Thermal Analysis Excellence

DMA/SDTA 1+
STARe System
Innovative Technology
Versatile Modularity
Swiss Quality

Dynamic Mechanical Analysis

Sets New Standards
 Precise Measurement Technology
DMA/SDTA 1+

for Highest Performance

Dynamic mechanical analysis (DMA) is used to measure the mechanical

and viscoelastic properties of a material as a function of temperature,
time and frequency while it is subjected to an oscillating stress.

Features and benefits of the METTLER TOLEDO DMA/SDTA 1+:

• Unique measurement of both displacement and force

results in a very accurate determination of moduli
• Wide force range from 1 mN to 40 N
allows you to measure very soft and very stiff samples
• Broad frequency range from 0.001 to 1000 Hz
means you can perform measurements under real conditions
or more rapidly at higher frequencies
• DMA Experiment Wizard
sets up the perfect experiment for the best results
• Patented SDTA technique
enables you to calibrate sample temperature and accurately
measure thermal effects
• Extremely wide stiffness range
means you can measure a sample from the glassy to the
liquid state in one single run
• Ergonomic design and touch-screen control
ensures faster setup and optimization of experiments

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Due to its revolutionary technology, the DMA/SDTA 1+ provides unattained
performance and offers time-saving external sample clamping.

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 Unsurpassed Measurement Results
DMA/SDTA 1+

Thanks to Innovative Solutions

The measurement principle of the DMA/SDTA 1+ ensures high accuracy

because it measures both displacement and force. This yields very accurate
modulus values. It was designed to measure material behavior at high
frequencies to match real-life conditions. This is enabled by its very stiff
stand resulting in an intrinsic resonance frequency of about 1500 Hz – well
above the measurement frequencies used (up to 1000 Hz).

Force measurement using Even more accurate Wide frequency range

a piezoelectric crystal displacement measurement from 0.001 to 1000 Hz

Force is measured directly by A special temperature-resistant The frequency range has been
means of a piezoelectric crystal LVDT allows measurements to extended to the kHz region for
and is not set using a force- be performed over a large mea- the first time ever in a DMA
current graph as in conventional surement range with nanometer instrument. In the shear mode,
DMA instruments. The force mea- resolution. The LVDT is located six decades are available. The
sured is that which is actually close to the sample so that only region above 1 Hz is particularly
applied to the sample. Compen- the deformation of the sample is interesting because it means that
sation for frictional losses, measured. This eliminates any measuring times can be kept to a
membrane force and inertia is no effect due to deformation of the minimum.
longer necessary. stand and also improves the ac-
curacy of measurement of the
phase shift. The reproducibility of
the displacement measurement is
improved by measuring the tem-
perature of the LVDT sensor and
correcting for the deviation.

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The stiffness range is given by the force and displacement ranges. With the
DMA/SDTA 1+, more than six decades are available. This means that it is
now possible to measure samples from the glassy to the viscoelastic state
in one experiment without having to change the sample geometry or the
deformation mode.
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 Simple Operation
DMA/SDTA 1+

Clever Sample Holder Design

Sample preparation and sample clamping are critical steps for accurate DMA
measurements. This is particularly the case for shear and tension samples
which are very often small and thin. The sample holder system therefore
offers important advantages.

Simplified sample holder Touchscreen terminal – for dis- Automatic switch mode
system placement and force calibration

The METTLER TOLEDO sample The touch-sensitive color terminal Force measurement also allows
holder system is a completely of the DMA/SDTA 1+ presents the instrument to be operated
new design that helps save valu- clear and precise information and in a way not possible with
able instrument operating time. is easily seen from a distance. conventional DMAs:
The samples are prepared and • All force and length calibra- The instrument can be operated
mounted externally in the sample tion routines are controlled via under either force or displacement
holder. This can then be quickly the terminal. This ensures that control and an intelligent
installed in the instrument. The these operations are performed automatic switch mode is also
concept also allows you to reliably and easily. possible.
change from one deformation • The 4-axis alignment adjust-
mode to another without perform- ment is also carried out via the
ing an adjustment. For example, terminal; the resulting values
you can prepare a bending ex- are transferred to the STARe
periment while a measurement in software. This eliminates any
the tension mode is in progress. possible transfer errors.

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The thermoelement can be placed close to the sample and allows thermal
events to be measured.

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 Calibration and Adjustment
Options and Accessories

for Maximum Accuracy

Calibration determines how well measurement equipment performs.

The standard DMA/SDTA 1+ calibration and adjustment procedures allow
the user to achieve compliance and avoid potential costs resulting from
inaccurate measurements. A Standard Operational Procedure is available
and describes the calibration of the individual quantities (force, length,
temperature).

