THE PHYSICOCHEMICAL TEST LABORATORY (L-8) :: Instytut Metalurgii i Inżynierii Materiałowej Polskiej Akademii Nauk
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  THE PHYSICOCHEMICAL TEST LABORATORY (L-8)


Scope of accreditation of research laboratory No AB 120
issued by Polish Centre for Accreditation Issue No. 17 of 12 June 2019.



Head of the laboratory

The experts

Adam Dębski, PhD DSc, Eng.
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Sylwia Terlicka PhD, Deputy Head of the Laboratory


Address:

Institute of Metallurgy and Materials Science Polish Academy of Sciences

ul. Reymont 25, 30-059 Krakow

phone: (48) 12 295 28 98, fax: (48) 12 295 28 04

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Procedure
Dilatometric measurement of solid and sintered materials (procedure no. P/19/IB-21)
Hydrogen sorption in solid materials (procedure no. P/19/IB-22)


Apparatus:

Optical dilatometer Misura® 3 FLEX-ODLT
Device for gas sorption (IMI HTP) Hiden Isochema


Description of the equipment

1. Dilatometric measurements of solid and sintered materials.

The optical dilatometer Misura® 3 FLEX-ODLT is designed for non-contact dilatometric measurements of very high accuracy. It is possible to register changes in the length of the tested samples as a result of temperature changes (both heating and cooling process) as a function of time, therefore determine the thermal expansion coefficient of investigated samples. Moreover, the optical dilatometer Misura® 3 FLEX-ODLT enables non-contact bending measurements.



The device is calibrated with the use of NIST certificated references sample material "SRM 738 Stainless Steel" (https://www-s.nist.gov/srmors/certificates/738.pdf) at an accredited range of temperature (20-507 â—¦C).


 


The dilatometric tests allow for:

  • Dilatometric analysis of the kinetics of phase transitions.
  • Study of phase transitions occurring in a solid state.
  • Determination of density dependence on temperature of ceramic materials.
  • Determination of density dependence on temperature of loose materials.
  • Determination of material thermal expansion coefficient.
  • Observing changes in specimen geometry during the sintering.
  • Performing non-contact bending measurements of materials.
  • Bending study caused by differences in thermal expansion between ceramic mass and glaze.

Technical parameters of the optical dilatometer Misura® 3 FLEX-ODLT

  • Accredited measuring a range of temperature is from 20 °C to 507 °C (resistance furnace), ± 15-25 % total length of the sample (maximum measuring temperature outside of accreditation up to 1600 â—‹C).
  • Speed of heating: 2-30 °C /min.
  • Protective gas: Ar (it is possible to change the inert gas to He or N2).
  • The sample orientation: horizontal.
  • Resolution: 0.5 µm.
  • Accuracy of α: 0.05·10-6·K-1.
  • Dimension of the sample (length, height, width):
         cuboid: 50 x 5 x 5 mm (± 1 mm),
         cylindrical: 50 x 5 mm (± 1 mm),
         thin materials (foils, sheets, plates etc.): 50 x 5 x without limit (± 1 mm).

  • Recording of changes in sample length: optical.
  • Cooling: natural.
  • Contactless measurement.


2. Hydrogen sorption in solid materials

The Hiden Isochema sorption measurement system allows for automatic isothermal absorption and desorption of hydrogen and other gases in both solid and powder samples using Sievert's method. It is possible to test samples in the temperature range from -196 â—‹C to 500 â—‹C in the pressure range up to 200 bar. Based on obtained results from hydrogen isothermal absorption and desorption cycles (presented as a mass or atomic percentage as a function of time) the enthalpy of formation and decomposition of tested materials can be determined. In addition, this device cooperates with a mass spectrometer and allows to perform the temperature programmable desorption (TPD). It is also possible to lead the sample into the reactor in a protective gas atmosphere (dedicated to reactive materials).

Performance parameters of the hydrogen sorption measurement apparatus Hiden Isochema:

  • Temperature can be controlled from the software with an accuracy of not less than 0.1 °C.
  • A special liquid nitrogen dewaring system and power supply system allow measurements to be taken at a temperature close to that of liquid nitrogen.
  • Possibility to test samples in to pressure ranges: low-pressure range (0-1 bar) and high-pressure range (0-200 bar).
  • Vacuum system with turbomolecular pump ensuring a vacuum in the reactor not less than 1·10-5mbar.



Preparation of samples for investigation in the L-8 laboratory.

The way samples are taken and delivered for analysis is the responsibility of the Customer. The Customer shall be advised to take samples so as to be representative of a given batch of material.
- Dilatometric tests:
Samples for dilatometric testing should be of sufficient length (50 mm). The surface of the test samples shall be smooth and clean. The parallelism of the test surfaces shall be maintained.
- Hydrogen sorption test:
The shape and form of samples for sorption testing are determined individually with the customer. Maximum test sample size: roller 10 mm long and φ 6 mm or powder.


The ones who are interested in carrying out the experiments by using the presented above methods should contact:

 

Head of the laboratory L-8:
Adam Dębski PhD DSc, Eng.
tel: 12 295 28 14
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