Dual Polarised Surface Plasmon Coupled Emission Tuning of Rhodamine B on SPR Metal Sensors

doi:10.21203/rs.3.rs-5293189/v1

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Dual Polarised Surface Plasmon Coupled Emission Tuning of Rhodamine B on SPR Metal Sensors

https://doi.org/10.21203/rs.3.rs-5293189/v1

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Surface plasmon coupled emission steering and emission tuning (SPCET) were demonstrated from metal-dielectric bi-layered structures in Reverse Kretschmann configuration. Rhodamine B dye doped Poly Vinyl Alcohol emissive layer was deposited on top of metal thin films (Silver, gold and copper) to realise bi-layered SPCET sensors. Apart from conventional p-polarised emissions, all sensor chips showed s-polarised emissions as well. These dual polarised emissions indicate a strong correlation between surface plasmon resonance and SPCET. Thickness of the dielectric layer show a major impact on the correlation between surface plasmon resonance and SPCET. Both p- and s- polarised emissions showed spectral narrowing. For thicker dielectrics, a decrease of 42% in the emission peak width was observed for p-polarised modes and was observed to be a constant for all metal sensors.

Surface plasmon resonance

coupled emission

sensors

emission tuning

multilayers

thin films

Surface plasmon resonance (SPR) based biosensors are extremely potent instruments for the investigation of physical, chemical, and biological areas^1–3. Using SPR biosensors, both malignant and viral infections might well be addressed⁴. In addition to being employed for biosensing, the SPR method has also been used to characterise a bunch of material thin films⁵. Photoluminescence is the emission of light with a greater wavelength or lower energy which is caused by the irradiation of a material with radiation and this occurrence is known as fluorescence. Surface plasmon-assisted fluorescence techniques, such as surface plasmon-enhanced field fluorescence spectroscopy (SPFS), surface plasmon coupled emission (SPCE), and SPCE imaging (SPCEi), undergo a paradigm shift because of the integration of the SPR methods with fluorescence techniques^6–8. The fusion of SPR with fluorescence emission has facilitated fluorescence imaging, molecular detection, and clinical diagnostics^9–11. Surface plasmon-assisted fluorescence techniques are effective for detection and furnish qualitative proof of molecular existence, but their quantitative aspects are insufficient. However, near field interactions of fluorescence with thin metal films through plasmon coupled emission (PCE)^12–13 are of interest because of their fluorescence intensification, modulation, steering, and directionality centred on Reverse-Krestchmann (RK) configuration^14–17.

The phenomena of excited fluorophores coupling with the surface plasmon resonance seen in thin metal films, particularly in silver, gold, aluminium, or copper of nearly 50 nm thickness, is known as surface plasmon coupled emission (SPCE). When fluorophores are a few nanometres apart from a metal surface, they produce directed emission over a narrow angle distribution instead of the usual isotropic emission¹⁸.The techniques for evoking surface-plasmon-coupled emission (SPCE) comprise direct excitation of a fluorophore thin film spread over a metal nanolayer (Kretschmann configuration) or irradiation of the sample through a glass prism and metal film (Reverse Kretschmann configuration)^19–20. Due to the exclusive collection of emitted light at the bio-affinity surface, the process pertaining to fluorophores and surface plasmons coupling only occurs therein, accordingly SPCE sensors have a high sensitivity.

Due to their strong plasmon oscillations within the visible region, metals like silver (Ag) and gold (Au) thin films are extensively utilized for SPR applications, but they are very expensive. There are several reports on SPCE involving Ag and Au²¹ based SPR sensors, but relatively a few works on Copper (Cu) based sensors²². Copper metal is less expensive, has superior SPR characteristics for a wide range of thin film thicknesses, exhibits great optical qualities, and is readily accessible when compared to Ag and Au²³. In the present work we have explored the possibilities of SPCE emission from Ag, Au and Cu based SPR sensors. we have also investigated surface plasmon coupled emission tuning (SPCET) studies in Ag, Au and Cu thin films in RK configuration. In addition to the SPCET of p-polarization in Ag thin films as reported by Resmi K R et al.²⁴, here we observed dual polarised SPCET from silver, gold and copper sensor substrates. These dual polarised plasmon coupled emissions in combination with the conventional reflection based SPRs could complement the sensing properties and hence could extract more information related to sensing as compared to SPR sensors.