Adjustment using Sample temperature measure- DMA Experiment Wizard

reference standards ment and calibration/adjustment

• The adjustment of force, Temperature calibration and ad- The DMA Experiment Wizard, with
displacement and temperature justment is particularly important. its built-in expert knowledge, is
is based on defined reference An additional temperature sensor designed to help users establish
standards. is located close to the sample. optimal sample dimensions,
• Force is adjusted using The sensor also allows thermal necessary for achieving accurate
a certified spring and effects to be simultaneously results. The software is also
displacement using gauge measured by SDTA (Single DTA). able to determine ideal force and
blocks. displacement amplitudes.
• Temperature measurement
close to the sample allows
calibration using the melting
points of pure substances.

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Matching accessories
For mounting clamp assemblies, sample holders, and for
performing calibrations, we supply an accessories box with all
the materials needed for calibration (temperature and
mechanical) and for installing samples (optional). This
ensures that you quickly obtain precise measurement results.

Small clamping assembly

Deformation mode Clamps Dimensions
Tension Small tension clamp 9 mm Length: 9 mm
Small shear clamp
Diameter: ≤15.0 mm
Shear Small shear clamp (for liquids)
Thickness: ≤6.5 mm
Small shear clamp (no surface structure)

Large clamping assembly

Deformation mode Clamps Dimensions
Bending clamp for 3-point bending Free length: 30 to 90 mm, max. length: 100 mm
Bending Single cantilever bending clamp Free length: 10 to 40 mm, max. length: 100 mm
Dual cantilever bending clamp Free length: 20 to 80 mm, max. length: 100 mm
Tension clamp 5.5 mm Length: 5.5 mm
Tension Tension clamp 10.5 mm Length: 10.5 mm
Tension clamp 19.5 mm Length: 19.5 mm
Compression Large compression clamp Diameter: ≤19.0 mm, thickness: ≤9.0 mm

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 Sample Holders
Options and Accessories

Simple, Ingenious and Timesaving

3-point bending Single cantilever bending Dual cantilever bending

This bending mode is ideal for This bending mode is suitable for Dual cantilever is the perfect mode
measuring extremely stiff sam- samples that expand or contract in for samples that would otherwise
ples, such as composite materials the longitudinal direction during bend excessively under strong
or thermosets, particularly below the measurement. This applies pretension. These are usually
the glass transition temperature. primarily to thermoplastic samples. thermoplastics or thermosets.

In the 3-point bending mode, the The single cantilever mode is In the dual cantilever mode,
ends of the sample rest on two very similar to the dual cantilever the ends of the sample are fixed
knife edges and an oscillatory mode except that only one end of and the middle is clamped to
force is applied to the middle of the the sample is fixed while the other the moving part providing the
sample by a moving knife edge. end is connected. oscillatory force.

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Tension Compression Shear

Tension is the mode most suitable This type of measurement is less The great advantage of the shear
for films, fibers and thin bars and suitable for the determination of mode is that everything from vis-
rods. The advantage is that sam- absolute values of the modulus; cous to very hard samples can be
ple clamping hardly affects the valuable relative information measured. This mode is therefore
deformation. can however be obtained when ideal for elastomers, thermoplas-
comparing soft materials like tics, and thermosets.
elastomers, pastes or foams.

In the tension mode, one end In the compression mode, the In the shear mode, two identical
of the sample is fixed and the sample is clamped between a samples are clamped sym-
other is subjected to an oscilla- fixed part and the moving part metrically between two fixed outer
tory force. The sample must be providing the oscillatory force. parts and a central moving part.
prestressed to prevent it from The sample is compressed The shear clamp guarantees a
buckling during the oscillatory statically and subjected to an homogeneous temperature
movement. alternating load. distribution.

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 DMA Theory
Theory

Force, Displacement and Phase Angle

The different moduli can be calculated from the raw data namely the
measured force and displacement amplitudes, Fa and La, and the phase shift δ:

• Complex modulus M*, elastic • Storage modulus M' (is rever- • Loss factor tan δ. Completely
modulus E* for bending, tension sible and proportional to the elastic materials exhibit no
and compression or the shear energy stored elastically). phase shift δ while purely
modulus, G*, for shear defor- • Loss modulus M" (irreversible viscous materials exhibit a 90°
mation. and proportional to the energy phase shift. The loss factor of
transformed into heat). viscoelastic materials is be-
tween 0 and infinity (δ = 90°).
Force in N
Kraft
Magnitude Force in N
1.4 Deformation in μm
1.2
1.0
0.8
0.6
0.4 ∆
0.2
0
– 0.2
– 0.4
– 0.6
– 0.8
–1.0
TimeTime
in s
Force and displacement at a frequency f of
–1.2 1 Hz. The time shift ∆ results in the phase
0 0.2 0.4 0.6 0.8 1.0 1.2 1.4 shift δ: δ = 2πf∆.
Force in N
Displacement in µm
The value of tan δ corresponds to where g is the geometry factor The stiffness of the sample can
the ratio of M" to M'. The moduli calculated from the sample thus be influenced by changing
are calculated from the measured dimensions. S is the stiffness of the sample geometry.
stiffness according to the following the sample (the actual measured
equations: quantity). M' = |M*| cos δ M" = |M*| sin δ
Fa Fa M"
|M*| = S * g = g S= tan δ =
La La M'

F: Static force
∆L: Deformation F

A thick sample is stiffer than a thin sample.

