1. Stabilization of γ-Fe2O3 nanoparticles to heat by doping Nb and its property studied by Mössbauer spectroscopy.
- Author
-
Rahman, Habibur and Nakashima, Satoru
- Subjects
- *
FERRIC oxide , *MOSSBAUER spectroscopy , *MOSSBAUER effect , *ENERGY dispersive X-ray spectroscopy , *X-ray powder diffraction , *CALCINATION (Heat treatment) - Abstract
• Nb5+-doped γ - Fe 2 O 3 were synthesized by sol–gel method. • As the Nb doping increases (≥3.8 at.%), the transformation from γ - Fe 2 O 3 to α-Fe 2 O 3 was suppressed up to 600 °C. • At elevated temperature of 700 °C, γ - Fe 2 O 3 went through full transformation to α-Fe 2 O 3 by expelling large amount of Nb to the surface of α-Fe 2 O 3 forming FeNbO 4. Nb5+-doped γ - Fe 2 O 3 was synthesized by sol–gel method followed by calcination at various temperatures from 200 to 700 °C, analyzed using Powder X-ray Diffraction (PXRD), Transmission Electron Microscopy (TEM), Energy Dispersive X-ray Spectroscopy (EDS) and Mössbauer Spectroscopy. PXRD results show the formation of γ - Fe 2 O 3 at 300 °C and it begins to transform to α-Fe 2 O 3 at 350 °C for pure and 2 at.% Nb-doped samples. As the Nb doping increases (≥3.8 at.%), the transformation was suppressed up to 600 °C. TEM EDS confirms the incorporation of Nb to γ - Fe 2 O 3 lattice in 9.1 at.% Nb sample calcined at 500 °C. At elevated temperature of 700 °C, γ - Fe 2 O 3 went through full transformation to α-Fe 2 O 3 by expelling large amount of Nb to the surface forming FeNbO 4. TEM EDS confirms the compositional change during this process with reduced Nb content in α-Fe 2 O 3 and Nb-rich nanoparticle on the surface of α-Fe 2 O 3. Superparamagnetic properties were observed for Mössbauer spectra when the Nb doping increased, which is caused by decreased particle size. The slight increase in internal magnetic field also indicated the transformation from γ - Fe 2 O 3 to α-Fe 2 O 3. High Nb doping with 20 and 40 at.% shows the formation of FeNbO 4 at lower temperature where limited or almost no Nb substitution in α-Fe 2 O 3 was detected by EDS. [ABSTRACT FROM AUTHOR]
- Published
- 2024
- Full Text
- View/download PDF