TMAThermomechanical Analysis

2

TMA / DTMA the methodThermo mechanical analysis (TMA) easily and rapidly measures sample

displacement (growth, shrinkage, movement, etc.) as a function of tem-

perature, time, and applied force. Traditionally, TMA is used to characte-

rize linear expansion, glass transitions, and softening points of materials

by applying a constant force to a specimen while varying temperature.

For expansion measurements, a probe rests on a sample on a stage with

minimal downward pressure. Other constant force experiments include

measurement of penetration, bending, tension, shrinkage, swelling, and

creep (sample motion measured as a function of time under an applied

load).

Typical Applications• Tension studies of the stress/strain properties of films and fibers

• Determination of softening behavior

• Glass transition temperatures and secondary transitions

• Phase change determination

• Determination of mechanical behavior under applied force

• Determination of expansion coefficient (dilatometry)

• Sintering behavior

• Volumetric expansion

• E modulus

• Slipping and friction resistance

General

• Highest Resolution

allows to measure smallest nanometer changes

• Dynamic Load TMA

measures weak transitions and elasticity

• Wide measuring range

from - 150°C to 1600°C*

• Calculated DTA

simultaneous measurements of thermal effects

• Modular design

allows future expansion of instrument

• Gas tight cell

controlled measurement environment

• Hyphenated techniques

evolved gas analysis

* Different furnaces (TMA PT1600)

TMA PT 1000 TMA PT 1600

3

The concept

Sample chamberThe easily accessible chamber is located in the center of the furnace.

Both temperature and atmosphere can be controlled. In addition an op-

tional mass flow controller is available for purge gas regulation. The gas

tight cell can be evacuated and allows you to measure under a defined

atmosphere. Only such a system can provide definitive information con-

cerning the samples sensitivity to oxidation.

FurnaceThe TMA Platinum Series comes with a robust and reliable furnace. Its

customized design enables rapid heat up and cool down times and an

excellent heating rate control over the entire temperature range.

The expansion and temperature sensorEvery dimensional change of the sample is transmitted via the pushrod

to the highly precise inductive transducer (LVDT sensor). Its precise and

reliable response over the entire temperature range guarantees highest

reproducibility of the TMA results. The temperature sensor is located

right beside the sample leading to the high accuracy.

The Dynamic TMA modeThis feature allows you to study the visco-elastic behavior of materials.

The Concept Technical Specifications

In D-TMA the force exerted on the probe alternates automatically by the

given frequency.

Sample Holders A broad range of sample holders is available for the TMA. Hence the best

method for testing can be selected for every application. Furthermore

LINSEIS can certainly provide aid for special customer requirements.

Automatic pressure controlThe contact pressure can be continuously varied between 10mN and

20 N depending on the system. This feature continuously adjusts the

contact pressure throughout expansion and/or shrinkage of the sample.

Cooling systemThe liquid nitrogen cooling system has been completely automated;

manual refilling is not necessary. This simplifies operation, improves

reproducibility and allows measurements to be performed over a long

period of time.

Integrated DTA signal:All LINSEIS TMA models are optionally equipped with the DTA evaluation

feature. This provides the user with valuable additional endo- and exo-

thermic sample information

TMA PT 1000 EM TMA PT 1000 TMA PT 1600

Temperature range -150 up to 1000°C -150 up to 1000°C-180 up to 500°CRT up to 1400/1600/ 1750/2000/2400°C

Force 1 or 5.7N 1, 5.7 or 20N 1 or 5.7N

Frequency 1 or 5Hz — 0.05 to 1 or 50Hz

Resolution 0.125 nm/digit 0.125 nm/digit 0.125 nm/digit

Sample size 30/50mm 30/50mm 30/50mm

Atmosphere inert, reduced react. gas inert, reduced react. gas inert, reduced react. gas

Technical Specifications

4

SoftwareAll LINSEIS thermo analytical instruments are PC controlled. The indi-

vidual software modules exclusively run under Microsoft® Windows®

operating systems. The complete software consists of 3 modules: tem-

perature control, data acquisition and data evaluation. The 32 bit soft-

ware incorporates all essential features for measurement preparation,

execution, and evaluation of a TMA/DTMA run. Thanks to our specialists

and application experts, LINSEIS was able to develop comprehensive

easy to understand user friendly application software.

