Analyzing & Testing

Dilatometry
Method, Instruments, Applications – From -180°C to 2800°C

Leading Thermal Analysis

 Dilatometry
Dilatometry
Dilatometry is a thermoanalytical
technique used to measure the
expansion or shrinkage of solids,
powders, pastes and liquids under
negligible load when subjected to a
controlled temperature/time program.
A precise understanding of this
behavior can provide insight into firing
processes, the influence of additives
and raw materials, densification and
sintering properties, reaction kinetics,
phase transitions, and thermal shock.
In addition, it can be used for glaze
development and to match CTEs
(glaze-ceramic, metal-ceramic in the
automotive industry).
Dilatometry can be applied not only
to solid samples, but also to powders,
pastes, and even liquids.
It can also be used to carry out rate-
controlled sintering studies on reactive
powders in fields such as advanced
ceramics or powder metallurgy.
DIL 402 C as an example of a pushrod dilatometer
2
Due to large technological advances,
this thermal analysis method can now
measure even the slightest of thermal
behaviors in ceramics.
Recent innovations in dilatometer
hardware and software design promise
to augment the possibilities provided by
thermal expansion measurement. Such
innovations include the application of
new thermokinetic analysis techniques
to model- and construct-optimized firing
and sintering processes, the combi-
nation of dilatometry with calculated
Differential Thermal Analysis (c-DTA®)
for a better understanding of thermal
behavior, and the designing of new
hardware to improve low-temperature
thermal expansion measurements.
All NETZSCH dilatometers are designed
in accordance with standards such as
DIN EN 821, DIN 51045, ASTM E831,
and ASTM E228.
Table of Contents

Dilatometry – Method and Principle of Operation  4

DIL 402 PC – The Reliable Workhorse for Glass and Ceramics  6

DIL 402 C – Perfect for Sophisticated Demands  8

DIL 402 CD – Dual and Differential Excellence  12

DIL 402 E – Precision at the Highest of Temperatures  16

Dilatometry Accessories  20

Dilatometer Software – Software Specialties  22

Performance and Low-Temperature Applications  26

High-Temperature Applications  28

c-DTA® and Other Specialties – Deep Insight into Material Behavior  32

Phase Transition Building Materials

Sintering
Refractories
Alloys
Density
Metals

Shrinkage Dilatometry
Softening

Expansion
Polymers
Ceramics Composites
Porcelain CTE
Glass

3
 Dilatometry – Method and Principle of Operation
Method and Principle of Operation
Method
Pushrod dilatometry is a method for
determining dimensional changes versus
temperature or time while the sample
undergoes a controlled temperature
program. The degree of expansion
divided by the change in temperature
is called the material’s coefficient of
expansion (α) and generally varies with
temperature.
Principle of Operation
To perform a dilatometric analysis, a
sample is inserted into a special holder
within a movable furnace. A pushrod is
positioned directly against the sample
and transmits the length change to a
linear variable displacement transducer
(LVDT).
Furnace
Sample holder
Pushrod
LVDT
system Sample
Schematic of a pushrod dilatometer
4
( )
1 ∆l
α = — —–
L0 ∆T
α coefficient of expansion
L0 initial sample length
∆T change in temperature
∆l change in length
As the sample length changes during
the temperature program, the LVDT core
is moved, and an output signal propor-
tional to the displacement is recorded.
The temperature program is controlled
using a thermocouple located either
next to the heating element of the
furnace or next to the sample.
Since the sample holder and the front
part of the pushrod are being exposed
to the same temperature program as
the sample, they are also expanding.
The resulting dilatometer signal is
therefore the sum of the length changes
of sample, sample holder, and pushrod.
It is thus necessary to correct the raw
dilatometer data in order to obtain a
true view of sample behavior. There are
two correction methods: the application
of tabulated expansion data, or – often
more precise – of a correction curve to
eliminate systematic error.
 Results and Measuring Accuracy
dL/Lo / %
Literature (1500°C): 1.307 %
Test #1 (1500°C): 1.309 % The thermal expansion in percent is
Sample: Polycryst. Alumina Test #2 (1500°C): 1.312 %
1.400 Test #3 (1500°C): 1.311 % an important value for evaluating a
1.200 material’s performance.
Literature (1000°C): 0.799 %
Test #1 (1000°C): 0.800 %
1.000
Test #2 (1000°C): 0.802 % In this diagram, the length changes of
Test #3 (1000°C): 0.802 %
0.800 3 test runs (lines) on polycrystalline
alumina (Al2O3) are presented together
Literature (500°C): 0.350 %
0.600 Test #1 (500°C): 0.349 % with the corresponding data from
Test #2 (500°C): 0.350 %
0.400
Test #3 (500°C): 0.351 % literature (crosses).

0.200
The differences between these values at
0.000 500°C, 1000°C and 1500°C generally
amount to less than 1%, demonstrating
200 400 600 800 1000 1200 1400 1600
Temperature / °C the outstanding accuracy of the
NETZSCH DIL 402 PC which was used
Comparison of the expansion data of polycrystalline alumina with literature values for these measurements.

Advantage of a Horizontal Pushrod Additional Advantages DIL Measurement Information

Dilatometer

The superior thermal uniformity of a  Wide temperature range  Linear thermal expansion
horizontal pushrod dilatometer can be  Easy handling  Coefficient of thermal expansion (CTE)
attributed to very low temperature  High accuracy  Volumetric expansion
gradients. A horizontal furnace is not  Homogeneous temperature profile  Shrinkage steps
subject to convection parallel with the  Flexible sample geometry  Glass transition temperature
sample.  Low risk of contamination (LVDT)  Phase transitions
 Sintering temperature/sintering step
Particularly for long samples, a  Density change
horizontal dilatometer system is  Softening points
essential in ensuring that the temper-  Influence of additives/raw materials
ature distribution is reasonably uniform.  Decomposition temperature –
e.g., of organic binders
 Anisotropic behavior
 Optimizing of the firing process
 Rate-controlled sintering (RCS)
 Caloric effects by using c-DTA®
 Thermokinetics

