Far-Field Plasmonic Resonance Enhanced Nano-Particle Image Velocimetry Within A Micro Channel

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Far-Field Plasmonic Resonance Enhanced Nano-Particle Image Velocimetry

within a Micro Channel

Zhili Zhang*, Quanshui Li, Sara S. Haque, Mingjun Zhang

Department of Mechanical, Aerospace and Biomedical Engineering, University of Tennessee,

Knoxville TN 37996

*To whom correspondence should be addressed: Zhili Zhang (zzhang24@utk.edu)

Abstract

In this paper, a novel far-field plasmonic resonance enhanced nanoparticle-seeded Particle Image

Velocimetry (nPIV) has been demonstrated to measure the velocity profile in a micro channel.

Chemically synthesized silver nanoparticles have been used to seed the flow in the micro channel.

By using Discrete Dipole Approximation (DDA), plasmonic resonance enhanced light scattering

has been calculated for spherical silver nanoparticles with diameters ranging from 15nm to

200nm. Optimum scattering wavelength is specified for the nanoparticles in two media: water

and air. The diffraction-limited plasmonic resonance enhanced images of silver nanoparticles at

different diameters have been recorded and analyzed. By using standard PIV techniques, the

velocity profile within the micro channel has been determined from the images.

1. Background

In the area of fluid mechanics and aerodynamics, velocity field is one of the most important

physical parameters [1, 2]. However the velocity measurement is not trivial, especially for

boundary layers or micro channels in which inherent compressibility effects, temperature and

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density gradient make the direct measurement of velocity somewhat more difficult. The existing

flow diagnostic techniques are not well suited for such measurements. Pilot-static pressure

probes, Hot Wire Anemometry (HWA) [3], Laser Doppler Velocimetry (LDV) [4, 5], Molecular

Tagging Velocimetry (MTV) [6-9], Particle Image Velocimetry (PIV) [2, 10-12] and micron

resolution PIV (µPIV) [13-16] etc. have many limitations for the purpose of such measurement.

The pilot-static probe is ineffective because of the inherent wave structure created by the probe.

It also requires additional measurements of temperature or density to calibrate the flow

conditions. The hot-wire probe becomes sensitive to the local mass-flux and total temperature.

Hence, data acquisition and data-reduction procedures are subsequently more challenging, and

velocity cannot be measured directly. Although non-intrusive laser-based techniques, such as

LDV, PIV and µPIV can provide direct measurement of the velocity in such flows, all methods

require seeding particles of large dimensions added to the flow. Due to the inertial effects of the

particles, they may not be able to track the flow accurately, especially across the shock wave or

the near wall region within the boundary layers. PIV has a significant degrading effect with

increasing particle size [17]. As a comparison, MTV tags air or other molecules themselves and

thus is able to follow rapid transitions: a shock wave in the flow. Of course no global information

can be obtained through MTV due to the limited tagging regions. In a universal point of view,

seeding particles in MTV are molecules which are on the order of a few Angstroms and have

perfect tracking property. While particles used in LDV and PIV are artificially injected which

are on the order of 100nm to tens of microns, they may not be able to track the flow perfectly.

A unique opportunity to resolve some of these difficulties is offered by a novel experimental

technique, nano-Particle Image Velocimetry (nPIV). Nanoparticles have many unique properties:

some of them may not even be well described by traditional theories in physics and mechanics

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due to the breakdown of the scale law [18]. Among the properties, the plasmonics-enhanced light

scattering and fluorescence emission can significantly improve nanoparticles’ visibility without

increasing their size and weight [19, 20]. According to Stokes’ theorem, as particles dimension

and weight decrease, particle response time to the flow conditions becomes shorter and flow

tracking capability gets better [21]. For example, PIV measurement have been successfully

conducted in hypersonic flows (M = 7) by TiO2 nanoparticles at diameters of ~50nm [22] and

shock boundary layer interactions by TiO2 nanoparticles at diameters of ~170nm [23], which are

not possible at all for common micron-sized particles. However, the spatial resolution of those

measurements is still insufficient to determine the near wall flow properties. Smaller

nanoparticles will be able to track the boundary layer flows at a more detailed manner. As an

example, natural seeding of condensed H2O and CO2 particles at diameters of ~10 nm has been

successfully used in the hypersonic boundary layer measurement [24]. Obviously natural seeding

is limited to flows at certain conditions and cannot approach the near wall region of the

supersonic boundary layers. This is because the condensed H2O and CO2 particles are evaporated

in the region at high temperatures.

