Thermal analysis

Thermodynamic Characterization and High-Temperature Dynamics: Quantifying Phase Transitions, Melt Viscosity, and Thermal Expansion up to 1700°C

The Thermal Analysis Laboratory forms the basis for all high-temperature experimentation on natural and synthetic materials. Thermal analyses are a standard procedure in material science as they provide a fundamental characterisation of the material properties, a matter which is of great importance in geosciences.

Differential Scanning Calorimetry

Room
C 014
Contact person
Kai-Uwe Hess
Device
Netzsch DSC 404 C - Differential Scanning Calorimetry
Working temperature
room temperature - 1500 °C
Gas flow
Argon (5.0) at 25 cm3/min

© Kai-Uwe Hess

Differential Scanning calorimetry is a frequently used method in geosciences. Here, we measure the thermodynamic properties of an unknown sample compared to a reference material as a function of temperature. It is thereby possible to study the thermal history of geomaterials, i.e. volcanic glasses.

This Differential Scanning Calorimeter (DSC) coupled to a ThermoGravimetric Analyser (TGA) can be used to determine 1) the heat capacity of material, 2) the glass transition, 3) phase changes (e.g., melting, crystallisation, crystal structure transitions), 4) weight gain/loss (e.g., hydration, dehydration, gas exolution, oxidation, decarbonation), and 5) sintering conditions. This system is coupled to a water vapour supplier to allow measurements in water vapour atmosphere as well as in traditional Ar or N atmospheres. Four furnaces are available to allow determination with a range of conditions:

Pt furnace: up to 1500 °C and heating up to 25 °C/min.
High-speed Pt furnace: up to 1250 °C and heating up to 3500 °C/min (linear heating rate up to 1500 °C/min).
Water-vapour atmosphere furnace: up to 1250 °C and heating up to 25 °C/min.
Si-C furnace: up to 1550 °C and heating up to 40 °C/min.

Room
C 015
Contact person
Kai-Uwe Hess
Device
Mettler-Toledo Flash DSC 2+ - Differential Scanning Calorimetry
Working temperature
room temperature - 1000 °C
Gas flow
Argon (5.0) at 25 cm3/min

Mettler-Toledo Flash DSC 2+ - Differential Scanning Calorimetry | © Kai-Uwe Hess

Fast Differential Scanning calorimetry is a frequently used method in geosciences. Here, we measure the thermodynamic properties of an unknown sample compared to a reference material as a function of temperature. It is thereby possible to study the thermal history of geomaterials, i.e. volcanic glasses. The sample size is here smaller than 80 micrometers, which allow to apply heating rates of up to 10000 K/s.

Thermomechanical analyser

Rooms
C 014
contact person
Kai-Uwe Hess
type
2x Thermomechanical analyser (TMA) 402F1 Hyperion (Netzsch GmbH)
Range of experimental parameters
Temperature: <1550 °C (up to 1000 °C/min)
Sample length: <30 mm
Sample diameter: <10 mm
Measuring range: +/- 2.5 mm
Length change resolution: 0.0125 nm
Compression force: 3mN-3N
ension force: 3mN-3N
Modulated force: up to 1 Hz
Force resolution: <0.01 mN
Vacuum pressure: <10-4 mbar

© Kai-Uwe Hess

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Quadrupole mass spectrometer

Room
C 015
Contact person
Kai-Uwe Hess

This apparatus can be used to determine 1) the expansion coefficient, 2) the expansion strain rate, 3) the viscosity of liquids (via the micropenetration technique), and 4) to assess the rheological/mechanical properties of magma and rocks a) in compression, b) in tension, and c) during oscillation. Measurements are traditionally run in Ar or N atmospheres. This high-accuracy dilatometric system is equipped with double furnace hoist to accommodate several furnaces simultaneously, currently:

  • Pt furnace: up to 1500 °C and heating up to 25 °C/min.

  • Si-C furnace: up to 1550 °C and heating up to 40 °C/min.

Simultaneous Thermal Analyser

Rooms
C 318
Contact person
Kai-Uwe Hess
Device
Simultaneous Thermal Analyser (STA) 449C Jupiter (Netzsch GmbH) combined with Differential Scanning Calorimetry and Thermogravity
Working conditions
· Sample type: powder, disks, chips
· Sample weight: <5 g
· Sample volume: <5ml
· Weight resolution: 25 ng
· Vacuum pressure: <10-4 mbar
Working temperatures:
RT to 1600°C
Gas flow
Argon (5.0) at 25 cm3/min

© Kai-Uwe Hess

The STA is a combination of a DSC and a thermogravimetric instrument. Besides heat capacity measurements one is able to study mass changes of a sample material, as a function of temperature with time, and additionally of pressure and gas composition.

Rooms
C 318
Contact person
Kai-Uwe Hess
Device
Mettler-Toledo TGA/DSC 3+ - Simultaneous Thermal Analysis (combined Differential Scanning Calorimetry & Thermogravimetry) and EGA
Working temperatures:
room temperature to 1300°C
Gas flow
Argon (5.0) at 25 cm3/min

Mettler-Toledo TGA/DSC 3+ - Simultaneous Thermal Analysis (combined Differential Scanning Calorimetry & Thermogravimetry) and EGA | © Kai-Uwe Hess

The STA is a combination of a DSC and a thermogravimetric instrument. Besides heat capacity measurements one can study mass changes of a sample material, as a function of temperature with time, and additionally gas composition by a gas mass spectrometer.

Optical Dilatometry

Room
C 328
Contact person
Dirk Müller, Yan Lavallée
Hesse Instruments EM301-M16
· sample size: up to 5x5x5 mm
· max. sample temp. 1500 °C
· max. heating rate 80 K/min
· can be purged with Ar or N2
DataPhysics OCA 25 – HTV 1800
· sample size: up to 10x10x10 mm
· max. sample temp. 1800 °C under atmospheric pressure / 1450 °C at 10-5 mbar
· max. heating rate 5 K/min
· can be operated under vacuum (down to 10-5 mbar) or purged/filled with Ar or N2
· measurement range of contact angle: 0-180° (+/-0.1° resolution)
Optical Dilatometer

© Antony Lamur

Through optical dilatometry, the heating and cooling behavior of solid materials (drill cores, powders, chips, etc.) can be investigated based on 2D-images. Questions of interest can be related to thermal expansion, sintering, melting and spreading, softening, foaming and contact angle analysis of the sample.

Both available instruments consist of a light source, a horizontally mounted tube furnace and a camera. Samples of interest need to be placed on an inert substrate (e.g. alumina plate) and loaded from the side (see below for possible sample sizes). Data reduction (shape analysis) can be done through specific software. All data can be exported in ACSII-format for further evaluation.

Dilatometry

Room
Contact person
Kai-Uwe Hess
Access regulations
Device
NETZSCH DIL 402C - Pushrod Dilatometry in horizontal geometry

© Kai-Uwe Hess

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