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C: Physical Processes in Nanomaterials and Nanostructures

Macroscopic Vortex Induced Optical Activity in Silver Nanowires Daniel K. Kehoe, Joseph E McCarthy, John James Gough, A. Louise Bradley, and Yurii K. Gun'ko J. Phys. Chem. C, Just Accepted Manuscript • DOI: 10.1021/acs.jpcc.9b02965 • Publication Date (Web): 24 May 2019 Downloaded from http://pubs.acs.org on May 24, 2019

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The Journal of Physical Chemistry

Macroscopic Vortex Induced Optical Activity in Silver Nanowires Daniel K. Kehoe, †,‡ Joseph McCarthy, † John J. Gough,# A. Louise Bradley,# and Yurii K. Gun`ko†,‡* †

School of Chemistry, Trinity College Dublin, College Green, Dublin, D2, Ireland

‡BEACON,

Bioeconomy Research Centre, University College Dublin, D4, Ireland.

# School of Physics, Trinity College Dublin, College Green, Dublin, D2, Ireland

ABSTRACT: In this paper, for first time, we present vortex induced optical activity in Ag nanowires. We demonstrate that the handedness of the observed optical activity depends on the orientation of the applied vortex. Using alignment studies on the Ag nanowires we further confirm that the optical activity is due to the orientation and motion of the Ag NWs within the intrinsically chiral vortex. Our results provide fundamental insights in the behavior of nanowires in solution and understanding of optical activity in one dimensional (1D) nanostructures.

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1. INTRODUCTION Synthesis of optically active and chiral nanostructures has received a great deal of attention over the last decade.

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Chirality is of vital importance in biological systems, many of which interact

only with a specific enantiomer of a particular molecule. This is particularly important for pharmaceutical drug production 2 and natural systems which only involve single enantiomers of molecules. Synthetic routes for fabricating nano/micro scale materials have generally focused on utilising a chiral molecular functionality

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or chiral templates to imprint a ‘handedness’ on the

structure. 6 Another common route is to take advantage of shapes that have a natural chirality, such as helices. This brings to focus also the size scale of the chiroptical effect being observed for a particular structure. As highlighted, helical shapes have a natural handedness or chirality inherent in the structure, therefore they can be scaled to a supramolecular structure whose component building blocks may even consist of achiral entities. There are many reports of the utilisation of this method in producing chiral structures specifically with plasmonic properties.

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Plasmonic

nanostructures encompass a vast range of research applications and activities due to their unique optical and electronic properties. Specifically metallic plasmonic nanostructures have been used as enhancement and sensitising agents for emission, absorption and energy transfer applications, 14-16

surface enhanced Raman spectroscopy (SERS), 17 bio-sensing and in optical tweezing. 18

The use of stirring or mechanical vortex flow is one of the approaches to achieve symmetry breaking in achiral species and this is an area gaining increasing interest. 19-21 In fluid dynamics, a vortex is a region within a fluid where the flow mostly spins around an imaginary axis, either straight or curved. 22-23 Vortex and stirring induced chirality has been established and reported for several organic achiral molecular and supramolecular systems such as ionic oligomers, polymers,

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proteins,

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liquid crystals,

28-29

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and for self-assemblies of supramolecular


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aggregates. 23, 29-39 The vortex induced chirality effect has mainly been observed and reported for self-assembled structures such as J-aggregate systems. For example, it was previously reported that stirring vortex forces can induce optical activity in the stirring direction in J-aggregate structures. 40-41,42,43 In this case a macroscopic helical chirality was induced by the vortex stirring causing the observed chiroptical effect and not a molecular level intrinsic chirality. This was completely or partly attributed to linear dichroism (LD) and linear birefringence (LB) artefacts manifested in the circular dichroism (CD) measurements. 44 LD is related to the difference in the absorbance of the material for different polarizations of the incident light. The effect could also be observed in orientated dip coated films of the aggregates on a quartz slide showing the chiroptical observation was not purely a rotational phenomenon in solution. Ribo et al. 45 has also reported on this macroscopic chirality effect and broke down the contributions of the stirring forces on Jaggregates to show the LD and CD components. Further studies have shown this effect with Jaggregates to be induced not only by stirring but also with thermal 46 and sound 43 application, also circularly polarized luminescence was observed using J-aggregates with a conjugated dye present. 47

The use of stirring and vortexing for the preparation of chiral nanomaterials seems to be a very promising approach, but there are only a very limited number of literature reports in this field. For example, chiral nanofibers from graphene oxide, MoS2, TiS2, TaS2, TaSe2, WSe2, Pt-MoS2, PtrGO have been produced by vigorous stirring of solution of the corresponding ultrathin 2D nanomaterials in the presence of carbon nanotubes or AuAg nanowires using an achiral triblock copolymer (PEO20PPO70PEO20)-assisted self-assembly process.

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It was also shown that the

produced chiral nanofibers can be further transformed to same-handed chiral nanorings. Clockwise and counter-clockwise vortexing has also been used to tune the chirality of graphene oxide and


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transfer a handedness to achiral hosts molecules (tetrakis(4-N-methyl pyridyl)porphyrins).