5
 Dilatometer 402 PC – The Reliable Workhorse for
Glass and Ceramics
Dilatometer DIL 402 PC – Precise Expansion and Shrinkage
Measurements in Routine Operation
The DIL 402 PC is specially tailored to
the needs of the ceramic and glass
industry. High resolution and stability, a
wide measurement range, and a robust
and compact design are only some of
the many advantages of this
cost-effective instrument. This
dilatometer combines easy operation,
high adaptability to different applica-
tions, and outstanding performance in
one instrument. The optimized design
of the measurement system with
inductive transducer compensates for
temperature fluctuations and yields
highly reproducible data. A chiller is not
required.
The DIL 402 PC operates in accordance
with nearly all national and international
standards (e.g., DIN 51045, or
JIS R 2207-contact version).
6
Design The forced-air cooling system of the
1600°C furnace makes it possible to
The instrument has a horizontal design cool from maximum sample temper­
with an easy-to-operate furnace. A large ature down to room temperature.
recess in the tube-type sample carrier
facilitates the placement of samples
even when their geometries are less Sample Holder Systems and Sample
than ideal. A thermocouple in direct Dimensions
proximity to the sample ensures repro-
ducible temperature measurement. Exchangeable sample holder systems
made of alumina and fused silica are
available. The maximum sample dimen-
Furnaces sions are 50 mm in length with a
diameter of up to 12 mm (optionally
The interchangeable furnaces with 19 mm).
temperature ranges up to 1200°C
and 1600°C allow for the analysis
of expansion control in solids, green
bodies, powders and pastes, for
production and quality assurance
purposes across a variety of applications.
DIL 402 PC – 1600°C version
Technical Key Data for the DIL 402 PC At a Glance – The Characteristics
of the DIL 402 PC
 RT to 1200°C
Temperature range/furnaces
 RT to 1600°C  High flexibility with two
Heating rate 0.1 to 50 K/min interchangeable furnaces
Temperature precision 0.1 K  Various accessories for special
applications (sample holders
Measuring range 500/5000 μm
and containers)
Load at the sample 15 cN to 45 cN (optionally 45 cN to 100cN)  Large sample dimensions
∆l resolution 8 nm/digit  Ease of operation
Sample diameter Up to 12 mm (optionally 19 mm)  Highly reproducible results
 Up to 25 mm
Sample length
 Up to 50 mm
 Alumina
Sample holders
 Fused silica
 3-point bending mode (determination
of the firing stability, set made of Al2O3)
Special sample holder
 Fibers in tension
systems
 Thin metals and ceramic foils
 Penetration
 Powders
Sample containers  Pastes
 Metals and glasses in the liquid state Special sample holder for the determination of
the firing stability
 Oxidizing static and dynamic
Atmosphere
 Inert dynamic
For temperature calibration and detection of
c-DTA®
endo- and exothermal effects
Gas flow controller For purge gas (optional) thermocouple furnace

sample

sample
inductive pushrod carrier
transducer

adjustment screw
base unit DIL 402 PC – 3-dimensional sectional view

7
 Dilatometer 402 C – Perfect for Sophisticated Demands
DIL 402 C – Flexibility Combined with Vacuum-Tightness
The Dilatometer DIL 402 C features an
excellent set of capabilities optimized
to fulfill any potentially occurring appli-
cation need. These include flexibility of
temperature range, sample holder,
and gas atmosphere, along with high
accuracy and easy handling – the
result of over 50 years of experience in
building dilatometers.
The state-of-the-art design is compact
and extremely flexible; it uses a number
of interchangeable furnaces with
horizontal movement and provides
easy access to the sample holder. It is
the perfect instrument for applications
in the areas of not only traditional
ceramics and glass, but also advanced
ceramics and powder metallurgy (e.g.,
when carrying out sintering studies on
reactive powders).
8
Measurement System
The high-resolution displacement trans-
ducer is employed in a Vacodil® (Invar)
measuring system. The maximum
measuring range is 5000 μm. The
extremely low drift exhibited by the
system guarantees measurements
with very high repeatability, accuracy
and long-term stability for application
temperatures up to 2000°C.
Wide Temperature Range and
Exchangeable Furnaces
Six easily exchangeable furnaces are
available to cover a temperature range
of -180°C to 2000°C. This not only
provides flexibility for different appli-
cations, but also ensures the smallest
temperature gradient along the sample
for both low- and high-temperature
applications.
Motorized Pushrod and Automatic
Zeroing
The motorized pushrod and the easy-
to-move furnace make it quite simple
to insert samples, even when sample
geometries are less than ideal. The
pushrod is brought into contact with
the sample via a software command
which also automatically brings the
LVDT to a zero/central position. Should a
different starting position be required for
large expansion or shrinkage, this can
be accomplished with a simple software
command as well.
DIL 402 C
 At a Glance – The Characteristics
of the DIL 402 C vacuum
flange sample
tube sample
 Wide temperature range thermocouple
carrier
 6 exchangeable furnaces pushrod sample
 Vacuum-tight by design heating shut-off valve
 Large sample dimensions element (gas outlet)

 Adjustable contact pressure reversing

 Extremely low drift and high tube
resolution
 Various accessories for special
applications
 Coupling to evolved gas analysis
(EGA)

DIL 402 C – 3-dimensional

sectional view

front furnace
panel
flow-through
protective tube

Atmosphere – High Vacuum Adjustable Contact Pressure Control System

The vacuum-tight design of the DIL
402 C allows for careful control of
the atmosphere and pure gas condi-
tions. For example, the system can be
evacuated and back-filled with pure
inert or non-reactive gas. Static or
dynamic reactive gas atmospheres can
be applied as well.
Materials sensitive to oxygen can be
studied under pure inert gas conditions.
To provide such conditions, an evacu-
ation system (optionally available) with
a two-stage rotary pump can be hooked
up to the standard vacuum flange. For
high-vacuum requirements (10-4 mbar),
a turbo molecular pump system is
available.
In the DIL 402 C, the contact force of
the pushrod can be adjusted between
15 cN and 45 cN, and optionally
between 45 cN and 100 cN. An
almost frictionless ball-bearing design
supporting the pushrod guarantees
smooth detection of changes in sample
dimension.
Thermostatic Control
To prevent any thermal influence from
the furnace or from changes in room
temperature, the LVDT system is kept at
a constant temperature using a precise
thermostat. This guarantees repro-
ducible measurements even in the most
sensitive measuring range.
The thermal analysis system controller,
TASC 414, combines a multi-step
programmer and PID controller with a
high-resolution data acquisition system.
A Sample Temperature Controller (STC)
unit provides for excellent sample
temperature control.
Evolved Gas Analysis
The vacuum-tight design of the DIL
402 C is ideally suited for connection
to a mass spectrometer via a capillary
coupling or to an FT-IR via a transfer
line. The outgassing of additives,
organic binders and decomposition
products can thus be studied.

9
 Dilatometer 402 C – Perfect for Sophisticated Demands

Large Sample Size

The maximum sample diameter for

the standard sample holders is 12 mm.
Special fused silica, alumina and
graphite sample holders are available
for diameters up to 19 mm.

Tube-Type Sample Carrier

The tube-type sample carrier is standard for the DIL 402 C. The sample is placed
within the tube. Supports can be used for centering and to prevent direct contact
(sticking) between the sample and carrier. The sample carriers are available in fused
silica (max. 1100°C), alumina (max. 1680°C), or graphite (max. 2000°C).

Rod-Type Sample Carrier

The fused silica or alumina tube-type sample carriers can optionally be replaced with
rod-type sample carriers for ideal heat transfer to the sample. These consist of three
support rods, leaving the sample open to the heat source and the gas atmosphere.
This results in an increase in accuracy.

