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Belay Zeleke Dilnesa - Eawag-Empa Library

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CHAPTER 3 SYNTHETIC FE-CONTAINING HYDRATES<br />

3.5.3. Fe-katoite, C3FH6<br />

C3FH6 was attempted to synthesize at 20, 50 and 80 °C by mixing C2F and CaO in 0.1 M<br />

KOH. Trace amounts of metastable C3FH6 were observed in the samples equilibrated up<br />

to 1 year at 20 °C (2θ = 19.71, Fig. 51). However, C3FH6 disappeared and decomposed to<br />

portlandite and iron hydroxide with time. At longer equilibration time C4FcH12 was<br />

formed due to CO2 contamination, which destabilized the CaO-Fe2O3-H2O system. This<br />

shows the metastability of C3FH6 with respect to Fe-hydroxide and portlandite and in the<br />

presence of CO2 to hemi/monocarbonate. This metastability of C3FH6 agrees with the<br />

findings of Ecker et al. [12] and Rogers et al. [119]. The CaO-Fe2O3-H2O system is very<br />

sensitive to carbonation at room temperature. The sample synthesized hydrothermally at<br />

110° C contained portlandite and Fe-oxide/hydroxides and traces of C3FH6. Another<br />

weak reflection was observed corresponding to a basal spacing d = 7.58 Å (2θ=11.65°)<br />

which persisted at longer age. It does fit neither to C4Fc0.5H10 nor to C4FcH12. The peak<br />

was tentatively assigned to C4FHx with an unknown number of water molecules. All the<br />

samples showed a reddish color of the solids indicating the formation of XRD amorphous<br />

Fe-oxide/hydroxide in the CaO-Fe2O3-H2O system. The TGA-DTG curve also revealed<br />

the formation of traces of metastable C3FH6 (see Fig. 49).<br />

117

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