. Generally the glass transition point depends on the processing of the material, as
well as that materials natural characteristics such as structure, bonding, and molecular weight.
The Tg is accompanied by a change in the polymers response to increasing temperature and is
identified on a TMA plot as a change in the slope of the expansion-temperature curve. See the
figure below for an example of the glass transition point.
While the TMA is not specifically designed to evaluate a materials melting temperature, it may
be used to perform this task. In thermomechanical analysis, a materials melting temperature is
identified as the point at which the sample stops expanding and starts flowing under the force
applied by the TMA probe. Thus, the point at which an increase in temperature creates a
decrease in size is that materials melting temperature.
Analysis of TMA curves is fairly straightforward, and all analyses may be performed within the
TA Instruments Universal Analysis software. The figure below is a TMA curve for a fiberglasspolyester composite prepreg material. The curve shows glass transition temperature (Tg) and the
difference between the CTE below and above the glass transition temperature of the polyester
component of the composite.

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References

Callister: Sections 19.3, 15.11-15.14, 2.5-2.7

Askeland: Chapter 21
ASM Engineered Materials Handbook Desk Edition (Online), Thermal Analysis and
Properties of Polymers

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Instrument Operation

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This section will walk you through the basic operation of the thermomechanical analyzer. Youll
have to follow a series of tasks that includes
Powering up the instrument,
Loading your sample,
Setting your testing conditions,
Running a scan and collecting data, and
Analyzing your results.

Startup
1. TMA: Turn on the main power switch followed by the heater power switch. Wait for the

instrument to boot.
2. Computer: Turn on the computer. Log in using the following username and password:
User name:
Password:
3. Open the Thermal Advantage software by double-clicking on the TMA-TA Instrument
Control icon on the desktop.

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Sample Loading
The following figure highlights the sample stage area (in yellow), which is hidden behind the
furnace assembly during operation of the TMA.

Load your sample, as follows:

1. Raise the furnace by pressing the FURNACE button on the instrument control panel.
2. Gently rotate the furnace to the left to move it out of the way of the sample stage. With the
furnace in the raised and rotated left position, you should notice a cylindrical quartz stage
(looks like a closed tube), a quartz probe (looks like a bent rod), and a thermocouple (metal
wires within a white ceramic sheath).
3. Raise the probe with the Probe up button on the instrument control panel, then lower the
probe with the Probe down button on the control panel. The probe should now be resting
on the sample stage.
4. Zero the probe position by pressing the Zero Length button on the control panel. Waitit
takes a little while for the probe to zero.
5. You now need to raise the probe and position your sample on the stage. If you press the
Probe up button one time, the probe will go up a little bit. If you need more room for your
sample, press the Probe up button again, and the probe will rise to its maximum height.
6. Carefully position your sample on the stage.
7. Lower the probe by pressing the Probe down button on the control panel. You may need to
press the button twice to lower the probe to your sample.
8. Gently rotate the furnace back to the center position (above the sample stage).
9. Lower the furnace by pressing the Furnace button on the control panel.

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Test Conditions
The figure below shows the TMA instrument control software window.

At the top of the window, you will notice a toolbar that includes buttons for starting
(green play arrow) and stopping (red square) the run.
At the left of the window, the run sequence is indicated. Usually a single run is shown
here, unless you have set up a multiple run sequence for your samples.
The middle of the window contains tabs that allow you to change the sample information
and testing parameters.
The top right of the screen shows the live signals from the hardware.
The middle right shows the run sequence for your test.
The bottom right shows a live graph of your data once the test has started.

After you have loaded your sample and closed the furnace (see Sample Loading section), follow
this sequence of steps to run a test:
Summary. This tab provides prompts for sample name, sample size, file name, etc.
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1. Measure your sample height by pressing the Measure Length button on the instrument

control panel (hardware). The measured sample height should be automatically displayed
after the Sample Size prompt in the Summary tab.
2. Enter your sample name, comments, and data file name in the appropriate spaces.
Procedure. This tab allows you to customize the test parameters.
1. Click on the Procedure tab.
2. If you would like to make changes to the ramp rate, temperature, or applied force, click the
Editor button and make appropriate changes. The following settings are recommended
for most specimens:
Force: 0.050 N
Ramp: 10.00 C/min
Temperature: -150 C to 1000 C (depends on the sample)
3. Click the Apply button to apply your changes to the current run sequence.

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Running the Test

To start the test run, simply click the green play arrow on the toolbar. Within moments, you
should see data appearing on the graph.

Cleanup
After the furnace and stage assemblies have cooled sufficiently, remove your sample and VERY
CAREFULLY clean off any debris on the sample stage. Cotton swabs are recommended for
cleaning the stage.
The quartz probe and sample stage are quite fragile, and the probe position and balance
calibrations may be affected if you apply too much force to the probe. If you have questions
regarding cleaning of the probe or sample stage, ask your instructor or TA for assistance.

Hardware Shutdown
You may leave the instrument and computer turned on. If you would like to shut it down,
1. Turn off the orange Heater and Power buttons on the instrument control panel.
2. Shutdown the computer.
3. If the heater and/or sample stage areas are hot when you are ready to leave the lab, place a
WARNING: HOT sign on the TMA.

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