Sample Containers

For measurements on pastes, powders, molten metals and other material configura-
tions, special sample containers made of fused silica, alumina, sapphire or graphite
are optionally available.

10
 Technical Key Data for the DIL 402 C
Temperature range -180°C to 2000°C
 Metal: -180°C to 500°C (two versions available; closed or open to one side)
 Stainless steel: -150°C to 1000°C (with extended heating zone)
 Tube furnace: RT to 1000°C (with protective tube made of fused silica)
User-interchangeable furnaces
 SiC: RT to 1600°C
 Rh: RT to 1600°C (especially for use in glove box)*
 Graphite: RT to 2000°C
Depending on furnace, available as open or closed tubes; made of:
 Alumina
Interchangeable protective tubes
 Fused silica
 Glassy carbon
Heating rate 0.01 to 50 K/min
Temperature precision 0.1 K
 Liquid nitrogen (low-temperature furnaces)
Cooling systems  Forced air integrated in the SiC furnace and tube furnace
 Water cooling (graphite furnace)
 Inert
 Oxidizing (graphite furnace up to 1680°C with special protective tube)
Atmosphere  Reducing
 Vacuum (<10-4 mbar (10-2 Pa))
 Static and dynamic operation
 Gas flow control supplement for 1 gas path
Gas flow control options
 Mass flow controller (MFC), box for 3 gases
c-DTA® For temperature calibration and detection of endo- and exothermal effects
Measuring range 500/5000 μm
 Standard: 15 cN to 45 cN
Load at the sample
 Optionally: 45 cN to 100 cN
∆l resolution 0.125 nm/digit, 1.25 nm/digit
Sample diameter Up to 12 mm (optionally 19 mm)
 Up to 25 mm (standard)
Sample length
 Up to 50 mm (optionally for low-temperature furnaces)
 Tube-type: fused silica, alumina, graphite
Interchangeable sample holders
 Rod-type: fused silica or alumina
 Thin metal, ceramic and glass foils
 Penetration
Special sample holder systems
 Bending (especially for determination of firing stability, set made of Al2O3)
 Rod-type sample holder in combination with the humidity generator and humidity sensor
For pastes, liquids, waxes and molten metals (incl. aggressive samples) in fused silica,
Sample containers
alumina, sapphire, graphite and steel
Optional for measurements under a relative humidity of between 5% and 90%;
Humidity generator
temperature range from 30°C to 80°C

*Special glove box designs available upon request

11
 DIL 402 CD – Dual and Differential Excellence
The Dual and Differential Dilatometer DIL 402 CD – Two Instruments in One
The DIL 402 CD offers the highest level
of performance in thermal expansion
measurements. In the double sample
arrangement, the system is capable of
high sample throughput. In the differ-
ential arrangement, the system offers
calibration-corrected measurements in
one run and improved long-term drift
stability.
Design
The horizontal, vacuum-tight instrument
construction offers specific advan-
tages, especially in the dual sample
arrangement: homogeneous heating
of both samples, easy sample insertion,
and effective protection of the
measuring system by gas flow.
In addition, no convective heat transfer
takes place between the measuring
system (two high-resolution inductive
displacement transducers) and the
sample area, thus eliminating increased
drift and noise.
12
Advantages of the Double Sample
Arrangement
 Corrected tests in one run
 Compensation of drift effects for
long-term measurements
 Corrected RCS (Rate-Controlled
Sintering, Super-Res®)
Furnaces
Five easily exchangeable furnaces cover
the temperature range from -180°C to
2000°C. The forced-air, liquid-nitrogen
and water-cooled furnaces offer fast
heating and cooling times along with a
homogeneous temperature profile over
the sample.
Measurement System
The high-resolution displacement trans-
ducer (LVDT, 0.125 nm/1.25 nm/digit) is
employed in an Invar measuring system.
The maximum measuring range is
5000 μm. The extremely low drift
exhibited by the system guarantees
measurements with very high repeat-
ability, accuracy and long-term stability
for application temperatures up to
2000°C.
DIL 402 CD
 thermostatically- sample
At a Glance – The Characteristics controlled support thermocouple
of the DIL 402 CD displacement
transducer (2x) vacuum sample pushrod sample purge gas outlet
 Wide temperature range (LVDT) flange carrier (2x) (2x) furnace (FTIR, MS)
 5 exchangeable furnaces
 Two measurement positions
 Higher sample throughput
 Calibration-corrected results in
one run
 Accurately corrected Rate-
Controlled-Sintering (RCS) tests
 Adjustable contact pressure
 Extremely low drift and high
resolution
 Coupling to evolved gas analysis purge gas inlet base plate/ flow-through
control panel protective tube

Cross-sectional view of the DIL 402 CD

Atmosphere – High Vacuum Thermostatic Control

The vacuum-tight (<10-4 mbar (10-2 Pa)) To prevent any thermal influence from
design of the DIL 402 CD allows for the furnace or from changes in room
careful control of the atmosphere and temperature, the LVDT system is kept at
pure gas conditions. Measurements in a constant temperature using a precise
inert, oxidizing or reducing atmospheres thermostat. This guarantees repro-
can be performed under static or ducible measurements even in the most
dynamic conditions. sensitive measuring range.
The gas flow can be controlled by a
simple gas control supplement or a mass
flow controller system (MFC). In order to
provide pure inert conditions for oxygen-
sensitive materials, various evacuation
systems are optionally available.

The DIL 402 CD transducer system with its two LVDTs

and two motors for the pushrod movements.

