High-Yield Production of Nano-Lateral Size Graphene Oxide by High-Power Ultrasonication
Abstract
:1. Introduction
- Intensive oxidation of graphite by increasing concentration of oxidizing agents or increasing the timescale/cycles of oxidation process
- Centrifugation of GO in aqueous dispersion and separation of the fractions with smaller dimensions
- Breakdown of GO sheets by high-power ultrasonication
- Selective precipitation of larger GO sheets by protonation with organic solvents or by pH adjustment
- Exfoliation of graphite nanofibers with very small diameter
- Electrical breakdown of graphite by arc-discharge
- Ball milling of graphite in the presence of oxidizing agents
- Electrochemical exfoliation of graphite electrodes
2. Materials and Methods
2.1. GO Lateral Dimensions Reduction Based on Centrifugation
2.2. GO Lateral Dimensions Reduction Based on High-Power Ultrasonication
2.3. Transmission Electron Microscopy (TEM)
2.4. Zeta Potential Measurements
2.5. Fourier Transform Infrared (FTIR) Spectroscopy
2.6. X-ray Photoelectron Spectroscopy (XPS)
2.7. Thermogravimetric Analysis (TGA)
2.8. X-ray Diffraction Analysis (XRD)
2.9. Raman Spectroscopy
3. Results and Discussion
3.1. Morphological Features and Dispersion Stability
3.2. Chemical Properties
- sp2 and sp3 hybridizations of carbon (C–C and C=C, C1s at. % = 45.5 for GO and C1s at. % = 38.4 for GOn) in the graphitic backbone;
- single bonds between carbon and oxygen (C–O) in hydroxyls and ethers (C1s at. % = 44.9 for GO and C1s at. % = 53.2 for GOn);
- double bonds between carbon and oxygen (C=O), indicating the presence of carbonyl groups (C1s at. % = 4.2% for GO and C1s at. % = 2.8% for GOn);
- multiple bonds between carbon and oxygen (O=C−O), indicating the occurrence of carboxyls (C1s at. % = 4.5 for GO and C1s at. % = 3.9 for GOn); and
- O=C bonds present in carbonyl and carboxyl groups (O1s at. % = 3.1 for GO and O1s at. % = 5.7 for GOn);
- O–C bonds in hydroxyl groups and ethers (O1s at. % = 92.4 for GO and O1s at. % = 92.5 for GOn); and
4. Conclusions
Author Contributions
Funding
Institutional Review Board Statement
Informed Consent Statement
Data Availability Statement
Acknowledgments
Conflicts of Interest
References
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GBM | Surface Charge (mV) |
---|---|
GO | −29.7 ± 1.2 |
GOn | −39.9 ± 2.2 |
Elemental at. %/Chemical Group | Binding Energy (eV) | GO (%) | GOn (%) | |
---|---|---|---|---|
C/O ratio | - | 1.94 | 2.16 | |
C1s | - | 62.1 | 66.3 | |
O1s | - | 32.0 | 30.7 | |
C 1s (at. %) | C–C and C=C | 284.5 | 45.5 | 38.4 |
C–O | 286.7 | 44.9 | 53.2 | |
C=O | 287.9 | 4.2 | 2.8 | |
O=C–O | 288.5 | 4.5 | 3.9 | |
π–π* | 292.6 | 0.93 | 1.8 | |
O 1s (at. %) | C=O | 531.2 | 3.1 | 5.7 |
C–O | 532.5 | 92.4 | 92.5 | |
O=C–O | 534 | 4.5 | 1.9 |
Samples | D Band | G Band | ID/IG Band |
---|---|---|---|
GO after low-power exfoliation of GtO | 1355 | 1605 | 0.998 |
GO after centrifugation | 1358 | 1600 | 0.968 |
GO after high-power exfoliation/breakup of GtO | 1365 | 1602 | 0.880 |
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Timochenco, L.; Costa-Almeida, R.; Bogas, D.; Silva, F.A.L.S.; Silva, J.; Pereira, A.; Magalhães, F.D.; Pinto, A.M. High-Yield Production of Nano-Lateral Size Graphene Oxide by High-Power Ultrasonication. Materials 2021, 14, 1916. https://doi.org/10.3390/ma14081916
Timochenco L, Costa-Almeida R, Bogas D, Silva FALS, Silva J, Pereira A, Magalhães FD, Pinto AM. High-Yield Production of Nano-Lateral Size Graphene Oxide by High-Power Ultrasonication. Materials. 2021; 14(8):1916. https://doi.org/10.3390/ma14081916
Chicago/Turabian StyleTimochenco, Licínia, Raquel Costa-Almeida, Diana Bogas, Filipa A. L. S. Silva, Joana Silva, André Pereira, Fernão D. Magalhães, and Artur M. Pinto. 2021. "High-Yield Production of Nano-Lateral Size Graphene Oxide by High-Power Ultrasonication" Materials 14, no. 8: 1916. https://doi.org/10.3390/ma14081916