SPR occurs when light is incident on a thin metal film through a hemicylindrical or triangular prism. Schematic of SPR excitation is shown in Fig. 1(a). We obtain a total internal reflection at the prism interface above critical angle using an angle tailored reflection spectrum. Thus, we normally forecast substantial reflectivity at incident angle beyond total internal reflection. But, due to the evanescent waves, free electrons within the metal oscillate generating surface plasmons. The oscillations hit their peak when the incident angle (θ_I) meets with the SPR angle (θ_sp), where the most incident radiation is absorbed. The incident wave vector's in-plane component matches the surface plasmon wave vector at this angle of incidence. This requirement is a result of solving Maxwell’s equation for the boundary conditions that the in-plane component of the electric field must be continuous across the interface. The following equations provide the in-plane component of the incident wave vector and the wave vector for plasmon oscillations:

$$\:{k}_{x}={k}_{o}{n}_{p}{sin}{\theta\:}_{I}$$

and $\:{k}_{sp}={k}_{o}{\left(\frac{{\epsilon\:}_{m}{\epsilon\:}_{s}}{{\epsilon\:}_{m}+{\epsilon\:}_{s}}\right)}^{1/2}$ (2)

respectively, where ε_m is the dielectric constant of the metal (m) and ε_s is the effective dielectric constant at the metal/PVA interface. When the surface plasmon wave vector as well as the light wave vector are matched, SPR absorption occurs and the requirement is given by

$$\:{k}_{sp}={k}_{x}={k}_{o}{n}_{p}{sin}{\theta\:}_{sp}$$

This is achieved by tuning the angle of the incident light, θ_I.

experimental setup for PCE studies and (c) Absorption and emission spectra of Rhodamine B.

Thin films of Silver (Ag), Gold (Au) and Copper (Cu) (thickness ~ 50 nm) were deposited on cleaned glass substrates by sputtering. Different weight percentages of Poly Vinyl Alcohol (PVA) were dissolved in de-ionized (DI) water and heated at 90°C to create viscous PVA solutions of different concentrations. Rhodamine dye solutions were prepared by dissolving 0.5, 1, 1.5 and 2wt% of RhB in DI water. RhB solutions were then mixed with the prepared PVA solutions to generate PVA + RhB solutions. Thin and thick films of PVA + RhB were deposited on top of metal thin film (Ag, Au and Cu) by spin coating PVA + RhB solutions. Based on the thickness of PVA + RhB layers and the metal on which the PVA + RhB films were coated, the samples were named as Ag220, Ag600, Au70, Au270, Au590, Cu200, and Cu550. To estimate thickness of thin films, the complex index of refractions of the metals and the polymer were used to simulated transmission spectra by transfer matrix model methods²⁵ and were compared with their corresponding experimental transmission spectra.

Figure 1(b) shows the experimental setup to investigate SPCE/SPCET. Using an index-matching fluid, (glycerine, n = 1.5), the SPCE sensors were integrated to a hemicylindrical prism. A diode laser of wavelength 532 nm was incident normally on the prism coupled SPCE sensor in reverse Kretschmann configuration to excite the dye molecules. The SPCE emission generated from the setup were collected and recorded by a compact high sensitivity spectrophotometer (Make: Ocean Optics, Model: Maya2000Pro). The prism coupled SPCE sensor was mounted on top of a rotational stage with necessary collection optics to capture angle tuned SPCE spectra.

