Texture study of divided solids by gas adsorption: application to beryllia, alumina and to gels and oxides

A certain number of porous materials have been studied in an adsorption apparatus developed by us and leading to a measurement of the surface area with a reproducibility as good as 1/1 000. We have shown that this is only obtained at the cost of a number necessary precautions in the measurement of the gaseous volume adsorbed in a monomolecular layer (especially in the case of microporous solids). It also appears convenient to substitute argon to nitrogen, the latter being sensitive to chemical or electrical interactions with the adsorbent. Calculation methods of the pore size distribution are analyzed and discussed. The experimental data shows that the thickness of the multi-molecular layer must be estimated from the number of layers given by Shull using a layer thickness of 3.6 angstrom. A new method of analysis of the desorption curve is also given. We have also shown that a certain number of lamellar, non porous, systems, such as Be(OH)2 present a hysteresis branch on the adsorption isotherm of type I or II. Using the numerical data obtained by our method together with the information provided by the electronic microscope, we have been able to conclude that this hysteresis can be ascribed to the lack of rigidity of the solid. On the contrary, samples of microporous texture (r < 20 A) of the type of beryllia, provide the case, which we have been able to characterize, of porous materials which do not exhibit a hysteresis phenomenon. The above conclusions have allowed us to describe the evolution of the texture during their progressive dehydration (thermal treatment from 150 to 1100 C) of two series of samples, namely beryllia and alumina. (author)