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. 2021 Jan 25;60(4):2553–2562. doi: 10.1021/acs.inorgchem.0c03452

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
a

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.