13
 DIL 402 CD – Dual and Differential Excellence
Motorized Pushrod and Automatic
Zeroing
The motorized movement of the
pushrods and the easy-to-move
furnace make it quite simple to insert
samples. The pushrods are brought
into contact with the samples via a
software command which also automati-
cally brings the LVDT to a zero/central
position.
Adjustable Contact Pressure
In the DIL 402 CD, the contact force of
the pushrod can be adjusted between
15 cN and 45 cN. An almost frictionless
ball-bearing design supporting the
pushrod guarantees smooth detection of
changes in sample dimension.
Dual sample arrangement of the DIL 402 CD. The
sample thermocouple can be adjusted above the
center of the two samples.
14
Evolved Gas Analysis
The vacuum-tight design of the DIL
402 CD is ideally suited for connection
to a mass spectrometer via a capillary
coupling or to an FT-IR via a transfer
line. Outgassing of additives, organic
binders and decomposition products
can thus be studied.
Tube-Type Sample Carrier
Tube-type sample carriers are available in:
 Fused silica (max. 1100°C)
 Alumina (max. 1680°C)
 Graphite (max. 2000°C)
In addition, a special sample carrier for
measurements on thin metal, ceramic
and glass foils can be used with the
DIL 402 CD.
Sample Geometries
Various sample geometries such as thin
rods or plates can be easily measured
in the horizontal arrangement. The
system allows for measurements on
samples with a diameter of max. 6 mm
which are between 0 and 25 mm long.
In the case of sample decomposition,
the design of the transducer system
protects it from contamination.
 Technical Key Data for the DIL 402 CD
Temperature range -180°C to 2000°C
Five user-interchangeable furnaces:
 Metal: -180°C to 500°C (two versions available; closed or open to one side)
 Stainless steel: -150°C to 1000°C (with extended heating zone)
Furnaces
 SiC: RT to 1600°C
 Rh: RT to 1600°C (for use in glove box, Ar atmosphere)
 Graphite: RT to 2000°C
Depending on furnace, available as open or closed tubes; made of:
 Fused silica
Interchangeable protective tubes
 Alumina
 Glassy carbon
Heating rate 0.01 to 50 K/min
Temperature precision 0.1 K
 Liquid nitrogen (low-temperature furnaces)
Cooling systems  Forced-air integrated in SiC furnace and tube furnace
 Water cooling (graphite furnace)
 Inert
 Oxidizing (graphite furnace up to 1680°C with special protective tube)
Atmosphere  Reducing
 Vacuum (<10-4 mbar (10-2 Pa))
 Static and dynamic operation
 Gas flow control supplement for 1 gas path
Gas flow control options
 MFC gas control box for 3 gases
c-DTA® For temperature calibration and detection of endo- and exothermal effects
Measuring range 500/5000 μm
Load at the sample 15 cN to 45 cN, adjustable
∆l resolution 0.125 nm/digit, 1.25 nm/digit
Sample diameter Up to 6 mm
Sample length Up to 25 mm
 Fused silica
Interchangeable tube-type
 Alumina
sample holders
 Graphite
Special sample holder system Slotted rod for measurements on thin metal, ceramic and glass foils

Sample holder for measurements on thin foils

15
 DIL 402 E – Precision at the Highest of Temperatures
Dilatometer DIL 402 E
For dilatometer measurements in
the highest temperature range, the
versatile, modular DIL 402 E is the
instrument of choice. The design of
this instrument is based upon the well-
proven dilatometer series, but it can
be equipped to achieve two additional
upper temperature limits.
Furnaces
Two user-exchangeable furnaces
are available, allowing for a broad
temperature range and high flexibility.
Measurements can be carried out either
conventionally with thermocouple
control (up to 2000°C), or using the
optical pyrometer (up to 2400°C or
even 2800°C). The furnace can be slid
back and forth on guide rails to allow
easy access for uncomplicated insertion
or change of the sample.
16
Depending on the furnace type, various
cooling facilities (e.g., forced air or
water) are available which offer fast
heating and cooling rates along with a
homogeneous temperature profile at
the sample. The water-cooled graphite
tube furnace allows for heating rates
of up to 50 K/min and short cooling
periods to room temperature.
Design
The measuring part, with sample
holder and graphite tube furnace, is
designed horizontally and can be used
in a protected gas atmosphere up
to 2800°C. The sample and furnace
chamber can also be separated by an
Al2O3 protective tube for measurements
in oxidizing atmospheres such as air
or O2. For this configuration, the
temperature is limited to 1680°C.
Safety System
A comprehensive safety system
continuously checks the flows of
cooling water and protective gas during
the measurement. The power supply to
the furnace would immediately be cut
off if trouble should arise.
Thermostatic Control
To prevent any thermal influence from
the furnace or from changes in room
temperature, the LVDT system is kept at
a constant temperature using a precise
thermostat. This guarantees repro-
ducible measurements even in the most
sensitive measuring range.
DIL 402 E
 At a Glance – The Characteristics
of the DIL 402 E micrometer thermostatically thermo- water
screw controlled area pushrod couple sample cooling
 Widest temperature range gas vacuum
 User-interchangeable furnaces glass fibre to
pyrometer
 Highly vacuum-tight
 High accuracy up to 2800°C
 Thermocouple or pyrometer gas
operation
 Adjustable contact pressure
 Short cooling times down to RT
 Rate-Controlled-Sintering
(RCS) tests inductive insulation graphite
 Extremely low drift and high transducter heating element

resolution

Schematic of the DIL 402 E with pyrometer operation

Atmosphere – High Vacuum Pushrod and LVDT Systems Data Acquisition

The DIL 402 E can be operated under
inert, reducing, static or dynamic
atmospheres. Various vacuum pumps
are available, including turbo molecular
pumps for creating the purest of
atmospheres.
This vacuum-tight dilatometer allows
for careful control of the atmosphere
and pure gas conditions by using a mass
flow controller.
The mechanics of the pushrod and
transducer (LVDT) are not influenced by
the furnace and sample holder. They
remain at a constant temperature due
to the thermostatic control. The pushrod
can apply a load as low as 15 cN to the
sample.
The transducer’s measuring signal is
evaluated in the TA system controller.
The rapid analog-to-digital conversion
is carried out at 4 million digits and
reaches a high resolution of
0.125/1.25 nm/digit.

17
 DIL 402 E – Precision at the Highest of Temperatures
Temperature Measurement
The instrument version covering a
temperature range from 25°C to
2000°C uses a W3%Re-W25%Re
thermocouple to control the furnace
and to measure the sample temper-
ature. A special thermocouple with a
molybdenum protective sheath can be
supplied upon request.
A special supplement allows tempera-
tures up to 2400°C to be measured
using an optical pyrometer (DIL 402
E/7). In addition, a second version
(DIL 402 E/8 Pyro) allows for measure-
ments up to 2800°C also with a
pyrometer in helium atmosphere.
In the temperature range between room
temperature and 650°C (i.e., below the
working temperature of the pyrometer),
the furnace is controlled by an electronic
supplement with a ramp generator, signal
amplifier and converter.
The furnace is heated to 650°C at a
constant heating rate of 50 K/min. The
change in length is recorded beginning
at room temperature, and the corre-
lation to the sample temperature starts
at 650°C using the pyrometer.
18
Optical Pyrometer
The non-contact optical pyrometer
measures the temperature at the end
of the sample holder by means of a
lens system placed in the furnace axis. In
this way, the material that is measured
always exhibits very similar radiation
behavior to that of a black body. The
advantage to using this as the temper-
ature measurement point is that varia-
tions in the emissivity of different sample
materials and surfaces will not influence
the measurement.
The infrared radiation from the
measurement point is collected by the
optics and then transmitted through a
glass fiber to the IR sensor of the
pyrometer electronics. The sensor signals
are linearized and digitally displayed
in degrees centigrade. Simultaneously,
they are sent to the TA system controller
to be processed for temperature control
and later evaluation.
Pushrods made of alumina,
graphite and glassy carbon
 Technical Key Data for the DIL 402 E
Temperature range Room temperature to 2800°C
 RT to 2000°C (thermocouple operation) to 650°C to 2400°C (pyrometer operation)
User-interchangeable furnaces
 RT to 2000°C (thermocouple operation) to 650°C to 2800°C (pyrometer operation)
Interchangeable protective tubes  Al2O3 for tests under oxidative atmospheres up to 1680°C
for the 2400°C furnace*  Glassy carbon
Heating rate 0.01 to 50 K/min
Cooling systems Water cooling or cooling thermostat
 Inert (He > 2000°C)
 Oxidizing (graphite furnace up to 1680°C with special Al2O3 protective tube)
Atmosphere
 Reducing
 Static and dynamic operation
Vacuum <10-4 mbar (10-2 Pa)
 Gas flow control supplement for 1 gas path
Gas flow control options
 MFC gas control box for 3 gases
c-DTA® For temperature calibration and detection of endo- and exothermal effects
Measuring range 500/5000 μmmax.
Load at the sample 15 cN to 45 cN
∆l resolution 0.125 nm/digit, 1.25 nm/digit
 12 mm in thermocouple operation
Sample diameter
 6 mm in pyrometer operation
Sample length Up to 25 mm in thermocouple or pyrometer operation up to 2800°C
Exchangeable sample holders and  For 2800°C furnace: Graphite
push rods  For 2400°C furnace: Graphite, glassy carbon, alumina (<1680°C)
Sample containers for pastes, liquids and molten metals made of
Special sample holder systems
fused silica, alumina and sapphire
Accessories Sample supports and protective sleeves
* The 2800°C furnace is operated without protective tube

