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Nanomaterials 2020, 10, 830 8 of 11 sample (fused silica/graphene) previously used and R6G was then deposited by spin coating. Ultra-small Ag NPs were used to preserve the transparency required for the interference process and because we recently demonstrated that, for the same plasmon absorption, the SERS effect is more efficient for these 4 nNmanoNmaPtseritahlsa2n02f0o,r10la, xrgFeOrRoPnEeEsRdRuEeVItEoWhigher hot-spot density [34]. 8 of 11 Figure 6. E.F. calculated at 488 nm laser excitation for (a) a dielectric formed by air and an Al2O3 barrier of the indicated thickness, (b) different pore fractions without barrier and (c) pore fraction of 20% and Figure 6. E.F. calculated at 488 nm laser excitation for (a) a dielectric formed by air and an Al2O3 Nanomaterials 2020, 10, x FOR PEER REVIEW 9 of 11 alumina barrier layer of 0, 2 and 5 nm. The horizontal green line corresponds to the experimental barrier of the indicated thickness, (b) different pore fractions without barrier and (c) pore fraction of E.F. value. 20% and alumina barrier layer of 0, 2 and 5 nm. The horizontal green line corresponds to the experimental E.F. value. Finally, 4 nm silver nanoparticles (NPs) were deposited [see Refs. 4 and 34 for the NPs characterization] onto the graphene layer on top of the membrane to check the possibility to further enhance the Raman signal of graphene and of an analyte. A schema of the resulting membrane based system is plotted in Figure 7a). In this case we used Rhodamine 6G (R6G) to test the amplification capability. Ag NPs were simultaneously deposited on the membrane platform and on the reference sample (fused silica/graphene) previously used and R6G was then deposited by spin coating. Ultra- small Ag NPs were used to preserve the transparency required for the interference process and because we recently demonstrated that, for the same plasmon absorption, the SERS effect is more efficient for these 4 nm NPs than for larger ones due to higher hot-spot density [34]. Optical images of the membrane and the fused silica surfaces are shown in Figure 7b,c. The R6G fluorescence is almost quenched allowing to easily detect the R6G Raman modes. In Figure 7d, a representative Raman spectrum obtained for the membrane/graphene/Ag NPs/R6G (pink curve) is compared to that for the fused silica/graphene/Ag Nps/R6G sample (dark blue curve). A 10−3 M solution of R6G was deposited by spin coating on both substrate which correspond finally to the equivalent concentration of one R6G monolayer on the substrates [4]. The spectra present the characteristic Raman peaks of R6G. In both cases the same SERS and CM amplifications are occurring so that the intensity increase in the membrane spectra is due to the interference process demonstrating the cooperative amplification of SERS and interference effects. Figure 7. (a) Schema of the membrane based amplification platform: supported membrane/graphene/Ag Figure 7. (a) Schema of the membrane based amplification platform: supported NPs/R6G, top view and cross section, (b) optical image of the Ag NPs region and (c) of the fused membrane/graphene/Ag NPs/R6G, top view and cross section, (b) optical image of the Ag NPs region silica/graphene/Ag NPs/R6G reference sample (images of 36 μm × 27 μm regions). (d) Typical R6G and (c) of the fused silica/graphene/Ag NPs/R6G reference sample (images of 36 μm × 27 μm regions). Raman spectra from both samples. (d) Typical R6G Raman spectra from both samples. Optical images of the membrane and the fused silica surfaces are shown in Figure 7b,c. The R6G is compared to that for the fused silica/graphene/Ag Nps/R6G sample (dark blue curve). A 10−3 amplification platforms to enhance the Raman signal of analytes by interference processes of the incoming and scattered light beams. The metallic aluminum support is used as the reflecting medium and the dielectric layer is the combination of the air of the pores and the alumina of the walls. Pore diameters in the 10–20 nm range are adequate to transfer a CVD single-layer graphene to serve as the substrate to deposit the analyte to be detected. Graphene mimics the membrane surface but presents a flat surface with small height fluctuations ~3 nm, which is found to be adequate for interference 4. Conclusions fluorescence is almost quenched allowing to easily detect the R6G Raman modes. In Figure 7d, a representative Raman spectrum obtained for the membrane/graphene/Ag NPs/R6G (pink curve) Supported alumina membranes where specifically designed and fabricated to be used asPDF Image | Supported Ultra-Thin Alumina Membranes with Graphene
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