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• W8823908 abstract "Recently for the first time, phase transitions have been observed both by calorimetric and adsorption isotherm measurements during the sorption of simple gases (argon, nitrogen) on the zeolite Silicalite I [1]. Such phenomena appear in the high loading and low temperature sorption regime. Silicalite I belongs to the MFI micropore structural network, it is the pure silica form of ZSM-5 zeolite which is of great importance in petroleum catalytic cracking. The Silicalite I pore network is rather complex. It is composed of straight channels and sinusoidal channels (their respective elliptical diameters are 5.4 × 5.6 Å and 5.1 × 5.4 Å). Our neutron diffraction studies, concerning the sorbed phases of both 36-argon and n-argon, have pointed out that the phase transition is associated with the appearance of a crystalline order (long range order) in the sorbed argon species. Moreover the Silicalite I structure modification seems to be very small during the gas sorption. These observations result from the large neutron coherent scattering length b difference between 36-argon and n-argon (b36Ar=2.43 and bAr=0.20). We can conclude that the adsorption isotherm substep observed during the argon loading of the Silicalite I zeolite is undoubtedly the signature of a phase transition concerning the sorbed species and not a consequence of a Silicalite I structural modification. The two sorbed phases are a disordered phase characterized by a short range atomic order (presumably a fluid phase) and a crystalline solid phase characterized by a periodic long range atomic order. The periodic organization of the argon atoms is induced by the Silicalite I adsorption sites. The phase transition corresponds to a change in the adsorption nature: from a mobile adsorption to a localized adsorption. Our neutron diffraction investigation of the argon/ZSM-5 (Si/Al=23) system has shown that the same phase transition is observed. The inner surface of the Silicalite I zeolite, which is accessible to gas molecules of lower diameter than 5.6 Å, is quite complex at the atomic level. This surface complexity is due to the two different familly of micropores (straight micropores, sinusoidal micropores and their intersections) and to the different local symmetry of the adsorption sites (square, pentagonal and hexagonal symmetry). The laboratory of Prof. K.K. Unger at Mainz was the first laboratory which succeded to prepare Silicalite I samples composed of large crystallites with high level of crystallinity. As a consequence sorption studies by isothermal volumetry and microcalorimetric measurements, of simple gases on these Silicalite I samples have revealed new and interesting phenomena. For the first time, the “signature” of a phase transition (as adsorption isotherm substep or exothermic heat peak of adsorption) was observed during the sorption of argon and nitrogen [1-2]. Recently several new examples of isotherm substeps have been observed during the sorption studies of Kr, CO, O2 and D2 on Silicalite I, Figure 1 [3-4]." @default.
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• W8823908 date "1994-01-01" @default.
• W8823908 modified "2023-10-16" @default.
• W8823908 title "Crystalline structure analysis by neutron diffraction of argon sorbed phases observed in the high loading regime of silicalite I and ZSM-5 (Si/Al=23) zeolites." @default.
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• W8823908 doi "https://doi.org/10.1016/s0167-2991(08)63115-8" @default.
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