Protective sleeve made of graphite

19
 Dilatometer Accessories

Dilatometry Accessories

Sample Containers, Supports and Atmospheric Control

Protective Sleeves

Special sample containers allow The vacuum-tight dilatometer systems

measurements on pastes, powders,
molten metals and other material
configurations. They are made of fused
silica, sapphire, alumina or graphite.
Supports come in fused silica, Al2O3
and graphite. Protective sleeves for the
sample are available in boron nitride
(BN), aluminum nitride (AlN) and
molybdenum.
(DIL 402 C, CD, E) allow for careful
control of the atmosphere and pure
gas conditions by using a mass flow
controller (MFC). Various evacuation
systems are available to support defined,
pure atmospheres.

20

Sample Preparation
Grinding machines for the prepa-
ration of plan-parallel samples and
vernier calipers for the online input of
sample length can be ordered with the
instrument.
Additional information
See brochure: Accessories for
Thermomechanical Analysis
Calibration
For calibration of the expansion, manu-
facturer-certified standards are available.
These come in different lengths and ma-
terials (fused silica, alumina, sapphire,
steel, platinum, tungsten, and POCO
graphite).
All calibration routines are supported by
the standard dilatometer software.
getter ring
carrier
OTS® system reduces the oxygen partial pressure in
the vicinity of the sample.
Oxygen Trap System (OTS®) for the
DIL 402 C
The presence of residual oxygen can
be critical in certain applications (e.g.,
metals, metal alloys) because possible
oxidation of the sample would lead to
undesired results and false interpre-
tations. The OTS® system allows for
effective reduction of the oxygen partial
pressure in the vicinity of the sample. A
ceramic substrate bearing a getter ring is
mounted on the sample carrier or in the
sample carrier tube. The residual oxygen
content remaining after evacuation is
thereby almost entirely eliminated
(< 1ppm).
21
 Dilatometer Software – Software Specialties
Proteus® Software for Dilatometry
All dilatometers run under Proteus® software on a Windows® operating system. User-
friendly menus combined with automated routines make Proteus® very easy to use
while still providing sophisticated analysis. The Proteus® software is licensed with the
instrument and can of course be installed on other computer systems.
Key Features of the General Software
 Fully compatible with other
Microsoft® Windows® programs
 Multi-tasking: simultaneous 
measurement and evaluation
 Multi-moduling: operation of
different instruments with one com-
puter 
 Context-sensitive help system
 Labeling: input and free placement
of text elements 
 Storage of the analysis results and
status for later restoration and 
continuation with analysis (original
file remains)
 Storage of c-DTA® curves which
can be directly accessed, as ‘true’ 
measurement files
 Results by e-mail
 Freely configurable ASCII import, 
import of measurement files for
coupled methods (QMS and FT-IR
22
data); data is linked to the DIL
temperature curve
Export of graphics with evaluation
results to clipboard or to common
formats such as EMF, PNG, BMP, JPG,
TIF or PDF
ASCII file export of the raw data
and/or the corrected measurement
data for data processing with more
extensive analysis programs
Data can be exported into Excel®-
compatible CSV-format
Multiple-window technique for
clear presentation and evaluation
of measurement curves or graphical
excerpts in multiple windows
Formatting of the results,
measurement values, and axis labels
optionally in technical format or as
scientific notation
Application languages: English,
German, French, Russian, Chinese
Key Features of the Measurement Software

 Repetitive measurements with  Loop programming: insertion, dele-

minimum parameter input
 Temperature program: up to 256
programmable temperature
segments 
tion, and annexation of temperature
segments, even in already existing
temperature programs
Fast definition for furnace heating

 Programming while the

measurement is running

 Monitoring of all MFC gas flows

(protective and purge gas)

RCS test to achieve a

constant shrinkage rate

23
 Dilatometer Software – Software Specialties
Key Features of the Evaluation Software
 Presentation/evaluation of the 
absolute (dL in μm, corrected or raw
data) or relative length change curve
(dL/Lo or dL/Lo in %)
 Calculation of 1st and 2nd derivative 
 Correction of the measured length
change either via sample holder
expansion or using a calibration run 
 Parallel curve offset (offset
correction) 
 Corrections as per ASTM (for
samples and calibration standards
of identical length) or as per DIN (for
samples and calibration standards of
not necessarily identical length)

 Correction possibility which allows
the reference temperature Tref (Lo)
to be shifted to values other than 
20°C (DIN)

 Offset correction for start value
and/or initial sample length can be 
carried out with offsets manually
defined, automatically read from
raw data or by graphical 
extrapolation
 Calculation/determination of
individual values and graphical
presentation of the technical and/or 
physical expansion coefficient
24
Possibility of extrapolating the 
coefficient of technical expansion
(CTE) to reference temperatures
between 20°C and 50°C 
Comparative analysis of up to 64
curves or segments from the same or
different measurements
Value determination on a single
curve or a curve family 
Semi-automatic routines for
determination of characteristic
temperatures of the length change
curve, its derivative and/or the curve
of the expansion coefficient, peaks;
simultaneously on multiple curves 
Smoothing of the measuring curves
with adjustable filter factors
Glass transition evaluation
Evaluation of sintering steps
Search for temperature for a given
percentage length change
Automatic softening point detection
(programmable, measurement stop
or jump into the next segment of the
temperature program)
Connection of segments by spline
interpolation
Snapshot: Online evaluation of the
running measurement
Comparative evaluation and
presentation of various signals and
methods (TGA, DSC, DTA, STA, DIL/
TMA, DMA, mass spectrometry and
FT-IR) in collective graphics or
evaluation windows
Macro-recorder for creating
analysis macros (“learning by doing”)
and for the automatic evaluation
of measurement series. Results
can additionally be annotated with
threshold values for quality control
Expanded evaluation function for
imported mass spectrometer data
from coupling with QMS 403 C
Aëolos®. The MS data is linked to
the dL/Lo data time-wise and
temperature-wise, incl. 3D
presentation together with
temperature and dL/Lo-signal
 Length/µm