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Using directional solvent evaporation from Mn-Doped ZnSe Nanorods vortex patterning of semiconducting nanorods was realised. 22 It has also been demonstrated that rotating vortex flows can be used to achieve chiral separation at the micro- and nanoscales. 20,50 Here we report the macroscopic optical activity effects in suspensions of plasmonic silver nanowires (Ag NWs) induced by vortex stirring. 2. RESULTS AND DISCUSSION Synthesis of high aspect ratio Ag nanowires The silver nanowires used in the study were produced using the ‘polyol’ synthesis, involving the reduction of silver nitrate by ethylene glycol in the presence of polyvinyl pyrrolidone (PVP) which acts as a structure directing agent during the synthesis to produce nanowire growth.

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Scanning

electron microscopy (SEM) analysis (Figure 1) shows Ag NWs with an average diameter of 83.4 nm and ranging up to several microns in length. The UV-Vis spectrum (Figure 1B) shows a typical absorbance profile for Ag NWs with peaks at 400 nm and 350 nm, which correspond to the transverse surface plasmon mode and plasmon resonance similar to that for bulk Ag , respectively. 52-54

The broadness of the peak can be attributed to variation in the nanowire dimensions.


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Figure 1. SEM image (A), UV-vis spectrum (B) with photograph of solution in-set and size distribution (C) of Ag NWs.

Effect of stirring orientation on induced optical activity As mentioned the stirring direction has a major role in defining the resulting optical activity expressed by the NWs. For the purpose of our studies all analysis was done using 20 mm diameter sample tubes as vessels, 140 mm magnetic stirring bar and the same stirring mantle (a Sigma Aldrich S46). In the case of clockwise (CW) stirred Ag NWs a modified magnetic stirring mantle was used under the same conditions. CD analysis of CW and anti-clockwise (ACW) stirred Ag NWs is shown in Figure 2. CD is measured as the difference between the extinction of left ciriclarly polarized (LCP) and right circularly polarized (RCP) light through the nanowire sample. In order


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to remove any discipency from concentration effects for the difference in absorbance bewteen RCP and LCP light, the CD is also presented in terms of G factor.

Figure 2. CD spectra of CW and ACW stirred Ag NWs expressed in mdeg (A) and G-factor (B) and time monitored CD spectra (C) of Ag NW monitoring the relaxation of the CD signal after 10 minutes of only ACW stirring and the associated plot of the change in CD signal over time.

The CD spectra (Figures 2A and B) showed optical signals of equal and opposite sign for the CW and ACW stirred NWs in the plasmonic region of the NWs. The spectral feature noted at 550 nm in the case of the ACW solution was regularly observed in these studies and is most like a result of scattering due to a disalignment of the some Ag NW in solution.55 The ACW stirred NWs showed a trend to produce (-) CD signals while CW stirred NWs tended to show (+) signals. This


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stirring induced chiroptical activity compliments the extensive work carried out by Ribo et al. 24, 56-57

with J-aggregates. However, the exact origin of this optical activity still remains in question,

with many reports in the field stating that this observed CD signal is an artifact arising from the partial alignment, in our case of the NWs, with the vortex which is intrinsically chiral, resulting in a macroscopic chiral arrangement.19, 21, 25, 58 Our time monitored CD study (Figure 2C and D) of a solution of Ag NWs after 10 minutes of only ACW stirring, further highlights how the observed CD signal for these NWs fluctuates and diminishes in intensity as the vortex flow relaxes over time, which further indicates that it may be due to alignment artefacts. Previously, hydrodynamic forces have been shown to induce chiral deformation.23, 49, 59 Theoretically, this CD originating mechanism is possible and was previously modelled for a system of long helices made of plasmonic nanocrystals. 13 However, in our case SEM analysis (Figure 3) showed no any physical change or chiral deformation such as helices in the NWs.

Figure 3. SEM image of Ag nanowires dried after 10 mins of ACW stirring.

We explored this further by drying a concentrated aliqout of the Ag NWs while continuously stirring them on a glass slide. SEM analysis (Figure 4) again showed no chiral deformations


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however in this case the NWs showed a very distinct alignment (i.e. NWs orientated in same direction) due to the stirring. In light of this we propose that the observed chiroptical activity is most likely due to the specific orientation and alignment of the NWs with the vortex. 21, 25

Figure 4. Photograph of the final dried film of Ag NWs (A) and SEM image (B) of Ag NWs dried on a glass slide while continuously stirring ACW.

CD analysis of aligned Ag NWs In order to investigate the origin of the chiroptical activity further alignment studies were performed. The Ag NWs in solution were aligned on a quartz substrate using a three-phase interface method. The method allows for the spontaneous alignment of aqueous Ag NWs in an oilwater-air interface. Aligned and unaligned NWs are presented in Figure 5.


