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Intensity, a. u.
Chapter 4 109
4.3.1 Preparation and characterization of Cu-DEMOF samples [Cu3(BTC)2-x(ip)x]n
All samples D1-8 have been prepared via mixed-linker soild solution approach with
distinct relative H3BTC : H2ip molar ratios under solvothermal conditions (80 °C, 20 h).
For each sample, various Cu-salts and solvents (DMF or EtOH) have been employed.
Samples D5 and D6 are prepared following reported method. [140]
4.3.1.1 Solids obtained using Cu(BF4)2∙6H2O as metal precursor
D4
D3
D2
D1
Cu-BTC_sim.
5 10 15 20 25 30
2, degree
Figure 4.40. PXRD patterns of the activated Cu-DEMOF samples D1-4 in comparison with the
patterns simulated from the single-crystal XRD data of the reported [Cu 3 (BTC) 2 ] n (Cu-BTC_sim).
Metal source: Cu(BF 4 ) 2 6H 2 O. Solvent used for synthesis of D1 and D2 (blue patterns): DMF; for
D3 and D4 (red patterns): EtOH.
PXRD patterns of all activated samples D1-4 (Figure 4.40) match well with the simulated
patterns of [Cu3(BTC)2]n (Cu-BTC_sim), suggesting that they all are all phase-pure,
crystalline and isostructural with the non-doped parent Cu-BTC. To note, the small double
reflection of the as-synthesized sample D4_as at around 9.4°and reflections at 5.7°for the