In an article published in Optical Materials: X, researchers introduced an innovative approach for synthesizing graphene oxide (GO), a versatile nanomaterial with extensive scientific and technological applications. They employed laser spectroscopy techniques to analyze the produced GO samples, determining their thickness and distribution patterns.
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Background
Graphene is a two-dimensional material consisting of a single layer of carbon atoms arranged in a honeycomb lattice. It possesses remarkable properties such as high electrical and thermal conductivity, mechanical strength, and optical transparency.
However, graphene is difficult to tailor for specific applications. GO, a modified form of graphene with oxygen-containing functional groups attached to its surface, addresses this challenge. These groups enhance the solubility, dispersibility, reactivity, and chemical tunability of GO, making it more versatile than graphene. Removing oxygen groups from GO can yield graphene-like structures, partially restoring the original properties of graphene.
Conventional methods for synthesizing GO involve oxidizing graphite using strong acids and oxidizing agents, followed by exfoliation in water or other solvents. These methods are often expensive, complex, and hazardous, resulting in GO with varying degrees of oxidation and defects. Therefore, there is a need for simpler, cheaper, and safer methods to produce high-quality and uniform GO.
Research Methodology
In this study, the authors developed a novel method for synthesizing GO based on the thermal decomposition of polyvinyl alcohol (PVA) on a silicon dioxide (SiO2) coated silicon (Si) substrate. The process involves spin coating a PVA solution onto the SiO2/Si substrate, followed by high-temperature thermal annealing.
Initially, the silicon substrates were oxidized by cleaning in an oxygen environment to form a thin SiO2 layer. Subsequently, a PVA solution was spin-coated onto the SiO2 layer to create a uniform film. Heating the PVA/SiO2/Si structure at high temperatures decomposes the PVA into volatile gasses, leaving behind a layer of GO on the SiO2/Si substrate.
Characterization Techniques
Various techniques were employed to characterize the synthesized GO, including X-Ray diffraction (XRD), Fourier transform infrared (FTIR) spectroscopy, and laser spectroscopy.
Laser spectroscopy, a powerful tool for analyzing molecular structure and properties, was particularly instrumental. Two laser spectroscopy techniques were utilized: Raman micro-spectroscopy and fluorescence lifetime imaging microscopy (FLIM).
- Raman Micro-Spectroscopy: Determined the number and thickness of GO layers, as well as the degree of oxidation and defects. It utilizes a laser beam to excite vibrational modes of molecules and detects scattered light with different frequencies.
- FLIM: Investigated the thickness and distribution of GO layers, along with the local environment and quenching effects. It employs a pulsed laser beam to excite fluorescence emission and measures emission decay time.
Research Findings
The proposed technique proved cost-effective, easy, and straightforward for producing uniform and homogeneous GO films, eliminating the need for oxidizing agents or solvents.
- XRD Analysis: Revealed a peak at 10.27°, indicating the interlayer spacing of GO and confirming the absence of graphite or graphene structures.
- FTIR Spectroscopy: Showed peaks at 1435, 1288, 1081, and 1732 cm⁻¹, corresponding to carbon-carbon, epoxy hydroxyl, and carbonyl groups, indicating the presence of oxygen-containing functional groups on GO.
- Raman Spectroscopy: Displayed two characteristic bands: the G band at around 1580 cm⁻¹, corresponding to the in-plane vibration of the carbon atoms, and the D band at around 1350 cm⁻¹, corresponding to the disorder and defects in the carbon lattice. The ratio of the intensities of the D and G bands (ID/IG) varied from 0.9 to 1.2, indicating a moderate oxidation and defect level.
- FLIM Imaging: Exhibited two emission peaks: a strong one at 475 nm and a weak one at 690 nm, corresponding to the two fluorescence transitions of GO. The fluorescence lifetime of the 475 nm peak was around 0.5 ns, while that of the 690 nm peak was around 1.5 ns. Variations in fluorescence intensity and lifetime across the surface indicated the heterogeneity and thickness variation of the GO layers.
Applications
The synthesized GO has potential applications in solar cells, filtration systems, energy storage devices like supercapacitors, biosensing applications, and as a platform for drug delivery systems. The simplicity and cost-effectiveness of the synthesis method make it a promising approach for large-scale production of GO.
Conclusion
The researchers demonstrated the feasibility of the novel approach for preparing GO. They successfully characterized the synthesized GO using laser spectroscopy, confirming its single-layer presence and even distribution on the substrate.
Moving forward, they proposed optimizing the method to control oxidation degree, layer count, and chemical environment by combining laser spectroscopy with other techniques like electron microscopy for comprehensive analysis.
Journal Reference
Atta, D., et, al. (2024). Graphene oxide: Synthesis and laser spectroscopy approach. Optical Materials: X. doi.org/10.1016/j.omx.2024.100302
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