98

94

90
Model: Three -Step Reaction A B C D

86 st
1 step: diffiusion
nd
2 step: n -th order
rd
82 3 step: n -th order

Correlation coefficient: 0.9999

78

200 400 600 800 1000 1200 1400

Temperature/°C

Investigation of the sintering behavior of Aragonite (CaCO3) on the base of a 3-step reaction model using the
Thermokinetics software

Software Specialties

 Patented c-DTA®  Peak Separation  Density Determination

The optionally available software
add-on c-DTA® (“calculated DTA”)
allows for simultaneous analysis
of length changes, endothermal/
exothermal effects, and temperature
calibration.
 Rate-Controlled Sintering (RCS) 
The RCS software add-on is a rate-
controlled temperature guidance for
optimization of the sintering process.
Three different modes are included:
start/stop, stepwise isothermal, and
dynamic heating rate.
For accurate separation and This optional program add-on
evaluation of overlapping effects, this supports determination of the
optional software program can also density of solid samples as a function
be used for further thermoanalytical of temperature beyond the melting
and gas analysis measurements such temperature. The software includes
as DSC, TGA, QMS, FT-IR, etc. volume expansion and can also be
used for liquids and pastes.
Thermokinetics
This optional software package
provides the basis for advanced
characterization of reactions and
kinetic analysis. It also provides
predictions of the process.

25
 Performance and Low-Temperature Applications

Unmatched Reproducibility
1.60
1 Run (Heat)
st

1.40 1st Run (Cool) Here, a sapphire sample was measured

2nd Run (Heat) twice in the direction of the c-axis
1.20
2nd Run (Cool)
during heating and cooling between
Thermal Expansion / %

1.00
room temperature and 1550°C. The
0.80 heating/cooling rates were 5 K/min.
0.60 The atmosphere was helium. The
comparison clearly demonstrates the
0.40
outstanding reproducibility of the DIL
0.20 402 C. As can be seen, the heating and
0.0 cooling data are almost identical. The
0 200 400 600 800 1000 1200 1400 1600
difference between the four test results
Temperature / °C
is typically less than 0.3%.
Thermal expansion of a sapphire sample during heating and cooling cycles.

2.25
Outstanding Accuracy
Platinum/
Copper 10 % Rhodium In this example, the linear thermal
1.75
Aluminum expansion behaviors of pure aluminum,
Thermal Expansion / %

Rhodium
copper and electrolytic iron are
1.25 Platinum
compared with literature values. Clearly
Iron there is excellent agreement. The differ-
0.75 ences are generally less than 1%. In
addition, Pt/10%Rh was compared with
Literature values
0.25 (error bars: 3 %) the values for platinum and rhodium.
Iron The test results are in the expected
-0.25 range between the pure metals.
-250 0 250 500 750 1000 1250 1500 1750
Temperature / °C

Thermal expansion of metals compared to literature values, measured with

the DIL 402 C.

Excellent CTE Repeatability –

Glass Ceramic
4

ZERODUR® is a glass ceramic produced

Thermal Expansion / 10-3 %

2
by SCHOTT, Germany. It is designed for
Temp. / °C T. Alpha / 1/K zero thermal expansion around room
0.0 ... 50.0 0.014E-06
0 temperature. This material is often
Temp. / °C T. Alpha / 1/K
0.0 ... 50.0 0.011E-06 used for high-performance terrestrial
-2 telescopes. The figure shows the linear
Literature: Temp./ °C T. Alpha / 1/K thermal expansion between -150°C
0.0 ... 50.0 0.00 +0.05E-06
-4
and 100°C. The sample was measured
twice at a heating rate of 3 K/min in a
-150 -100 -50 0 50 100 helium atmosphere. The measured CTEs
Temperature / °C
between 0°C and 50°C are in excellent
High-precision measurements in very low temperature ranges are easy with the agreement with the literature values
DIL 402 C – even for materials with zero thermal expansion. (SCHOTT brochure) for this material.

26
Fiber-Reinforced Polymer

A two-dimensional fiber-reinforced 1.5

polymer was measured in and perpen-
dicular to the fiber orientation. Both
Thermal Expansion / %
1.0 ⊥ :
tests were carried out between -100°C Temp./°C T. Alpha 1/K
0.0 ... 50.0 86.285E-06
and 100°C. In the fiber direction, the 0.5
CTE is strongly reduced by the influence
of the fibers. Perpendicular to the fibers, 0
their influence is small; the CTE is in ≡ :
Temp./°C T.Alpha 1/K
the typical range for the polymer matrix. 0.0 ... 50.0 3.427E-06
-0.5
Additionally, the glass transition of the
polymer is clearly visible in the perpen- -100 -50 0 50 100
Temperature / °C
dicular direction. This example shows
that fiber reinforcement has a signif- The DIL 402 C is also suitable for tests on polymer materials.

icant effect on the thermal expansion

behavior.

Roof Tiles
0.10
-1.8 °C
A fired roof tile was exposed to water
for 24 hours and then tested with the 0.05 Heat
DIL 402 C between -20°C and 25°C.
Thermal Expansion / %

Upon cooling, the water in the pores

of the ceramic body freezes at -7°C. 0.0
Cool
(The low freezing temperature is due to -7.2 °C
super cooling of the water.) The freezing
-0.05
causes an increase in the sample length
of nearly 0.08%. Upon heating, the ice
begins melting at -2°C, resulting in a -0.10
-20 -15 -10 -5 0 5 10 15 20 25
shrinkage of the sample. The irreversible Temperature / °C
length change of the sample after cyclic
cooling and heating may be partially The possibility of running controlled heating and cooling cycles in the DIL 402 C
results in a better understanding of the material’s behavior.
due to cracks.
The use of this roof tile type in certain
climate zones should be given careful
consideration prior to installation.
Freezing effects will reduce its lifetime.

