SPIONs Prepared in Air through Improved Synthesis Methodology: The Influence of γ-Fe2O3/Fe3O4 Ratio and Coating Composition on Magnetic Properties
Abstract
:1. Introduction
2. Materials and Methods
2.1. Materials
2.2. Experimental Methodology
2.2.1. SPIONs Synthesis
2.2.2. SPIONs Coating
2.2.3. Characterization Techniques
Transmission Electron Microscopy (TEM)
Fourier Transform Infrared (FTIR) Spectroscopy
Powder X-ray Diffraction (XRD)
Mössbauer Spectroscopy
Magnetization Measurements
3. Results
3.1. Size, Morphology and Structural Analysis
3.2. XRD and Mössbauer Characterization
3.3. Magnetic Properties Evaluation
4. Discussion
Supplementary Materials
Author Contributions
Funding
Acknowledgments
Conflicts of Interest
References
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Sample | Washing | Drying |
---|---|---|
A 1.1 | Centrifuged | Air |
A 2.1 | Sedimented | Air |
A 3.2 | Centrifuged | Vacuum |
Sample | Sample Type | Synthesis |
---|---|---|
B 1.1 | SPIONs + PEG1000 | Method 1 |
B 2.2 | SPIONs + Dextran T10 | Method 1 |
C 1.1 | SPIONs + PEG1000 | Method 2 |
C 2.1 | SPIONs + Dextran T10 | Method 2 |
C 3.1 | SPIONs + PEG6000 | Method 2 |
C 4.1 | SPIONs + Dextran T70 | Method 2 |
Sample | TEMD (nm) | Phases Identified by XRD | Phases Identified by Mossbauer |
---|---|---|---|
A 1.1 | 10.5 ± 3.1 | goethite spinel | goethite maghemite |
A 2.1 | 8.1 ± 1.9 | goethite spinel | goethite maghemite |
A 3.2 | 7.5 ± 1.5 | goethite spinel | goethite maghemite magnetite |
B 1.1 | 4.4 ± 1.1 | Goethite Ferrihydrite | Goethite Ferrihydrite |
B 2.2 | 1.1 ± 0.4 | Ferrihydrite | Ferrihydrite |
C 1.1 | 7.9 ± 2.3 | Spinel | Maghemite Magnetite |
C 2.1 | 8.5 ± 1.9 | Spinel | Maghemite Magnetite |
C 3.1 | 7.6 ± 2.1 | Spinel | Maghemite Magnetite |
C 4.1 | 7.7 ± 2.0 | Spinel | Maghemite Magnetite |
Sample | T | IS | QS | Bhf or <Bhf> | I | Fe Species |
---|---|---|---|---|---|---|
A1.1 | 295 K | 0.35 | −0.03 | 25.4 | 100% | * |
A1.1 | 4 K | 0.50 0.45 0.45 | 0.52 −0.07 −0.25 | 52.5 53.3 51.4 | 16% 34% 50% | Fe3+ CN = 6 γ Fe2O3 Fe3+ CN = 4 γ Fe2O3 Fe3+ CN = 6 α FeOOH |
A2.1 | 295 K | 0.35 0.32 | 0.60 −0.11 | −23.5 | 32% 68% | * |
A2.1 | 4 K | 0.49 0.44 0.47 | 0.40 −0.10 −0.25 | 52.7 53.3 51.2 | 18% 15% 67% | Fe3+ CN = 6 γ Fe2O3 Fe3+ CN = 4 γ Fe2O3 Fe3+ CN = 6 α FeOOH |
A3.2 | 295 K | 0.33 0.65 | 0.03 −0.18 | 30.6 33.3 | 84% 16% | Fe3+ CN = 4, 6 γ Fe2O3, Fe3O4 Fe2.5+ CN = 6 Fe3O4 |
