mc2note-poresize-mesoporosity
mc2note-poresize-mesoporosity
Materials Characterisation
Experimental details
Method: Analysis of mesopores by gas material, dried for 3 h at 350 °C under
adsorption, ISO 15901-2:2006(E) [1] vacuum (unrestricted from 1.33⋅10-2 mbar)
Instrument: Micromeritics 3Flex Amount of sample: 230 mg
Adsorptive gas: N2 at 77 K Sample holder: glass tube of 12 mm outer
Sample: reference silica-alumina porous diameter with a seal frit
20
Amount adsorbed (mmol/g)
15 desorption
10
adsorption
5
0
0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1
Relative pressure
Adsorption isotherm of the reference silica-alumina porous solid. According to the classification of
standard physisorption isotherms (IUPAC [2]) this is a type IV isotherm with a hysteresis loop of
type H2: it is the signature of a mesoporous solid. The adsorption and desorption branches are
different, and a hysteresis loop with non-parallel branches is observed, typical of pores whose size
distribution is wide and shape is not well defined.
MC² – Material and Chemical Characterisation Facility
Materials Characterisation
Results
The adsorption isotherm already contains
Conclusion
The distribution of pore size of a Pore sizes screened by this method range
mesoporous solid can be extracted from the from 2 nm to 150 nm. For larger pores
measurement of its adsorption isotherm mercury intrusion may be used.
using the BJH model. This method only works on porous solids
The BJH model is only valid for well-defined that have been dried beforehand, in order
pore shapes, with minimal interconnection to clean the surface and the pores from any
between the pores. adsorbed molecule. This can be done under
The quantity needed for that experiment is vacuum or dry gas sweeping, and at high
rather large: at least several hundreds of temperature too. If the porous solid cannot
mg and it needs to be known within 2 % undergo drying, thermoporometry may be
error, as the results are always presented in used: it uses calorimetry instead of
specific units. volumetry.
[1] Pore size distribution and porosity of solid materials by mercury porosimetry and gas adsorption —
Part 2: Analysis of mesopores and macropores by gas adsorption, ISO 15901-2:2006(E)
[2] Sing K.S.W., Everett D.H., Haul R.A.W., Moscou L., Pierotti R.A., Rouquérol J. and Siemieniewska T.,
IUPAC Recommendations 1984: Reporting Physisorption Data for Gas Solid Systems with Special
Reference to the Determination of Surface Area and Porosity, Pure & Applied Chemistry 57, 1985, pp. 603-
319