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 1

1. 4-axis alignment (x/y, α/b) 5. Sample

2. Force sensor 6. Furnace
3. LVDT (displacement sensor) 7. Drive shaft
4. Clamp 8. Linear motor

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 Characterization of Materials
Wide Variety of Applications

for a Wide Range of Applications

The DMA/SDTA 1+ is the perfect solution when maximum accuracy is

required over a wide range of stiffness or frequency. Thanks to its wide
dynamic force and displacement ranges and the large variety of sample
sizes and geometry, the DMA/SDTA 1+ can be used to analyze practically
all solid materials as well as medium and high viscosity fluids.

Materials are subjected to a wide range of different stresses in practical daily use. The
most important factors are the frequency and intensity of the stress, the temperature,
and the environment in which the load or stress is applied.

Effects and properties that can be characterized by the DMA/SDTA 1+:

• Viscoelastic behavior • Crystallization and melting

• Relaxation behavior • Gelation
• Glass transition • Phase transitions
• Mechanical modulus • Composition of blends
• Damping behavior • Curing and polymerization reactions
• Softening • Material defects
• Viscous material flow • Effects caused by filler materials

Application fields Materials tested by DMA

Stability testing, damage and fail- Thermoplastics, thermosets,

ure assessment, usability tests, elastomers, adhesives, metals,
material characterization. composites, paints, films and
fibers, construction materials,
pharmaceuticals, and foodstuff.

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Today's composites are often less expensive compared to traditional materi-
als, and highly sought after in many different industries where high strength
to weight ratios are paramount. DMA is ideal for the characterization of com-
posite materials with a wide range of moduli.

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Wide Variety of Applications

Phase transitions of PTFE by DSC and DMA

The DSC curve of PTFE shows the glass transition of the mobile amorphous fraction (γ) at about –100 °C followed
by two crystal-crystal transitions (β) at 30 °C. The crystallites melt at 330 °C. These transitions can also be
measured by DMA. The technique shows in addition the glass transition of the rigid amorphous fraction (α) at
130 °C. Glass transitions are easier to detect by DMA than by DSC. From Poisson's ratio, it follows that E' is in
principle always greater than G'.

Vulcanization of ethyl-vinyl acetate (EVA)

The vulcanization of EVA was investigated in the shear mode. The diagram displays the storage modulus of two
consecutive heating runs. The first heating run shows a glass transition at about –30 °C followed by melting
of the crystalline ethylene segments above about 50 °C. The increase of the modulus from 120 °C onward is a
result of the vulcanization or curing reaction. The second heating run shows the glass transition and melting of
the fully vulcanized EVA.
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Characterization of polyethylene terephthalate (PET)
The mechanical behavior of amorphous PET (polyethylene terephthalate) was investigated between –130 and
260 °C in the shear mode at a frequency of 1 Hz. The broad peak at –60 °C in the tan delta curve is due to
secondary relaxation (beta relaxation). The glass transition occurs at about 80 °C. The storage modulus increases
at about 110 °C as a result of cold crystallization. Reorganization processes then occur followed by melting of the
crystallites.

Viscosity of silicone oil

When silicone oil is rapidly cooled, crystallization is suppressed and the oil vitrifies. If a sample is then heated,
a glass transition (frequency dependent) is observed at about –110 °C (at 1 Hz) followed by crystallization
(frequency independent) at about –85 °C and melting (frequency independent) from about –45 °C onward. The
viscosity and its frequency dependence (inset diagram) can then be calculated from the modulus curves in the
liquid state (i.e. above –10 °C).
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Wide Variety of Applications

Master curves of styrene butadiene elastomers

Master curves over a wide frequency range provide detailed information about material properties. The excellent
temperature stability and accuracy together with the possibility of performing measurements at high frequencies
allow master curves to be quickly constructed. The figure displays master curves of unvulcanized and vulcanized
SBR. The curves not only describe dynamic behavior but also provide information about the molecular structure
and network.