27
 High-Temperature Applications

Determination of the Softening

Softening point:
dL/Lo / % 611,2°C Point – Quality Control
614,0°C
613,6°C

0.600
Coefficients of thermal expansion
Glass transition
temperature: (CTE), glass transition temperatures and
549,4°C
0.500 554,5°C
softening points are crucial parameters
554,7°C for characterization of glass materials.
0.400 This plot shows three tests on the same
Temperature CTE / 1/K
20 ... 300°C: 8.918E-06
type of glass but from different batches.
0.300 20 ... 300°C: 8,902E-06 It can clearly be seen that the coeffi-
20 ... 300°C: 8.910E-06
cients of the thermal expansion are
0.200
in good agreement within the instru-
ment’s uncertainty boundaries. The
0.100
glass transition temperatures and the
softening point of sample no. 3 (blue
0.000
100.0 200.0 300.0 400.0 500.0 600.0 curve) show lower values, indicating
Temperature / °C a slightly different composition. The
Glass samples of the same type but from different batches show slight deviations in composition which can thermal expansion tests were, of course,
be well observed in the softening point (DIL PC measurement). switched off automatically by the
softening point detection in order to
protect the system from contamination.

Brick Clay
Thermal Expansion / % Phys. Alpha 10-6 1/K
2
Brick and tile products contribute
400
1 878.8 °C
-0.26 %
Sintering significantly to the development and
98.3 °C 576.5 °C quality of construction projects all
0
200 over the world. This figure of a brick
-2.59 %
-1 Dehydration 587.3 °C clay measurement exhibits a step in
the thermal expansion curve (red) at
-2 0
118.7 °C 576°C which can clearly be seen in the
919.8 °C
-3 Quartz formation and -2.02 % physical α-curve as a peak at 587°C.
dehydration of clays 1305.9 °C
-200 This change in thermal expansion is
-4
1116.3 °C due to the overlapping dehydration of
-5 1250.9 °C clays and phase transition of quartz.
-400
Melting Above 800°C, sintering starts. During
-6
200 400 600 800 1000 1200 1400
the sintering process, a melting effect
Temperature / °C can be observed which could be due
to an inorganic component of the raw
Dehydration, quartz transition and sintering of a brick clay measured with the DIL 402 C material.

28
High Sample Throughput –
Fired Tiles with Different Expansion dL/Lo / %

Behavior 0.8

0.7
Two colored tiles were simultaneously
red tile
0.6
heated at 3 K/min to 1100°C using the 971.6 °C
DIL 402 CD. The curves for the relative 0.5
brown tile
expansion of these fired tiles show 0.4 567.0 °C

significant differences in expansivity and 0.3

567.0 °C
quartz content (> 567°C).
0.2
expansion difference
The powerful NETZSCH Proteus ® 0.1 580.0 °C

measuring and evaluation software 0

allows a graphic display of the
200 400 600 800 1000
expansion difference in a separate curve. Temperature / °C

DIL 402 CD measurement on two different fired tiles. The dual sample arrangement ensures a high sample
throughput for routine applications.

29
 High-Temperature Applications

Comparison Between an Already

dL/Lo/% dL/dt/(%/min) Sintered Zirconia and Its Green Body
Temperature CTE/1/K
5.00
30 ... 500°C 10.760E-06 Sintered Zirconia
30 ... 1000°C 11.511E-06 0.40
30 ... 1500°C 12.042E-06 969.9°C Zirconia is used as a refractory material
0.00 0.20 in insulation, abrasives, enamels and
Binder burnout Green Body
ceramic glazes, but it is also used in
0.00
389.4°C
-20.07% the manufacture of subframes for the
- 5.00
-0.20 construction of dental restorations.
This plot compares an already sintered
- 10.00 -0.40
Sintering material with a zirconia green body.
-0.60 While the sintered material shows a
1402.7°C
- 15.00 nearly linear thermal expansion, the
-0.80
green body still exhibits the binder
- 20.00 -1.00 burnout at 389°C and sintering which
200.0 400.0 600.0 800.0 1000.0 1200.0 1400.0 1600.0 starts at 970°C. The highest sintering
Temperature /°C rate is achieved at 1403°C (dL/dt curve).
With the DIL 402 CD, comparative measurements are easy. The comparison between the green body and
sintered zirconia is demonstrated here.

30
Silicon Nitride
1200.6 °C
Because of its excellent thermal and 0 -1.05 % 0.10
mechanical properties, silicon nitride 1424.5 °C
-2 -0.0
is used increasingly often in high-tech
applications (e.g., valves in automobile -4 1278.9 °C
engines). Of course, the properties of -0.10
Thermal Expansion / %

1789.5 °C

Rate of Expansion / %
-6
the final parts are heavily influenced
by the production/sintering process. -0.20
-8 -14.33 %
Depicted in this plot are the thermal
-10 -0.30
expansion and rate of expansion of a
1511.0 °C
silicon nitride green body. The sintering -12
-0.40
step starting at 1201°C is due to the
influence of sintering additives. The -14 1760.3 °C
-0.50
major shrinkage step occurred at -16
1424°C (extrapolated onset). The effect
-0.60
above 1760°C is most probably due to 0 500 1000 1500 2000
the evaporation of additives. Temperature / °C

DIL 402 C allows measurements under well-defined atmospheres up to 2000°C. This allows observation of
the complete sintering behavior of many ceramic materials.

Natural Carbon
Thermal Expansion / %
The reduction of impurities in natural
2602 °C
carbon can be seen during heating
under a helium atmosphere. The 2.00
sintering behavior changes during
reduction, which can be observed 2165 °C
1.50
in the effects between 1150°C and
1600°C. After these effects, the thermal
expansion increases almost linearly up 1.00
to 2600°C. Reliable measurements can 1146 °C 1441 °C
be performed at the highest tempera-
tures with the DIL 402 E up to 2800°C. 0.05 1602 °C

The temperature is monitored with a

pyrometer. 0.0
1000 1500 2000 2500
Temperature / °C

The purest of gas atmospheres and highest of temperatures can be achieved with the DIL 402 E.

31
 c-DTA® and Other Specialties – Deep Insight into Material Behavior

c-DTA® Feature

The c-DTA® calculation is a mathe- can be detected. Therefore, more

matical routine based on the temper-
ature measurement at the sample.
Transitions associated with exo- or
endothermal effects, of course, slightly
influence the temperature change
during dynamic heating or cooling. By
comparing the measured temperature
change of the sample with a theoretical
one, these exo- or endothermal effects
detailed insight into the material behavior
during expansion, shrinkage and
sintering can be obtained. If a calibration
run on a standard sample is carried out
prior to the sample run, this will also be
taken into consideration in the calcu-
lation process.
In addition, c-DTA® is used for temperature
calibration of the dilatometer systems.

