LABORATORY OF MICROCALORYMETRY (L-5)
Authorisation:
Accredited activity is defined in the Scope of Accreditation No. AB 120
Address:
Aleksander Krupkowski Institute
of Metallurgy and Materials Science,
Polish Academy of Sciences,
25, Reymonta Str., 30-59 Kraków,
phone: (48)(12) 295 28 00,
fax: (48)(12) 295 28 04,
Head of Laboratory:
Tomasz Czeppe, PhD ( Adres poczty elektronicznej jest chroniony przed robotami spamującymi. W przeglądarce musi być włączona obsługa JavaScript, żeby go zobaczyć. )
Experts:
Grzegorz Garzeł, PhD, Eng.
Marek Kopyto, PhD, Eng.
Anna Wierzbicka-Miernik, PhD
Tomasz Gancarz, MSc, Eng.
The laboratory performs measurements on two differential scanning calorimeters:
I. Differential Scanning Calorimeter (DSC) TA Instruments, model 910
II. Differential Thermoanaliser (DTA) TA Instruments, model 1600
Description of the equipment:
DSC-Microcalorimeter is designed to carry out precise measurements of temperature and heat input or output during phase transformation or the Cp of a material. The TAInstruments calorimeter is a „heat flux” type calorimeter.
The apparatus works in the temperature range from –200 to +700oC in argon or nitrogen protective atmosphere, which can be additionally purified. It may be applied both to “continuous heating” and isothermal measurements. It may also be used to observe crystallization processes during cooling at different rates, or to realize thermal cycling of a sample. Precision of measurements depends on the instrument calibration. Moreover, Cp measurements are relative, because sapphire is the applied standard. As it is possible to determine the systematic error in a series of measurements, the results may be also calibrated for the ”0 heating rate”, which enables to identify points on phase diagrams.
DSC DuPont 910
Type: heat flux, range of temperatures: -50 - 700 oC; 1 - 40 deg/min; standard rate of heating/cooling; isothermal measurements; protective atmosphere: Ar, N2: cooling: ballistic; measurement of transformation enthalpy and relative Cp; measurement of heat flux versus time.
DSC Q 1000 TA
Type: heat flux, range: -120 – 400 oC; standard rate: 1 – 40 deg/min; precise isothermal measurements; protective atmosphere: He, Ar, N2; controlled cooling with liquid nitrogen; measurement of transformation enthalpy and Cp; calibration of basic line as Cp; method of heat modulations; measurement of heat flux versus time.
The laboratory caries out also measurements on two differential thermal analysers
Description of the equipment
Differential Thermoanalyser DTA can carry out precise measurements of temperature differences between a sample and the applied standard in the temperature range from 50 to 1600 oC. It is possible to investigate a phase transformation during continuous heating, with the possibility of defining the heating rate within a wide range. It is also possible to carry out experiments during cooling at slow rates, depending on the required temperature range. Measurements are performed in a protective atmosphere.
A computer registers results of experiments. They may be analysed by means of supplied software or any available programs for graphic analysis. The results are presented in the form of drawings or numerical data files and stored in Laboratory archives. An appropriate set of results may be used to determine kinetic equations of an investigated process on the basis of one of available theoretical models.
DTA DUPont 1600
Range of temperatures: 200 -1600 oC; standard rates: 1-10 deg/min; isothermal measurements; protective atmosphere: Ar, N2: cooling with the protective gas; measurement of temperature versus time.
SDT Q 600 TA
Range of temperatures: 300 - 1500 oC; standard rates: 1 - 40 deg/min; isothermal and thermo-gravimetric measurements; protective atmosphere: Ar, N2: cooling with the protective gas; measurement of temperature, mass, heat flux versus time.
Typical research topics
Martensitic transformation in shape memory materials like Cu-Ni based alloys, effects of decomposition and degradation.
Temperature induced phase transformations; heat stability of phases: recrystallization in deformed Al and Zr based alloys, phase transformations in magnetic Fe-Co alloys.
Experimental verification of phase systems like Cu-Ag_In, lead free alloys designed for welds.
Glassy transformation, crystallization and kinetics of transformations, C-P-T diagrams: metallic glasses (EC RTNNetwork) and polymers.
Specific heat of metallic systems: multiphase intermetallic compounds (program COST)
Nanomaterials: phase transformations at grain boundaries.
Intermetallic compounds (construction materials): heat stability of phases.
Processes of decomposition: nitrides of IN and Ga.
Sample preparation:
Samples should be of appropriate weight and size. For the DSC, a sample weight should be within the range from 0,1 to 100 mg. Approximately 10 mg is the recommended weight. Powder samples are also admissible. Powders are examined when enclosed in hermetic calorimetric pans designed mainly for reactive massive samples. The diameter of a massive sample must be smaller than 5 mm, while sample thickness should be as small as possible. For the DTA measurements, samples are placed in a platinum, ceramic or silica cup. That is why, massive sample size must fit within the following ranges: diameter < 4 mm, thickness <3mm.
The sample surface should be clean and smooth. Depending on the type of material and the required analysis, it may be subjected to mechanical preparation, provided it does not change its thermodynamic properties.
In the case of powder mixtures, it is important to preserve representative character of small measured volume of the investigated material.
Persons interested in co-operation should contact:
The Head of the Laboratory L-5:
Tomasz Czeppe, PhD.
phone: (0-12) 295 28 64, 295 28 77
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