Free spectral emission (FSE) of RhB molecules were collected from RhB + PVA films coated on glass substrates using the SPCE setup as mentioned above without prism coupling. On exciting the molecules at 532 nm, FSE were observed at wavelengths above 550 nm. A broad spectrum spanning in the range of 550 nm to 750 nm was recorded and is presented in Fig. 1(c). The same dye molecules in the vicinity of metal thin films show different pattern as compared to its FSE. To observe this variation, RhB + PVA films were coated on top SPR metal sensors Ag, Au and Cu and their respective SPCE spectra were recorded and analysed. SPCE spectra for silver based SPCE sensor with RhB + PVA film thickness of 220 nm (Ag220) was first studied in detail. The spectra were collected at angles from 20⁰ to 80⁰ with an interval of 1⁰. It was observed that the emission was only for a few angles between 40⁰ and 45⁰ and no emission was observed for other angles. It shows a highly anisotropic emission as compared to its free spectral emission which was isotropic in nature.

All the collected SPCE spectra were organised as a matrix with wavelength along x-direction, angle along y-direction and emission intensity as colour scale along z-direction. The same is presented as an image plot in Fig. 2 (a). A controlled emission within 40⁰ and 45⁰ was evident in the image plot. SPR reflection curves were generated by transfer matrix model simulations²⁵ to correlate the SPCE emission with the SPR reflection. On comparing the emission spectra of Ag220 with its simulated SPR reflection image (Fig. 2. (b)), it is evident that the emission steering matches well with the p-polarised dispersion curve between 40⁰ and 45⁰. The SPR image (Fig. 2(b)) also shows s-polarised dispersion curve between angles 48⁰ and 58⁰ which is missing in SPCE image (Fig. 2(a)). This might be due to the weak coupling of emission with the corresponding s-polarised SPR.

SPCE emission spectra for the angles between 42⁰ and 47⁰ is presented in Fig. 2(c). On analysing individual spectra obtained in between 42⁰ and 47⁰ we could see that the peak wavelengths differ from its FSE. Peak wavelength of FSE of RhB was at 600 nm and for the SPCE spectra at 42⁰ it was at 650 nm (Fig. 2(c)). As the angle was increased from 42⁰ to 43⁰ the peak wavelength shifted to 625 nm. The peak shit decreased as angle increased from 42⁰ to 47⁰. Once the peak shift reached 600 nm then no further shift was observed. On comparing SPCE with FSE emission intensity, more than an order of magnitude in emission intensity was evident. In contrast to emission peak intensity enhancement the full width half maximum (FWHM) of SPCE emission was observed to be reduced as compared to FSE emission. The observed emission tuning and steering in SPCE matches exactly with the simulated SPR curves and hence a perfect correlation between SPCE and SPR could be confirmed. The emission tuning confirms a strong coupling of dye molecules with the plasmons within the metal dielectric interface. Figure 2(d) show polar plot of the SPCE emission at different angles for a particular wavelength (610 nm) (corresponding to peak FSE wavelength) which confirms the SPCE emission directionality. Thus, from our studies, the plasmon coupled emission shows emission tuning apart from the typical emission steering effects reported previously¹⁸.

Further studies on SPCE tuning were carried out to examine the effect of the emission tuning on the thickness of the dielectric layer. Figure 3(a) shows the experimental SPCE image plot of Ag600 (t = 600 nm) in RK configuration and Fig. 3(b) shows the corresponding simulated SPR image.