A3.2 | 4 K | 0.49 0.43 0.93 | 0.02 −0.03 0.12 | 53.7 51.5 46.2 | 39% 51% 10% | Fe3+ CN = 6 γ Fe2O3 Fe3+ CN = 4, 6 γ Fe2O3, Fe3O4 Fe2+ Fe3O4 |
B1.1 | 295 K | 0.37 | 0.76 | − | 100% | Fe3+ CN = 6 Ferrihydrite, αFeOOH |
B1.1 | 4 K | 0.50 0.49 0.48 | 0.35 −0.10 −0.25 | 50.3 46.3 50.5 | 9% 69% 22% | Fe3+ CN = 6 Ferrihydrite Fe3+ CN = 6 Ferrihydrite Fe3+ CN = 6 α FeOOH |
B2.2 | 295 K | 0.37 | 0.75 | - | 100% | Fe3+ CN = 6 Ferrihydrite |
B2.2 | 4 K | 0.50 0.49 | −0.04 −0.11 | 49.5 45.8 | 36% 64% | Fe3+ CN = 6 Ferrihydrite Fe3+ CN = 6 Ferrihydrite |
C1.1 | 295 K | 0.35 0.64 0.35 | 0.01 −0.12 0.60 | 34.7 33.8 − | 91% 7% 2% | Fe3+ CN=4, 6 γ Fe2O3, Fe3O4 Fe2.5+ CN = 6 Fe3O4 Fe3+ CN = 4,6 γ Fe2O3 |
C2.1 | 295 K | 0.33 0.65 0.36 | −0.02 0.02 0.47 | 34.3 49.1 − | 84% 14% 2% | Fe3+ CN=4, 6 γ Fe2O3, Fe3O4 Fe2.5+ CN = 6 Fe3O4 Fe3+ CN = 4,6 γ Fe2O3 |
C3.1 | 295 K | 0.37 0.65 0.30 | −0.03 0.29 0.66 | 33.4 33.4 − | 90% 7% 3% | Fe3+ CN=4, 6 γ Fe2O3, Fe3O4 Fe2.5+ CN = 6 Fe3O4 Fe3+ CN = 4,6 γ Fe2O3 |
C4.1 | 295 K | 0.29 0.64 0.37 | 0.11 −0.19 0.64 | 31.8 32.3 − | 42% 31% 27% | Fe3+ CN=4, 6 γ Fe2O3, Fe3O4 Fe2.5+ CN = 6 Fe3O4 Fe3+ CN = 4, 6 γ Fe2O3 |
Sample | Ms * (emu/g) (300 K) | Ms * (emu/g) (10 K) | TB ** (K) | Tv ** (K) |
---|---|---|---|---|
A 1.1 | 47 | 56.5 | 126 | - |
A 2.1 | 29 | 36.5 | 78.5 | - |
A 3.2 | 64 | 71 | 150 | 37.7 |
B 1.1 | ~8 | 13 | 112 | - |
B 2.2 | ~1.4 | 4.5 | 20 | - |
C 1.1 | ~56 | 65.5 | ~180 | 35.0 |
C 2.1 | ~62 | 69.0 | ~194 | 32.8 |
C 3.1 | ~50 | 58.0 | ~165 | 34.8 |
C 4.1 | ~41 | 48.5 | ~160 | 32.8 |
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Matos, J.C.; Gonçalves, M.C.; Pereira, L.C.J.; Vieira, B.J.C.; Waerenborgh, J.C. SPIONs Prepared in Air through Improved Synthesis Methodology: The Influence of γ-Fe2O3/Fe3O4 Ratio and Coating Composition on Magnetic Properties. Nanomaterials 2019, 9, 943. https://doi.org/10.3390/nano9070943
Matos JC, Gonçalves MC, Pereira LCJ, Vieira BJC, Waerenborgh JC. SPIONs Prepared in Air through Improved Synthesis Methodology: The Influence of γ-Fe2O3/Fe3O4 Ratio and Coating Composition on Magnetic Properties. Nanomaterials. 2019; 9(7):943. https://doi.org/10.3390/nano9070943
Chicago/Turabian StyleMatos, Joana C., M. Clara Gonçalves, Laura C. J. Pereira, Bruno J. C. Vieira, and João Carlos Waerenborgh. 2019. "SPIONs Prepared in Air through Improved Synthesis Methodology: The Influence of γ-Fe2O3/Fe3O4 Ratio and Coating Composition on Magnetic Properties" Nanomaterials 9, no. 7: 943. https://doi.org/10.3390/nano9070943