Thermal analysis

Thermal analysis is a general term defining a technique used to analyze the time and temperature at which physical changes occur when a substance is heated or cooled.

Each technique is defined according to the types of physical changes being analyzed. When evaluating material characteristics, it is necessary to use different techniques or a combination of multiple techniques depending on the purpose.

At MMK we have the follwing instruments to use for thermal analysis.

 

Heat flow DSC for low temperature range -170 -600 °C with oxidizing or inert atmosphere (Ar, N2). Heating rates 0.001 K/min to 500 K/min.Temperature and enthalpy calibrations can be done up to 6 standard materials. 

Capabilities:

Heat capacity (Cp) measurements and temperature modulated DSC runs, normal working temperature range -70-600 °C with liquid nitrogen down to -170 °C, other gases can be discussed such as CO2, MACAL provides Aluminium or Aluminium oxide cups with lid.

Examples: 

Phase transitions, adsorption, crystallisation, glass transformation, Impurity measurements, Heat capacity, etc
 

 

Simultaneous Heat flow DSC and TG instrument for high temperature applications. Temperature range room temperature up to 1600 °C with vacuum (10-4 mbar1), oxidizing or inert atmosphere (Ar, N2). SiC furnace does not allow heat capacity measurements. Heating rates 0.001 to 50 K/min

Capabilities

DSC/TG sensor, TG sensor, Temperature and enthalpy calibrations can be done up to 6 standard materials. Other gases can be discussed such as CO2, oxygen trap for residual oxygen, balance resolution 0.1 μg, maximum sample load 35000 mg (incl. crucible), MACAL provides Al2O3) cup, with users then being responsible for the intactness of the cup.

Example

Phase transitions, adsorption, crystallisation, glass transformation, Impurity measurements, heat capacity, etc

 

A relatively simple hung down TG for thermo-gravimetric measurements from room temperature to 950°C (max. 1000 °C). Measurements can be made in neutral and oxidizing gas atmospheres. However, it is not possible to evacuate the sample container and the atmosphere is simply established by flushing before the measurements.

Sample weights can be 1-30 mg, with a weight sensitivity reaching 0.1 µg. Al2O3 cups are used (Pt cups with stir-up are available), cup is attached to a hang-down Ni-Cr wire. The temperature is measured by a chromel-alumel thermo-couple placed below the position of the Pt cup.

Capabilities/Accessories

The accuracy of the measured temperature is limited, but can be improved by a two-point temperature calibration using suitable Curie point standards. The small, Pt wound micro-furnace allows rapid heating and cooling rates, up to 200°C/min. The system is controlled via a computer and a program written in DOS.

MACAL keeps a few sets of cups available and sets of weights and Curie point standards exist for calibrations of weight and temperature, respectively.

Examples of use: decomposition, oxidation, carbonization, etc

 

 

Thermal gravimetric instrument TA Instruments Discovery is a state-of-the-art TG of the hung-down wire type operating from RT to 1200°C (Pt cups to 1000°C) at oxidizing or neutral (Ar, N2) conditions.

Capabilities/Accessories

The IR furnace provides for regulated heating rates up to 500°C/min and ballistically 1000°C. A 4-gas input gas delivery module for mixing or changes gases, auto-sampler, modulated TG and HiRes TG. Typical sample weights are 0.5-2 mg, with a weight sensitivity of 0.1 µg. The TRIOS software can be down-loaded for free from the TA Instruments home-page. TG/MS coupling to a Pfeiffer Thermostar MS
Larger research groups are recommended to purchase their own Al2O3 or Pt cup. MACAL provides Pt (Al2O3) cup, with users then being responsible for the intactness of the cups. Other gases can be discussed such as CO2.

Examples: decomposition, oxidation, carbonization, adsorption, etc

 

A quadrupole mass spectrometer (MS), the Pfeiffer Omnistar GSD 320, is a bench-top instrument. The MS and the Discovery TG can be started at the same time by a trigger. 
The MS data can be collected in two basic ways; either all 200 amu channels are scanned consecutively for a period of time, to find signals of interest, or a selected number of channels are scanned, giving a higher sensitivity for each channel.

Capabilities:

Detecting 1-200 amu. The detection limit is <1 ppm for the C-SEM detector and <40 ppm for the Faraday cup. It is controlled by the software Quadrera.
 

MMK User

 

No assistance (SEK)

Operator assistance (SEK)

DSC 100/h 200/h
STA 100/h 200/h
TGA 100/h 200/h
MS 100/h 200/h

 

Academic user (not MMK)

 

No assistance (SEK)

Operator assistance (SEK)

DSC 200/h 400/h
STA 200/h 400/h
TGA 200/h 400/h
MS 200/h 400/h

 

Commercial user

DSC Full cost coverage, including operator. Contact us for quote.
STA Full cost coverage, including operator. Contact us for quote.
TGA Full cost soverage, including operator. Contact us for quote.
MS Full cost soverage, including operator. Contact us for quote.

For scheduling the training of the instrument contact the manager

User training, all fees in SEK

Instrument

MMK user    

External academic user 

Commercial users          

DSC 250/h 500/h 1000/h
STA 250/h 500/h 1000/h
TGA 250/h 500/h 1000/h
MS 250/h 500/h 1000/h

 

 

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