The results of the sample Ag600 are shown in Fig. 3. For dielectric layer thickness less than 200nm we could observe only p-polarised emission. As the thickness was increased to 600 nm both s-and p-polarised emission were dominant (Fig. 3(a)). Thus, dual polarised SPCE could be realised for thicker dielectric layers. As thickness of the dielectric layer increases multimode SPCE were observed for both s and p polarised emissions (Fig. 3(b)). The number of SPCE emission modes exactly matches with the simulated SPR reflection images as shown in Fig. 2(a) and Fig. 2(b) respectively. It is to be noted that as compared to Ag220 where we could observe only p-polarised mode, in Ag600 we could observe that both s- and p-polarised modes were prominent with considerable emission intensity. All the modes show SPCE tuning apart from emission enhancement and emission steering. S1 and S2 modes tune between 42⁰ and 44⁰ and between 58⁰ and 62⁰ respectively. P1 and P2 modes get tuned between 46⁰ and 52⁰, and between 64⁰ and 70⁰ respectively. Corresponding to the angular tuning, emission peak wavelength also gets tuned as follows. The first plasmonic mode S1, shows SPCE tuning from 570 nm to 670 nm for an angular span of 2⁰, the second mode P1, shows SPCE tuning from 560 nm to 680 nm for an angular span of 6⁰. Similarly, the S2 mode shows a tuning from 590 nm to 750 nm for 4⁰ shift and P2 mode shows a tuning from 580 nm to 830 nm for an angular span of 6⁰. In addition to the observed emission steering and tuning, SPCE enhancement was also prominent in Ag600. These observed results confirm that the surface plasmon coupling gets improved on increasing dielectric thickness of the sensor chip. The enhancement in SPCE intensity reveals that the p-polarisation modes have better plasmon coupling than the s-polarisation modes. These observations again support the direct correlation between SPCE and SPR and the effect of SPCE on the dielectric thickness coated on the SPR sensor chips. Figure 3(d) presents the polar plot of Ag600 at 610 nm wavelength, which confirms dual polarised emission apart from the emission steering, tuning and enhancement as compared Ag220. The increase in sharpness of these lines with thickness is due to strong plasmon coupling. In our previous work we could observe only p-polarised mode SPCE for all the dielectric layer thicknesses (210 nm to 690 nm). In our present studies we could observe dual polarised SPCE emission and emission tuning. We have detected two modes for both S and P polarisations when the sample thickness was increased from 220nm to 600nm. The observed emission results had a direct correlation with the simulated SPR image (Fig. 3(b)).

SPCE investigation studies were extended on gold and copper SPR metal sensors. Dielectric layer thickness of 70, 270 and 590 nm on Au were coated for the SPCE studies (named as Au70, Au270 and Au590). The results of Au70 are shown in Fig. 4. The experimental image plot of the sample Au70 and its simulated SPR image are shown in Fig. 4(a) and Fig. 4(b) respectively. The SPCE from Au70 sample was observed to be highly directional and it shows tuning effect (SPCET). Results show only p-polarised SPCE and the emission peak was observed to be tuned from 780 nm to 560 nm as the angle of detection was varied from 50⁰ to 75⁰. As the samples thickness was very thin, plasmon coupling effects were feeble and hence the SPCE studies showed low emission intensities. The Fig. 4(c) represents plasmon coupled emission curves extracted from the image plot (Fig. 4(a)) between angles 50⁰ and 75⁰ and Fig. 4(d) represents the angle scanned SPCE of the sample as a polar plot.

Thicker dielectric layers on Au metal films were also investigated to compare the higher order SPCE modes. The image plot and its simulated SPR image of Au270 are shown in Fig. 5(a) and Fig. 5(b) respectively. Similar to Ag metal sensors, Au also showed dual polarised surface plasmon coupled emissions. On comparing simulated SPR image (Fig. 5(b)) with the SPCE image (Fig. 5(a)), it was evident that the two SPCE emissions in the angular regions 42⁰ to 48⁰ and 56⁰ to 66⁰ corresponds to p and s polarised emissions respectively. Tuning was observed for both s- and p-polarised emissions. For s-polarised emission the peak emission got tuned from 580 nm to 750 nm for an angular span of 6⁰. For p-polarised emission, the emission peak got tuned from 610 nm to 720 nm for an angular span of 10⁰. Moreover, p-polarised mode showed higher emission intensity as compared to the s-polarised mode. SPCE curves extracted from the image plot between angles 40⁰ and 70⁰ are presented in Fig. (5(c) and polar plot of the same is presented in Fig. 5(d). As in the case of SPCE from silver-based metal films SPCE from gold-based metal films also showed an emission enhancement for thicker dielectric layer. As compared to Au70, where the dielectric layer thickness was only 70 nm, Au270 (dielectric layer thickness ~ 270 nm) showed 400% increase in the SPCE. These results confirm the nature of strong plasmon coupling for metal sensors with thicker dielectric layers is applicable for gold metal sensors as well.

