Magnetic properties of Co–Al, Ni–Al, and Mg–Al hydrotalcites and the oxides formed upon their thermal decomposition
The magnetic behaviour of Co–Al, Ni–Al, and Mg–Al hydrotalcites (HTlc) with a M2+/Al3+ molar ratio of 3 and carbonates in the interlayer, as well as the mixed oxides obtained after calcination at 823 K for 5 h, has been investigated by DC and AC magnetic susceptibility measurements and isothermal magnetisation. The samples were also characterised by ICP-OES and XRD. The magnetic measurements show that Co–Al and Ni–Al HTlcs behave as ferromagnets, with ordering temperatures of approximately 6–7 K in both cases, and displaying hysteresis loops at 2 K with coercive fields of 4.2 and 5.5 mT, respectively, whereas the Mg–Al-HTlc shows the expected diamagnetic behaviour. A solid solution of cobal…
Steam-activated FeMFI zeolites. Evolution of iron species and activity in direct N2O decomposition
Abstract In this paper the effect of the composition and steaming conditions of FeMFI catalysts on activity in direct N2O decomposition is investigated. MFI zeolites with different framework compositions (FeAlSi, FeGaSi, and FeSi) and without iron ( 100 mbar H2O in N2) favor the extraction of framework iron, enabling the application of lower activation temperatures. The optimum temperature during steam activation is that at which extraction of framework iron is complete without extensive clustering of extra-framework iron species into oxide particles, as was demonstrated by transmission electron microscopy and electrochemical characterization of the samples. Additional experiments show…
Physicochemical Characterization of Isomorphously Substituted FeZSM-5 during Activation
Physicochemical characteristics of isomorphously substituted FeZSM-5 both after preparation and after activation have been determined by gas (Ar and N2) physisorption, 27Al and 29Si magic-angle spinning–nuclear magnetic resonance, NH3 temperature-programmed desorption, transmission electron microscopy, H2 temperature-programmed reduction (TPR), 57Fe Mossbauer spectroscopy, and voltammetric response techniques. The activation of as-synthesized FeZSM-5 comprises calcination at 823 K and a subsequent steam treatment (300 mbar of H2O in N2) at 873 K. Calcination leads to complete removal of the template. During this process a significant fraction of iron is dislodged to extraframework positions…
Electrochemical characterization of iron sites in ex-framework FeZSM-5
Abstract The electrochemical response of FeZSM-5 prepared by an ex-framework method has been studied using Paraloid B72 polymer film electrodes immersed in aqueous media using H2SO4, HCl, Na2EDTA and NaCl electrolytes. The ex-framework method comprises the hydrothermal synthesis of isomorphously substituted FeZSM-5, followed by calcination at 823 K and subsequent steam treatment (300 mbar H2O in N2) at 873 K. During this process iron is extracted to extra-framework positions. Also partial dealumination of the zeolite framework takes place. Characteristic voltammetric responses in the +1.0 to −0.6 V versus SCE potential range have been recorded and were used to characterize the iron species …