Features -Software• Program capable of text editing

• Data security in case of powerfailure

• Thermocouple break protection

• Repetition measurements with minimum parameter input

Software

• Evaluation of current measurement

• Curve comparison up to 32 curves

• Storage and export of evaluations

• Export and import of data ASCII

• Data export to MS Excel

• Multi-methods analysis (DSC TG, TMA, DIL, etc.)

• Zoom function

• 1st and 2nd derivation

• Programmable gas control

• Statistical evaluation package

• Automatic axis re-scaling

• E-Modulus

• Several system correction features

• Automatic zero point adjustment

• Auto-scheduler for up to 16 uninterrupted runs

5

TMA / DTMA Features

With low constant load• Linear thermal expansion evaluation

• Change of volume

• Phase transformation

• Sinter process evaluation

• Softening point determination

• Transformation points

• Swelling behavior

• Tension

With increased constant load• Penetration

• Transition and comparison tests

• 3 point bending test

With dynamic load• Visco-elastic behavior

Additional optional features• DTA evaluation

• (RCS) Rate controlled sintering software

Features

Linear Motor

LVDT

Sample

Furnace

Frontview

Side view

Expansion Penetration E-Modulus

3-Point Bending VolumetricExpansion

Tension

6

40 60 80 100 120 140 160 180

3.8

3.6

3.4

3.2

3.0

2.8

2.6

2.4

2.2

2.0

1.8

1.6

1.4

1.2

1.0

0.8

0.6

0.4

0.2

0.0

0

-100

-200

-300

-400

-500

-600

-700

-800

-900

-1000

-1100

-1200

-1300

Delta

-L (c

onne

cted

) [µm

]

Temperature (smoothed) [°C]

E-Modulus [PVC-1]

Onset86.0°C

Delta-L [PVC-1]

Delta-L (1)[PIR2-1]

E-M

odul

us (s

moo

thed

) [Lo

g(N/

mm

2 )]

Offset100.5°C

Glass Point93.3°C

-80 -70 -60 -50 -40 -30 -20 -10 0 10 20 30 40 50 60 70 80 90 100 110 120

4.84.64.44.24.03.83.63.43.23.02.82.62.42.22.01.81.61.41.21.00.80.60.40.20.0-0.2

36

34

32

30

28

26

24

22

20

18

16

14

12

10

8

6

4

2

0

-2

Delta

-L (c

orre

cted

) [µm

]

Temperature (smoothed) [°C]

E-Modulus [PIR3-1]

Glass Point-55.°C6

Delta-L [PIR3-1]

E-M

odul

us (s

moo

thed

) [Lo

g(N/

mm

2 )]

Offset-54.8°C

Onset-58.2°C Delta-L [PIR3-1]

-80 -60 -40 -20 0 20 40 60 80 100 120Temperature [°C]

E-Modulus [PIR2-1]

Delta-L [PIR2-1]

Delta-L (1)[PIR2-1]

150

140

130

120

110

90

80

70

60

50

40

30

20

10

0

-10

Delta

-L (1

) [µm

]

5.0

4.5

4.0

3.5

3.0

2.5

2.0

1.5

1.0

0.5

0.0

E-M

odul

us (s

moo

thed

) [Lo

g(N/

mm

2 )]

Glass Point33.0°C

PolyvinylchlorideThis plastic has found extensive use as an electrical insulator for

wires and cables. Cloth and paper can be coated with it to produce

fabrics that may be used for upholstery materials and raincoats. The

glass point of the PVC sample was detected at 93.2°C. The elastic

range starts from approximately 150°C. At higher temperatures the

change of the sample into the plastic range can be detected very well.

Applications

Silicon rubberThe nature of its origin gives silicone a number of significant advan-

tages over conventional rubber polymers. These include the ability to

perform in extreme operating temperatures, excellent resistance to

weather and ozone, electrical resistance or conductivity, flame retar-

dency, and the ability to match nearly any colour. This type of rubber

was especially developed for use at low temperatures. The glass point

is at -54.9°C. The E-modules is shown over the entire temperature

range and the mean value of the expansion. The length change is up

to 50°C an expansion (elastic range) and thereafter a change into the

plastic range was detected.