Production of a Cordierite Ceramic

dL/dt /(%/min)
dL/Lo / % c-DTA / K
481.4 °C 894.1 °C exo
20 0.05
0.000
522.2 °C -0.891 %
10 0.00
296.2 °C
348.1 °C
-0.500 190.5 °C 517.3 °C
-0.05
0
218.3 °C
-1.000 273.0 °C 966.6 °C -0.10
-10
Oxidation and burnout
of organics Sintering and -0.15
-1.500
formation of the -20
cordierite phase
-0.20
-2.324 %
-2.000
-30
1412.8 °C -0.25

-2.500 -40
-0.30
356.8 °C
1178.4 °C -50
-3.000 -0.35
200.0 400.0 600.0 800.0 1000.0 1200.0 1400.0
Temperature / °C

Simulation of the production process of cordierite by using the DIL 402 PC in combination with c-DTA®
(sample length 24.83 mm, heating rate 5 K/min)

During the production of cordierite
(an alumina-silica ceramic carrier for
catalysts), various raw materials are
ground and mixed to form a green
body. This plot shows the simulation
of the firing process of a cordierite raw
material. Under oxidizing atmospheres,
the organic additives are burnt out.
Using the c-DTA® software, the burnout
of the additives can be observed as an
exothermic effect between 190°C and
525°C (blue curve). At high tempera-
tures (> 890°C), sintering starts and the
cordierite phase is formed.

32
Volumetric Expansion and Bulk Density of Powders, Pastes and Liquid Metals

Dilatometers are generally used for liquid metals can now be accurately
measurement of solids. However, determined. Knowledge of the thermo-
by using the liquid metal containers physical properties such as volumetric
(made of fused silica, graphite, alumina expansion and bulk density of metals
or sapphire) and a special software during melting is of paramount impor-
extension, the volumetric expansion and tance for the simulation of casting
bulk density of powders, pastes and processes using finite element models.

Superalloy – Inconel 718

8.2
12 The volumetric expansion and bulk
1346°C
8.1 density of a nickel-based superalloy
10 (Inconel 718) were measured in the
8.0
DIL 402 C solid and liquid regions as well as in the
3.1%
Sample: Inconel 718
Sample length: 12 mm
“mushy” zone. A sapphire container
Volumetric Expansion / %

7.9
8 Sample holder: Sapphire
was employed for this test. The
Density Change / g/cm3

Atmosphere: Helium 1292°C

Heating rate: 5 K/min
7.8
influence of the container on the result
6
was corrected by the NETZSCH Density
7.7 Determination software. The onset of
melting of the sample was detected
4
7.6 at 1292°C. The melting process was
finished at 1346°C. The volume change
2
7.5 during melting was 3.1%. Since the
room temperature bulk density and
7.4 thermal expansion were known, it
0 was possible to calculate density as a
7.3
function of temperature.
0 200 400 600 800 1000 1200 1400
Temperature / °C

The NETZSCH Density Determination software allows calculation of the density as a function of
temperature based on the thermal expansion.

33
 c-DTA® and Other Specialties – Deep Insight into Material Behavior

Cast Iron – Volume and

Density Change dL/Lo /% Completely molten T. Alpha *10-6 /K-1
7.00
dL/Lo /% Completely End:
molten
1370 °C
T. Alpha *10
60 /K
-6 -1
6.00
Cast iron is a ferrous alloy which has 7.00
End: 1370 °C
been heated until it liquefies, and is 5.00 60
6.00 50
then poured into a mold to solidify. 4.00
5.00 Onset: 1334 °C
3.00 50
4.00 40
In this plot, simulation of the expansion Onset: 1334 °C
2.00
behavior during the casting process of a 3.00
1.00 40
cast iron sample was realized by using a 2.00 30
Melting
sample container made of Al2O3. Nearly 0.00
1.00
a constant expansion behavior (dL/L0) 30
-1.00
0.00 Tref.: 50 °C
Melting 20
was observed until melting of the -2.00
sample at 1334°C (extrapolated onset). -1.00
Tref.: 50 °C 20
200 400 600 800 1000 1200 1400
During melting, a big leap is monitored -2.00 Temperature /°C
for the expansion dL/L0 and the 200 400 600 800 1000 1200 1400
technical expansion coefficient α. The Temperature /°C
Measurements on a cast iron sample from the solid state into the liquid phase
sample is completely molten at 1370°C Created with NETZSCH Proteus software

(extrapolated endset).
Created with NETZSCH Proteus software
Density /(g/cm^3) dV/Vo /%
The volumetric expansion and temper-
14.0
ature-dependent density change were Density /(g/cm^3) dV/Vo /%
calculated using the software module 7.800 12.0
14.0
Density Determination. During melting, Density Onset: 1331 °C
10.0
12.0
the sample experienced an expansion 7.800
7.600
step of more than 4% within a temper- Density Onset: 1331 °C 8.0
10.0
ature difference of 40°C. 7.600
7.400 6.0
8.0

7.400 4.0
6.0
7.200
Volume Onset: 1331 °C
2.0
4.0
7.200
7.000
Volume Onset: 1331 °C
0.0
2.0

7.000 200 400 600 800 1000 1200 1400

Temperature /°C 0.0

200 400 600 800 1000 1200 1400

Temperature /°C

Density determination of a cast iron sample

34
Dilatometry under Humidity

For the DIL 402 C, a humidity generator Measurements in a humid atmosphere

is available for measurements under a
relative humidity of between 5% and
90% in the temperature range from
30°C to 80°C.
are carried out with a rod-type sample
holder for optimum access of the humid
atmosphere to the sample surface.
In place of the standard rod-type sample
holder, a special rod-type sample holder
with a humidity sensor is available.

Influence of Humidity on a Polymer

dL/µm
Here, a polymer sample (length 14
11.8 mm) was measured with the
DIL 402 C connected to the humidity 12

generator. The temperature was kept

10
constant at 55°C. The atmosphere was
4.3 µm
preset to nitrogen with 70% humidity.
8
After switching on the humidity
generator, the sample immediately 6
expands in two steps. After 200 min,
7.3 µm
the humidity generator is switched 4

off and the sample begins drying. The

2
drying process can be observed in the
200.0 400.0 600.0 800.0 1000.0
subsequent shrinkage of the sample.
Time/min
However, even after 15 h of the drying
process, the sample does not shrink
back to its initial length. DIL 402 C measurement on a polymer under humid conditions up to 200 min

35
The NETZSCH Group is an owner-managed, internationally operating technology
company headquartered in Germany.

The three Business Units – Analyzing & Testing, Grinding & Dispersing and Pumps &
Systems – provide tailored solutions for highest-level needs. Over 2,500 employees
at 130 sales and production centers in 23 countries across the globe guarantee that
expert service is never far from our customers.

When it comes to Thermal Analysis, Adiabatic Reaction Calorimetry and the

determination of Thermophysical Properties, NETZSCH has it covered. Our 50 years
of applications experience, broad state-of-the-art product line and comprehensive
service offerings ensure that our solutions will not only meet your every requirement
but also exceed your every expectation.

NGB · DIL · EN · 1000 · 1012 · LH · Technical specifications are subject to change.

NETZSCH-Gerätebau GmbH
Wittelsbacherstraße 42
95100 Selb
Germany
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