Characterization of the Auburn Catalysts Sample Clauses

Characterization of the Auburn Catalysts. The six Co/SiO2 and Co/Al2O3 catalysts received from Xx. Xxxxxxx are listed in Table I. These include fresh 15% Co/SiO2 catalysts A1 and B1 and their calcined forms A1/C and B1/C. The remaining two catalysts are: calcined 15% Co/Al2O3 listed as C1, and C1/U which is C1 used for 12 days in a reactor. The results of our findings from the XRD, magnetic and EMR investigations are summarized in Table I. For the fresh samples A1 and B1, XRD (Fig. 1) gives only a broad signal due to amorphous SiO2 around 2θ = 24o and no peaks due to crystalline Co(0), CoO or Co3O4 are observed even though 15 % Co concentration is high enough for detection by XRD. This implies that Co in these samples is in highly dispersed (noncrystalline) form. Temperature variation of the magnetic susceptibility χ is found to follow the Xxxxx-Xxxxx law and magnetic field variation of the magnetization at 2 K shows Co to be in the Co2+ state with concentration of 3.7 % for A1 and 3.0% for B1 [1]. These concentrations are a factor of about five smaller than the nominal 15% Co concentration. A possible explanation for this discrepancy is the presence of Co3+ in the low spin state with zero magnetic moment. In the EMR studies, a resonance line due to Sample Description XRD Magnetic EMR A1 15% Co/SiO2-Fresh 15% Co/SiO2-Fresh Calcined A1 Calcined B1 15%Co/Al2O3-calcined C1 used for 12 days SiO2 Xxxxx-Xxxxx Co2+ Xxxxx-Xxxxx Co2+ Co3O4 Co3O4 Co3O4 CoO, Co(0) Co2+-broad line g = 4.3 Co2+-broad line g = 4.3 No line Co2+-weak line g = 4.3 Co2+-line,g=4.3 with sharp line Co2+-line. Co(0)-line B1 SiO2 A1/C SiO2, Co3O4 B1/C SiO2, Co3O4 C1 Co3O4, δ-Al2O3 C1/U CoO, Al2O3(α,δ,χ) Co2+ is observed. For the calcined samples A1/C and B1/C, we clearly see the presence of Co3O4 (Fig 1) which contains Co2+ and Co3+ configuration. This is also confirmed in the χ vs T studies where a magnetic transition near 40 K due to Co3O4 is clearly observed [2]. The electronic state of Co3O4 can be written as CoO.Co2O3 so that the concentration of Co3+ ions with zero magnetic moment is twice of that of Co2+, explaining the above concentration discrepancy. Thus we conclude that in the fresh Co/SiO2, Co is present in highly-dispersed non-crystalline form which is a precursor to Co3O4, and transforms to crystalline Co3O4 upon calcinations. For the Co/Al2O3 based sample C1, the room temperature XRD pattern shows the presence of Co3O4 and Al2O3. When the sample is used in the reactor for 12 days yielding the sample C1/U, Co3O4 is reduce...
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