ElastomersBecause of their very special and versatile properties, polyurethanes

Elastomers have found wide application in virtually every industry, va-

rying from the automotive, electrical and electronic industry, design

and textile industry, to the mining and heavy duty industry.

Evaluation of Elastomers specifically developed for applications above

0°C. The glass point was detected at 29.9°C. When further increasing

the temperature, additional expansion of the material in the elastic

range occurs. The plastic range of the material has not been reached

during this evaluation.

7

200 240 280 320 360 400 440 480 520 560 600 640 680

80

60

40

20

0

-20

-40

-60

50

40

30

20

10

0

-10

-20

Delta

-L [µ

m]

Temperature [°C]

DTA

Sign

al (s

moo

thed

) [µV

]

Temperature [°C]

DTA Signal (smoothed) [BK-00-3]Base Line [BK-00-3]

Point of Reaction576.1°C

Max/Min577.4°C 2.207µV

Onset575.2°C

FPM 2.4306 mm

EPDM 2.5267 mm

5%

0.01 N 1.0 N 0.01 N

0 15 30 45 60 75 90Time [min]

40 50 60 70 80 90 100 110 120 130 140 150 160 170

40

35

30

25

20

15

10

5

0

-5

-10

-15

-20

-25

-30

Load 2cN

Load 1cN

Delta

-L [µ

m]

Temperature [°C]

145.5°C

150.4°C

DTA - FeatureThe thermal expansion of rock crystal (α-SiO2) can be easily evalu-

ated with the L75 Dilatometer. The additional DTA feature enables

an in depth view of the thermal behavior of the material. The DTA

measurement is a mathematical routine based on the sample tem-

perature. Exo- and endothermic effects influence the change of the

sample temperature during the dynamic heating or cooling cycle.

At app. 575°C the phase transition from α- to β-SiO2 takes place.

The deviation of the measured temperature from the literature value

(574°C) can be used for a temperature calibration.

Creep Behaviour of ElastomersThe recovery behavior of sealing rings can be determined by the use

of Creep measurements. In the two different experiments a force of

1N was applied to two different sealing rings for 60 minutes at room

temperature. The recovery behavior was measured with an applied

force of 0.01N. This measurement allows to determine the elastic

deformation, the viscoelastic deformation (gradual change in thick-

ness), and the viscous flow (irreversible change in shape, creep). The

deformation of the EPDM sealing ring is grater than that of the FPM

ring. In comparison FPM, the EDPM used has a greater degree of

viscous flow and has a smaller elasticity modulus.

Polycarbonate PCAn important limiting factor for thermoplastic applications is the glass

transition point. With the different loads on the polycarbonate molded

parts investigated here, the TMA shows that softening occurs long be-

fore the glass transition temperature is reaches. During this investiga-

tion the material has been penetrated by a pushrod with two different

forces (1cN and 2cN). Depending on the load, the depths of the pene-

trations have varied. The heating rate for both evaluations has been

5K/min.

LINSEIS GmbHVielitzerstr. 4395100 SelbGermanyTel.: (+49) 9287–880 - 0Fax: (+49) 9287–70488E-mail: info@linseis.de

LINSEIS ChinaKaige Scientific Park 2653 Hunan Road201315 ShanghaiTel.: (+86) 21 6190 1202Fax.: (+86) 21 6806 3576

LINSEIS PolandDabrowskiego 105-800PruzkowTel.: (+48) 678 21 15 344

LINSEIS Inc.109 North Gold DriveRobbinsville, NJ 08691USATel.: (+1) 609 223 2070Fax: (+1) 609 223 2074E-mail: info@linseis.com

LINSEIS FranceBureaux Paris52 Boulevard Sébastopol75003 ParisTel.: (+33) 173-028 272

www.linseis.com

Products: DIL, TG, STA, DSC, HDSC, DTA, TMA, MS/FTIR, In-Situ EGA, Laser Flash, Seebeck Effect, Thin Film Analyzer, Hall-Effect

Services: Service Lab, Calibration Service

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