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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: [email protected]
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: [email protected]
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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