Developing New Routes for Mechanical Characterization of Metal-Organic Frameworks Public Deposited

http://ir.library.oregonstate.edu/concern/graduate_thesis_or_dissertations/3j3335420

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  • Metal-organic frameworks (MOFs) represent an exciting, new class of porous materials. Their hybrid organic-inorganic structure opens up near infinite possibilities to tune and design their structure for specific properties and applications. A new generation of flexible MOFs, following a generation of stiff MOFs, has created additional design space and complexity. To date, the properties even of known MOFs, especially mechanical properties, remain largely unexplored. In this thesis, methods to synthesize MOFs and characterize their mechanical properties are explored. Solvothermal methods were chosen to synthesize MOF-5, a stiff MOF, and MIL 53(Al), a flexible MOF. X-ray diffraction data proved that both MOFs were synthesized in phase pure form. Immobilization and polishing methods were developed to prepare the MOFs for mechanical testing. S1813 photoresist and Buehler epoxy were chosen as media to immobilize MIL-53(Al). The goal was to produce samples flat enough for reproducible and consistent mechanical measurements using nanoindentation and atomic force microscopy. Mechanical testing produced high quality, reproducible measurements. However, the media employed to immobilize the MOFs, as well as the polishing process, played an undesired role in altering both the structure and mechanical properties of the MOFs. AMFM, an AFM mode capable of mapping mechanical properties, produced images of MIL-53(Al) immobilized in S1813 photoresist showing elastic moduli of 7 to 7.5 GPa for the MIL-53(Al) particles. AMFM of MIL-53(Al) immobilized in Buehler epoxy produced images of MIL-53(Al) with elastic moduli from 8 to 12 GPa. Nanoindentation proved inconclusive for determining the elastic modulus of MIL-53(Al) in S1813 since the system was not sensitive enough to reliably indent small MIL-53(Al) particles that ranged in size from 1 to 5 μm.
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