Polyimide film measured in tension

Polyimides are high performance polymers that are not brittle at low temperatures and that can be exposed to
temperatures of up to 400 °C for a short time without losing their mechanical stability. The loss modulus curve
(E") of a 20-µm thick polyimide film measured in the tension mode at 1 Hz shows relaxation processes at about
–59 °C, 186 °C and 311 °C (maxima in E"). The process at 311 °C is the glass transition. The material begins to
decompose at about 450 °C.
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Determination of the modulus of a composite material
Printed circuit boards are made of fiber-reinforced plastics. Their maximum working temperature must be known
and is usually about 10 °C below the glass transition temperature. Another important factor is the modulus.
This and the glass transition can be easily determined by means of a DMA measurement in the 3-point bending
mode. In this example, the maximum operating temperature should not exceed 114 °C. Up to this temperature,
the modulus remains practically constant (24 GPa).

Shear measurement of an adhesive tape

The sample was a 20-µm thick double-sided adhesive tape. The adhesive layer (3 µm) on one side was slightly
stickier than on the other side (3 µm). The figure shows the storage modulus of the tape. In the first heating
run, the modulus decreases in two steps. The steps correspond to the glass transitions (Tg) of the two adhesive
layers (the Tg of the stickier layer is lower). The layers cure in the range 100 to 140 °C. The second heating run
shows the glass transition of the fully cured material.
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Wide Variety of Applications

DMA analysis of powders

Powder samples can be analyzed by DMA using a so-called powder pocket. This consists of a thin folded steel
sheet which is filled with powder and measured in the single cantilever mode. Alternatively, powders can be
compressed to a pellet and measured in compression. This allows relaxation processes to be detected with
better sensitivity. The diagram shows DMA curves of a compressed active pharmaceutical ingredient. The
sample exhibits β-relaxation at about 9 °C and a glass transition at about 107 °C.

Analysis of PEEK in single cantilever mode

Polyether ether ketone (PEEK) is a high-temperature resistant plastic with a melting point of 335 °C. It is, for
example, used in the automobile industry for thermally stressed components. To characterize the sample by
means of DMA, a thin plate (17 x 5 x 2 mm) was measured in the single cantilever mode between –120 and
240 °C. Two effects were detected: the secondary relaxation at –65 °C and the glass transition at 155 °C.

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Complete thermal analysis system
A complete thermal analysis system consists of four basic measuring techniques. Each technique characterizes
the sample in its own specific way. The full picture that simplifies interpretation is only obtained when all the different
results are combined. The techniques measure the mechanical modulus (DMA), the heat flow (DSC, Flash DSC), the
weight change (TGA), and the change in length (TMA). All these measurement variables change with temperature.

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Important Services

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METTLER TOLEDO’s portfolio of services is designed to ensure the continuous

performance and reliability of your thermal analysis systems. Factory-trained
in Switzerland, our worldwide teams bring the professional expertise and
know-how needed to provide you with the highest level of after-sales support
as well as the experience necessary to optimize services for your own
particular needs.

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are now available in METTLER TOLEDO's application database.
www.mt.com/ta-applications

23
DMA/SDTA 1+ Specifications
Temperature
Range –150 to 500 °C
Technical resolution 0.003 K
Accuracy 0.5 K
Force
Range 0.001 to 40 N
Technical resolution 0.15 mN (0 to 5 N), 1.5 mN (5 to 50 N)
Sensitivity 1 mN
Displacement
Range ±1.6 mm
Technical resolution 0.6 nm
Sensitivity 5 nm
Stiffness
Range 10 to 108 N/m
Precision 0.2%
Tan delta
Range 0.0001 to 5000
Technical resolution 0.00001
Sensitivity 0.0001
Frequency
Range 0.001 to 1000 Hz (*)
Technical resolution 0.00001
Frequency increments (∆f) 0.0001
• Linear or logarithmic
Frequency modes • Frequency series
• Multi-frequency
Deformation modes
3-point bending Length: 30 to 90 mm, length: 20 to 80 mm
Dual cantilever Width: <15 mm, thickness: <5 mm
Single cantilever Max. Sample length: 100 mm
Bending stiffness range 1 to 106 N/m
Shear Diameter: ≤15 mm, thickness: ≤6.5 mm
Shear stiffness range 1 to 108 N/m
Length: 19.5 mm, 10.5 mm, 9.0 mm, 5.5 mm
Tension
Width: ≤7 mm, thickness: ≤3 mm
Tensile stiffness range 1 to 107 N/m
Compression Diameter: ≤19 mm, thickness: ≤9 mm
Compressive stiffness range 1 to 107 N/m

Approvals
IEC/EN 61010-1, IEC/EN61010-2-010 and IEC/EN61010-2-081
CAN/CSA C22.2 No. 61010-1, No. 61010-2-010 and No. 61010-2-081
UL Std. No. 61010-1
IEC/EN61326-1 (class B)
IEC/EN61326-1 (industrial requirements)
FCC, Part 15, class A
AS/NZS CISPR 11, AS/NZS 61000.4.3

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Subject to technical changes.

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