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weight loss, %
Chapter 5 141
Table 5.5. The assignment of binding energies as well as the determined molar fraction of Pd 2+
and Pd 0 in Cu/Pd-BTC_4.
sample
Molar fraction (%)
Binding energy, eV
Assignment
Pd 3d 3/2 Pd 3d 5/2 Pd 2+ : (Pd 2+ +Pd 0 ) Pd 0 : (Pd 2+ +Pd 0 )
Cu/Pd-BTC_4
343.6 338.4 Pd 2+ (Pd1)
342.4 337.2 Pd 2+ (Pd2)
340.9 335.7 Pd 0 (Pd3)
30 70
100
90
80
Cu-BTC
Cu/Pd-BTC_3
Cu/Pd-BTC_4
70
60
50
40
100 200 300 400 500 600
T, C
Figure 5.20. TG curves of the activated Cu/Pd-BTC_4 and _5 solids in comparison with the parent
Cu-BTC and Cu/Pd-BTC_3.
In order to gain information on the quantitative incorporation of palladium, AAS analysis
of the activated Cu/Pd-BTC_4 solids has been performed. Thus, with respect to the taken
feeding ratios of the metal-precursors (20%), amount of the incorporated Pd in Cu/Pd-
BTC_4 sample is 12%, which is a little lower than that in Cu/Pd-BTC_3 (20%). TGA of the
Cu/Pd-BTC_4 (Figure 5.20) demonstrates the preserved thermal stability after palladium
introduction and show the framework decomposition after 300 °C. Interestingly, N2