Porous materials receive a high level of scientific and technological interest due to their applications in various fields such as adsorption, separation and storage, catalysis, ion exchange, nanotechnology, etc. Gas adsorption is a well-established tool for the characterization of the texture of porous solids. Physisorption isotherms are generally expected to be well reproducible for rigid adsorbents, but this is not always the case for nonrigid (flexible) materials. The presence of a metastability region and sensitivity of the activation barriers to the material's texture often influence the isotherms' run. Here, we address the complexity that arises in terms of reproducibility and sample handling for flexible metal-organic frameworks, with the example of DUT-8(Ni). It belongs to the group of "gate opening"metal-organic frameworks and is a typical representative of the pillared layer compounds. We propose characteristic parameters for the analysis and comparison of adsorption isotherms, showing the "gate opening"step, associated with the adsorption-induced solid-state phase transition. A set of 50 nitrogen physisorption isotherms measured at 77 K were analyzed and correlated with the synthetic and outgassing conditions. The study highlights the importance of accurate descriptions and record-keeping of experimental details and their role in the replication of scientific results.
|Seiten (von - bis)
|Veröffentlicht - 22 Nov. 2022
ASJC Scopus Sachgebiete
- Organic framework dut-8(ni), Determining surface-areas, Hydrogen storage, Bet method, Particle-size, Adsorption, Flexibility, Physisorption, Pressure