Porosity and Specific surface area Platform - PORES

 

The PORES platform brings together several analysis techniques such as physisoprtion, capillary flow porometry and gas pycnometry to determine porosity, specific surface area and true density.

Adsorption/Désorption - BET

Nitrogen adsorption/desorption can be used to determine :

  • the specific surface area of a solid sample using the Brunauer, Emett and Teller "BET" method.
  • the pore distribution and pore volume of the material using the adsorption/desorption isotherm obtained

The adsorption-desorption isotherm is defined by the quantity of nitrogen adsorbed - desorbed (physisorption) by the solid at the temperature of liquid nitrogen (77K) as a function of the relative pressure (P/Po), between 10-3 and 1. Here is an example:

This isotherm can be used to determine :

  • the specific surface area (in m2/g) of the solid using the BET method
  • the total pore volume (in cm³/g)
  • the pore distribution using the BJH method (mesopores), (Horvath-Kawazoe during a micropore/CO2 adsoprtion analysis - Langmuir type isotherm)

 

We define the nature of porosity as a function of the size of the pores on the surface :

  • mesoporous solid: 2 nm < dpores < 50 nm
  • microporous solid: dpores < 2 nm

The platform has 3 adsorption-desorption units:

1. For mesoporous and microporous samples :

  • Micromeritics ASAP 2420, adsorbate : N2 , CO2

2. For mesoporous and microporous samples :

  • Micromeritics Tristar, adsorbate : N2
  • Micromeritics Tristar II+, adsorbate : N2

The platform also has a degassing station for 6 samples, the Micromeritics Vac Prep 061, which can heat up to a maximum of 450°C, dedicated to the preparation of samples analysed on the Tristars.

For optimum analysis conditions, samples must be degassed and stable under vacuum and temperature. The sample quantity should be between 50 and 200 mg. A standard analysis takes a few hours, and the equipment can be reserved for day or night use.

Contacts

Technical Referee :

  • Fabrice VIGNERON

Scientific Referees :

  • Ksenia PARKHOMENKO (microporous analysis)
  • Dominique BÉGIN (microporous analysis)

To request an analysis, please complete the downloadable form below and return it to the Technical Referee :
- Analysis/training request form 

For more information, please refer to the fact sheets below:

Capillary flow porometry

The aim of porometry is to determine the pore distribution of through-pore materials using the MP² (Multistage Pressure Process) technique. When a pore opens following a controlled rise in P, a flow rate is detected. This method results in a very accurate measurement of pore size and enables the true pore size distribution to be calculated.

It is the ideal technique for characterising a wide range of materials with a complex porous structure, such as porous membranes or ceramics, fibres, fabrics, etc.

The ICPEES has a Porolux Revo porometer that can investigate pore sizes ranging from 13 nanometers (1,3.10-8 m) to 500 micrometers (5.10-4 m).

Contacts

Technical Referee :

  • Fabrice VIGNERON

Scientific Referee :

  • Émeline LOBRY

 

Gas pycnometry

Gas pycnometry is used to determine the true volume and density of a sample using the gas displacement method. It is a non-destructive technique that uses inert gases (nitrogen, helium, etc.) as the displacement medium, the most commonly used being helium because of its ideal behaviour.

A cycle of purges (number to be defined) is carried out before the measurements. The latter are carried out in cycles (number to be defined), in order to compare the accuracy of each measurement with the others and to refine the average value.

The platform is equipped with a MICROMERITICS AccuPyc III, which enables volume measurements to be taken on a wide variety of powders, solids and slurries:

  • At temperatures between 5 and 60°C
  • In sample cells of 10, 3.5, 1 and 0.1 cm3

Density is determined directly from the sample mass (in g) and its measured volume (in cm3)

Contact

Technical Referee :

  • Fabrice VIGNERON
[Translate to English:]
[Translate to English:]
[Translate to English:]