We have also explored SPCE on thicker dielectric layer, sample named Au590. The experimental image plot of the sample Au590 and its simulated SPR image are shown in Fig. 6(a) and Fig. 6(b) respectively. In the simulated SPR image (Fig. 6(b)), we could observe two s-polarised plasmonic modes for Au590: S1 at 42⁰ and S2 at 62⁰. Both exhibited tuning effect, and the later has better tuning from 560 nm to 750 nm for an angular span of 9⁰. Similarly, there are two p-polarised plasmonic modes: P1 at 55⁰ and P2 at 75⁰ also exhibited PCE tuning. On comparing these SPR results (Fig. 6(b)) with the SPCET results (Fig. 6(a)), we could see that the SPCE emission of s-mode and p-mode were integrated to give a single curve. This might be due to the broad emission of both s- and p-polarised emission which appeared closely together due to increase in the thickness of the dielectric and hence an overlap of these peaks resulted into a single peak. But for higher modes, i.e. for S2 and P2, both the modes were well separated in the SPR image and hence the peaks were expected to be resolved in SPCE image. We could see a prominent S2 mode in the SPCE image, but was not able to capture the P2 mode which might be because P2 appears in the higher angular region as shown in Fig. 6(b). The Fig. 6(c) shows the SPCE curves extracted from image plot for the angles between 40^o and 70^o confirms the tuning of both plasmonic modes. The Fig. 6(d) represents the polar plot of the sample Au590. Apart from dual polarised modes, number of modes got increased with increase in thickness of the dielectric layer. The SPCE intensity of p-polarised emission is more prominent than s-polarised emission. The simulated plot in Fig. 6(b) confirms this observation. Like the sample Au270, a SPCE enhancement of about 300% and emission tuning were also detected in Au590. Thus, a correlation between sample thickness and SPCE enhancement has been confirmed.

Further we investigated SPCE studies on two Cu samples, Cu200 and Cu550. The experimental image plot of the sample Cu200 and its simulated SPR image are shown in Fig. 7(a) and Fig. 7(b) respectively. Unlike Ag and Au samples, dual polarization modes were observed in the SPCE spectra of thin Cu sample. SPCE curves extracted from the image plot are shown in Fig. 7(c). For Cu200, the directionality of SPCE and SPCET were seen in the image plot. The polar plot of Cu200 is given in the Fig. 7(d), which demonstrated the SPCE steering similar to Ag220.

Figure 8(a) and 8(b) represent the experimental SPCE spectral image of the sample Cu550 and its simulated SPR image respectively. SPCE curves corresponding to s and p-polarizations of Fig. 8(b) were observed in Fig. 8(a). The extracted SPCE curves from the image plot are shown in Fig. 8(c). There are three SPCE modes at angular regions: 41⁰ to 44⁰, 46⁰ to 54⁰ and 58⁰ to 65⁰, and they are named as P1, S1 and P2 respectively. Mode Pl shows a PCET from 570 nm to 650 nm with an angular span of 3⁰ and S1 shows a PCET from 580 nm to 760 nm for an angular span of 8⁰. Similarly, the P2 has a PCET effect from 600 nm-720 nm for an angular span of 7⁰. Due to weak plasmon coupling the SPCE due to S2 mode was not observed. On increasing the dielectric thickness, we could observe PCET in Cu samples too as in the case of Ag and Au samples.

The Full Width at Half Maximum (FWHM) values of different SPCET modes of the samples investigated are tabulated in Table.1. Dual polarised plasmonic modes were observed for all metal sensors but are more prominent for metal sensors with thicker dielectric layers as compared to thin dielectric layers. The TWHM of P-polarised modes were observed to be sharper than that of S-polarised modes. FWHM were also compared between sensors with thick and thin dielectric layers. The FWHM values were high for thin dielectric layers but got decreased for thicker dielectric layers. It was interesting to note that there was a decrease of ~ 42% in the FWHM values of P-polarised emission modes for samples with thick dielectric layers as comparison to the samples with thin dielectric layers. Moreover, a 42% decrease in FWHM was found to be a constant in case of all the studied metal sensors. The strong plasmon coupling thus influenced in narrowing the emission by a constant factor of 42%.

