Table 2. Parameters Obtained from Fitting 57Fe Mössbauer Data of Products from Reaction between Fe3O4 and NaNH2a.
sample | site | δ (mm s–1) | Δ (mm s–1) | Γ (mm s–1) | fraction (%) | assignment | approximate composition | average formal Fe oxidation state |
---|---|---|---|---|---|---|---|---|
170 °C/24 h | S1 | 0.13 | 0.18 | 14 | γ″-FeN | FeNx | 3.00 | |
D1 | 0.43 | 0.30 | 0.16 | 30 | ε-Fe2+xN Fe(III) | Fe2.38N | 1.26 | |
D2 | 0.25 | 0.46 | 0.19 | 26 | ε-Fe2+xN Fe(II) | Fe2.38N | ||
D3 | 0.27 | 0.83 | 0.17 | 29 | FeO1–xNx | FeO0.20N0.80 | 2.80 | |
170 °C/96 h | S1 | 0.16 | 0.14 | 8 | γ″-FeN | FeNx | 3.00 | |
D1 | 0.44 | 0.29 | 0.18 | 31 | ε-Fe2+xN Fe(III) | Fe2.38N | 1.26 | |
D2 | 0.25 | 0.46 | 0.18 | 28 | ε-Fe2+xN Fe(II) | Fe2.38N | ||
D3 | 0.28 | 0.84 | 0.20 | 33 | FeO1–xNx | FeO0.25N0.75 | 2.75 | |
190 °C/24 h | S1 | 0.16 | 0.16 | 12 | γ″-FeN | FeNx | 3.00 | |
D1 | 0.45 | 0.28 | 0.17 | 26 | ε-Fe2+xN Fe(III) | Fe2.38N | 1.26 | |
D2 | 0.26 | 0.48 | 0.17 | 23 | ε-Fe2+xN Fe(II) | Fe2.38N | ||
D3 | 0.30 | 0.92 | 0.24 | 39 | FeO1–xNx | FeO0.35N0.65 | 2.65 |
δ – Isomer Shift, Δ – Quadrupole Splitting, Γ – Half-Width Full Max. Δ is given relative to metallic Fe at room temperature. Estimated precision on δ, Δ, and Γ is 0.02 mm s–1 and 2% on the site fraction. Site assignment for each spectral component is indicated.