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Figure 5. Unaligned (A) and aligned (B) Ag NWs on a quartz substrate viewed through a 50X microscope objective.

The optical activity of the aligned NWs was then assessed by using a linear polariser in combination with a quarter-wave plate to convert the light incident on the sample to circularly polarized light. Measurements of the CD response to both right (RCP) and left circularly polarized (LCP) light were recorded (Figure 6).


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Figure 6. Absorption spectra of the aligned Ag NWs on a quartz substrate using left and right circularly polarized light.

As shown in Figure 6 there is no difference in the absorption of left and right circularly polarized light for the aligned Ag NWs. Since there is no chirality associated with these structures, and the region measured was perfectly aligned, it was expected that there would be no optical activity. This result confirms that the chiroptical activity observed for these NWs is due to the orientation and motion in the intrinsically chiral vortex rather than chiral deformation of the Ag NWs.

Linear dichroism and Polarisation Resolved Absorption of Silver Nanowires Then, we performed linear dichroism (LD) studies on stirred solutions of Ag NWs of different concentration to further assess the origin of the observed optical activity. Upon stirring (ACW) both the low concentration ( ~ 20 mg) (Figure 7A) and the high concentration (120 mg) (Figure 7B) solutions of Ag NWs demonstrated LD activity, with both samples showing an increase in LD signal with increasing revolutions per minute (RPM). Comparison of the CD and the LD


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spectrum (Figure 7C) for the higher concentrated NW solution shows identical spectral profiles. These result further indicate the Ag NWs align with the torsional flow of the intrinsically chiral vortex. The interaction between an electromagnetic wave and a medium depends on the angle between the polarization axis of the electromagnetic wave and the axis of the dipole oscillation in the medium. This is provided that there is asymmetry in the axis of the material to allow for a polarization dependence. There is an obvious anisotropy in these nanowires which can be observed in the absorption measured as a function of the polarization of the incident light, displayed in Figure 7D.

Figure 7: LD studies of lower concentration (A) and high concentration (B) at various RPM, Comparison of LD and CD spectra for high concentration Ag NWs (C) and polarization resolved response of the aligned Ag NWs as the polarizer was moved through 90 degrees in 15 degree increments (D).


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The linear polarization resolved measurements showed clearly that the Ag NWs are aligned. The polarization dependence of the absorption spectrum that is illustrated in Figure 7D. When the incident light is polarized perpendicular to the long axis of the Ag NW the absorption below 400 nm is higher due to excitation of the transverse mode resonance. This corresponds to a polarization of 90o in Figure 7D. As the incident polarization is rotated to 0o, along the length of the nanowire, the absorption at in the region of the transverse plasmon mode decreases.

3. EXPERIMENTAL SECTION Synthesis of large aspect ratio Ag nanowires Ag NWs were synthesized using a typical polyol synthesis procedure.51 PVP (0.2 g, 55000 wt) was added to ethylene glycol (25 mL) and sonicated until completely dissolved. AgNO3 (0.25 g) was then added into the PVP solution and sonicated for 30 sec. Finally 3.5 g of a FeCl3 solution (600 µM) dissolved in ethylene glycol was then added into the above solution. The resulting mixture was then added into a preheated reaction vessel at 130 ℃ and heated for 5 hours. The solution was then allowed to cool to room temperature and washed with acetone and ethanol followed by centrifugation (9000 rpm, 30 min) three times. The precipitated nanowires were then re-dispersed in ethanol. Alignment of Ag nanowires The Ag NWs were aligned on a solid quartz substrate using a three phase interface method1 followed by a controlled dip coating procedure. In order to carry out smooth, controlled immersion of the slides in the solution, a KSV NIMA Small Multi Vessel Dip Coater was used. Following the immersion and removal of the substrate from the solution, the substrates were left to air dry in the fume-hood.


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Characterization CD spectra were recorded on a Jasco J-815 using quartz cuvettes with an optical path length of 1 cm. LD measurements were performed using a Jasco J-815 with an LD attachment at 25 ℃. SEM images were taken using a Zeiss Ultra Plus microscope.

4. CONCLUSIONS In conclusion we showed for the first time, vortex induced optical activity of large aspect ratio Ag NWs. Through the use of alignment, CD, LD and polarization studies we confirmed that the induced optical activity observed is a result of the orientation and motion of the Ag NWs with the intrinsically chiral vortex rather than chiral deformation of the NWs. By changing the direction of the vortex (i.e. ACW or CW) it is possible to produce opposite LD and CD signals. We believe that these studies provide fundamental insights in the behaviour of nanowires in solution and understanding of optical activity in 1D nanostructures.

AUTHOR INFORMATION Corresponding Author *E-mail: [email protected] (Y.K.G.). Notes The authors declare no competing financial interest.


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ACKNOWLEDGMENT We acknowledge School of Chemistry (Trinity College Dublin), Science Foundation Ireland (SFI) under grant numbers 12/IA/1300, 16/IA/4550 and Bioeconomy SFI Research Centre (grant number SFI 16/RC/3889) for financial support.

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