We are interested in trying some of our chemistry to make MOF, but have no idea about how to work. I would need some info in how to characterise basically the main basic things.
For characterization of MOFs,after proper solvent washing and drying to eliminate the solvent in the MOF structure.The first characterization is basically TGA-DTA analysis to determine the thermal stability of MOF.It will also help us determine the out-gassing temperature for BET surface area analysis.If the surface area obtained is large (which depends on the length of organic linker used) mostly >100m2/g.Followed by isotherm studied and single crystal XRD or PXRD .You can compare your PXRD pattarn with once available in the literature.
We basically follow the above protocol pattern in our lab.
Yes, you can synthesis them easily based on some conditions you need to optimize or standardize for -the crystallization
Various Crystallization techniques used for MOF synthesis
1. Solvothermal reaction in vials - where you use mixture of solvents and heat them to get MOF crystals.
2. Hydrothemral reactions - using only water for the synthesis and heating them till crystallization starts.
3. Hydrothermal/ Solvothermal in Teflon (PTFE lined autoclave) - Where teflon autoclaves are used and high pressure is generated by the vapours of solvents
4. Layering diffusion techniques- Where metal and ligand solutions are layered over each other depending on solution density and let them diffuse into each other slowly and crystallization takes place in 3-4 weeks.
5. Microwave assisted synthesis - where microwave energy is used for instant crystallization or fast crystallization.
For getting powder MOF or microcrystalline MOFs you can use mechanochemical synthesis technique ( either solvent free or solvent assisted) or sonochemical synthesis ( where sonochemical energy is used for the synthesis )
For more insight you can go through some of my papers where I used these techniques to synthesize porous MOFs