Table 1

FWHM values of the SPCET modes (P and S represents P-pol and S-pol respectively and 1,2 are plasmonic mode numbers)
Sl.No.	Sample	Experimental FWHM (nm)
1	Ag220	71 (P1)	-	-	-
2	Ag600	60 (S1)	30 (P1)	94 (S2)	28 (P2)
3	Au70	85 (P1)	-	-	-
4	Au270	56 (S1)	36 (P1)	-	-
5	Au590	67 (S1)	36 (P1)	72 (S2)	34 (P2)
6	Cu200	37 (S1)	90 (P1)	-
7	Cu550	49 (S1)	38 (P1)	102 (S2)	38 (P2)

Surface plasmon coupled emission and emission tuning (SPCE and SPCET respectively) were demonstrated using Silver (Ag), Gold (Au) and Copper (Cu) as metal films and Rhodamine B (RhB) dye doped Poly Vinyl Alcohol (PVA) as dielectric layer. Samples were coupled to a hemicylindrical prism in Reverse Kretschmann (RK) configuration to demonstrate SPCE and SPCET phenomena. Due to surface plasmon coupling, an emission steering was detected for lower dielectric thicknesses and emission steering and tuning together for higher dielectric thicknesses. The dielectric layer thickness had a significant impact on PCET. The higher plasmonic modes show good emission tuning with respect to the angular tuning. Dual polarised (both S- and P-) emissions were observed for thicker dielectric layers on top of all the studied metal sensors (Ag, Au and Cu). Dual polarised emission observed in Cu metal sensors even for thin dielectric layer on top of the Cu metal films make Cu unique from Ag and Au metal films. The number of plasmonic modes were increased with increase in dielectric thickness on top of Ag, Au and Cu metal films. Ag films were found to have an emission peak shift of 270 nm for an angular span of 6°, Au films were found to have an emission peak shift of about 190 nm for an angular span of 9^o and Cu films to have an emission peak shift of 120 nm for an angular span of 7°. In addition to the SPCE steering and tuning there was an enhancement in the SPCE intensity for thicker dielectric layers on top of Ag, Au and Cu films. It was interesting to note that there was a decrease of ~ 42% in the FWHM values of P-polarised emission modes for samples with thick dielectric layers as comparison to the samples with thin dielectric layers. Moreover, a 42% decrease in FWHM was found to be a constant in case of all the studied metal sensors. These dual polarised plasmon coupled emissions in combination with the conventional reflection based SPRs could complement the sensing properties and hence could extract more information related to sensing as compared to SPR sensors.

Author Contribution

All authors contributed to the study, conception and design. Data collection and analysis were performed by Ajeesh P. Vijayan, A. Sreelakshmi, Fasna Sharin, Kuppathil R. Dhandapani, and Pradeesh Kannan. The first draft of the manuscript was written by Ajeesh P Vijayan and all authors commented on previous versions of the manuscript. All authors read and approved the final manuscript.

Acknowledgement

Authors acknowledge DST-FIST India (No: SR/FST/College-325/2016(c)) for the funding provided to our institution. Authors acknowledge DCE, Kerala, India for the fund provided to our institution under Centre of Excellence head. A. Sreelakshmi, Fasna Sharin thank KSCSTE, Kerala, India for providing financial assistance under student project scheme (00636/SPS 65/2021/KSCSTE). A portion of this work was supported by INUP-i2i at IISc Bangalore funded by the Ministry of Electronics and Information Technology (MeitY). The work was performed using Facilities at CeNSE, Indian Institute of Science, Bangalore, funded by Ministry of Education (MoE), Ministry of Electronics and Information Technology (MeitY), and Nano mission, Department of Science and Technology (DST), Govt. of India.

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Dual Polarised Surface Plasmon Coupled Emission Tuning of Rhodamine B on SPR Metal Sensors

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Abstract

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1. Introduction

2. Theory of Surface Plasmon Resonance (SPR)

3. Materials and Methods

4. SPCE experimental setup

5. Results and Discussion

6. Conclusions

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Author Contribution

Acknowledgement

References

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