Exploring Reliable and Efficient Plasmonic Nanopatterning for Surface- and Tip-Enhanced Raman Spectroscopies
Abstract
:1. Introduction
2. Basic Principles of Raman Spectroscopy
3. Surface- and Tip-Enhanced Raman Scattering
4. Development of Plasmonic Platforms
4.1. Bottom-Up Approaches
4.2. Top-Down Approaches
4.3. TERS Probe Production
5. Silver-Based Nanopatterns Obtained by Self-Assembling of Block Copolymers
5.1. Fabrication of SERS Substrates and TERS Tips by Self-Assembling Block Copolymers
- (a)
- BCP selection;
- (b)
- Formation of the PS-b-P4VP crew-cut micelles in toluene solution;
- (c)
- Incorporation of the silver precursor (silver ions) into the P4VP micelle core;
- (d)
- Reduction by BaBH4 of the coordinated silver ions to silver NPs;
- (e)
- Centrifugation and phase separation of the solution;
- (f)
- Spin-coating of the solution on the glass substrate;
- (g)
- Polymer removal by UV-light exposure.
5.2. Study of Cell Membranes Using SERS
5.3. Study of Protein Overexpression in Cancer Cells
5.4. TERS Tip Fabrication and Characterization
6. Nanostructured Ag Films using Solid-State Dewetting
- (i)
- The reactive species (atomic oxygen) produced in the discharge can oxidize the silver layer [132]. As the oxide layer grows, internal stresses due to mechanical or thermal excursions can induce the cracking of the formed layer [133]. However, as experimentally observed by the same authors and by our group, this cracking-induced process is not sufficient to explain the growth of nanostructures on the silver surface.
- (ii)
- Another mechanism is oxide diffusion at the interface (Kirkendall effect [134]). The different diffusion rates of metals and oxides produces a disequilibrium of the material flow that is compensated with the inter-diffusion of vacancies; the condensation of excess vacancies can give rise to void formation (Kirkendall voids), which leads to the formation of nanopores [135]. Nevertheless, since the Kirkendall effect cannot be activated unless the material is exposed to an elevated temperature, the authors of ref. [136] suggest that the temperature could rise locally due to the exothermic nature of the chemical oxidation reaction of silver. Another explanation could be that the energy carried by the oxygen atoms is converted into heat in the oxide layer [133]. Nevertheless, the Kirkendall effect is considered responsible for the formation of nanovoids inside nanocrystals and below the formed oxide layer. In fact, this effect is used to produce hollow structures, as reported in several works [137,138,139].
- (iii)
- Compared to the works of El Mel’s group, we suggest that the formation of porous nanostructures could be triggered by the solid-state dewetting of the oxidized silver layer. To minimize the energy of the system as the exposure time to the RF plasma increases, the structure of the oxide film rearranges to form grain boundaries along which atoms can easily migrate to form islands. In fact, a similar process is also reported in the work of Zhao et al. [140], where the Kirkendall voids have been proposed to explain the initial stage of thermally induced SSD of Cu films deposited on native Si oxide substrates. Our assumption is that the cracking process and the Kirkendall effect might weaken and destabilize the thin oxide layer, promoting the SSD of the silver oxide. Moreover, the morphology of the silver layer is more like the classical picture of spinodal dewetting because the nanostructures exhibit similar spatial correlation.
6.1. Fabrication of SERS Substrates and TERS Probes
- Oxidation of the Si AFM probe. This is necessary to modify the refractive index from the value of silicon (n = 4.4) to that of SiO2 (n = 1.5) in order to match better the refractive index of the air and tune the plasmon resonance in the visible region. Oxidation is obtained by heating the tips in a muffle furnace at 1000 °C for 10 h to produce a 200 nm SiO2 thick layer.
- Coating of the AFM tip using magnetron sputtering. This is done to improve the adhesion of the Ag layer on the tip. First, a bi-layer of Cr-Au (with respective thicknesses of 3 nm and 10 nm) is deposited, and then the layer of Ag is deposited with an optimized thickness of 30 nm.
- Plasma treatment in air. The AFM tip is exposed to the plasma of a radio-frequency discharge (inductively coupling plasma, ICP) sustained by synthetic air. The optimal exposure around 90 s was chosen following a procedure described in [141]. After this treatment, a structured Ag film covered by a Ag oxide (AgO and Ag2O [142]) layer is formed.
- Plasma treatment in argon. Further exposure to the Ar-plasma is necessary to reduce the formed Ag oxide. In this case, the exposure time is optimized by monitoring the presence of the oxide using X-ray diffraction (XRD) until it disappears, but preserving the metallic silver nanostructure.
6.2. SERS-Active Sensors for the Detection of Pollutant Molecules
7. Conclusions
Author Contributions
Funding
Institutional Review Board Statement
Informed Consent Statement
Data Availability Statement
Conflicts of Interest
References
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Sasso, A.; Capaccio, A.; Rusciano, G. Exploring Reliable and Efficient Plasmonic Nanopatterning for Surface- and Tip-Enhanced Raman Spectroscopies. Int. J. Mol. Sci. 2023, 24, 16164. https://doi.org/10.3390/ijms242216164
Sasso A, Capaccio A, Rusciano G. Exploring Reliable and Efficient Plasmonic Nanopatterning for Surface- and Tip-Enhanced Raman Spectroscopies. International Journal of Molecular Sciences. 2023; 24(22):16164. https://doi.org/10.3390/ijms242216164
Chicago/Turabian StyleSasso, Antonio, Angela Capaccio, and Giulia Rusciano. 2023. "Exploring Reliable and Efficient Plasmonic Nanopatterning for Surface- and Tip-Enhanced Raman Spectroscopies" International Journal of Molecular Sciences 24, no. 22: 16164. https://doi.org/10.3390/ijms242216164