2. Flow Seeders

2.1 Size of the seeders

First, light scattering from a particle, either Mie or Rayleigh scattering, can be calculated from

Mie scattering theory, which reveals that light scattered by a particle is proportional to the square

of its volume. The cross section σ of light scattering can be expressed as [25, 26]

2
 m
  24 V3 2
(1)
  2 m

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where V is the volume of the particle, ε is the dielectric constant of the particle, and εm is the

dielectric constant of the surrounding. The light scattering power P is the product of the cross

section and incident light intensity I, P  I . So in the light scattering, large particles always

dominate smaller ones. When radius of the particles decreases by a factor of 100, for example

particles at diameters of 10 nm instead of 1 µm, the scattering power will decrease by 1012. The

light scattering from the nanoparticles is weak and difficult to be measured. It will be extremely

hard to collect light scattering from nanoparticles if large dust particles are present. Table 1

shows typical scattering cross sections of particles as a function of the particle size. In general,

the smaller the particle is, the more difficult for it to be detected by Mie/Rayleigh scattering.

Table 1. Scattering cross sections of particles as a function of diameters

Particles diameters Scattering cross section (cm2)

Air molecules at 0.3nm [26] 10-26-10-28

CO2 cluster at 10nm [27] 10-17

Seeding particles at 1 µm [21] 10-8

Seeding particles at 10µm [21] 10-5

Second, tracking capability of seeding particles can be estimated by Stokes’ theorem. The basic

assumptions of Stokes’ flow are that flow is incompressible and Reynolds number is very small.

Thus the inertia terms can be neglected in the Navier-Stokes equations, and only the viscous

force balances the pressure that drags the particle. The supersonic flow is compressible and

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temperature gradient in the boundary layer causes variations in viscosity. However, the local

flow velocity fluctuation relative to the moving particle is still subsonic. Local Mach number

fluctuation from its mean value is still below 0.3 when the free stream Mach number reaches 4

and below 1 when the Mach number reaches 7.2 for a zero-pressure-gradient adiabatic boundary

layer at moderately high Reynolds numbers [28]. So Stokes’ theorem can still be used to

approximate and analyze how the nanoparticles follow the supersonic flows. The relaxation time

of the particle can be expressed as [21]

p
 p  d p2 (1  2.7 Knd )
18 f
(2)

Where dp and ρp are the diameter and density of the particle, respectively, µf is the viscosity, Knd

is the Knudsen number. Approximately the response time of the particle is proportional to the

density of the particle and the square of the diameter of the particle. Air molecules tagged by

MTV can perfectly measure the velocity across the shock, while particles seeded in PIV show

degraded effects. Therefore the smaller and lighter the particle is, the better for it to track the

flow motion. The lower limit for the seeding particle is set by the measurement uncertainties due

to Brownian motion of the particles. [14, 15]

2.2 Plasmonic Resonance Enhanced Light Scattering

Plasmonic effect is the generation of highly localized light fields in the near-field of metallic

nanostructures [29]. Light scattering, including Rayleigh and Raman scattering, can be

significantly enhanced by the plasmonic resonance. To quantify the plasmonic resonance effects,

Discrete Dipole Approximation (DDA) method [30] has been used to calculate the light

absorption and scattering from various nanoparticles in solution and in air.

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In Figure 1, comparison between silver nanoparticles with TiO2 nanoparticles at the same sizes is

shown. With a diameter of 22.3 nm, silver nanoparticles show the resonance enhanced light

scattering at 360nm in air and ~400nm in water. TiO2 nanoparticles show no resonance effects.

Figure 1. Comparison of light scattering spectra between silver and TiO2 nanoparticles at

diameters of 20nm in air and in water

In Figure 2, comparison between experimental and computational results of nanoparticle

scattering is shown. In Figure 3, comparison of light scattering spectra among silver

nanoparticles at different diameters in water is shown. The resonance peaks shift toward the red

region and get broader when the diameters of the nanoparticles become larger. The position of

the peaks and the width of the peak can be used to estimate the diameters of the nanoparticles.

Light scattering intensity can be plasmonic resonance enhanced if the incident light is around the

resonance frequency. The cross sections for the silver nanoparticles can be resonance enhanced

by more than 10 times when the incident light varies from ~300nm to ~400nm in water. Since it

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is only possible for the silver nanoparticles, light scattering from other particles can be filtered or

blocked efficiently. This will eliminate other potential disturbances from the dust particles for the

velocity measurement.

Figure 2. Comparison of experimental and simulation results of silver nanoparticles.

Figure 3. Comparison of light scattering spectra among silver nanoparticles with different

diameters in water.

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3. Nanoparticle Synthesis and nPIV

3.1 Nanoparticle Synthesis & Characterization

Silver nanoparticles are synthesized by chemical reduction method. First, AgNO3 (90 mg) is

dissolved in 500 mL of deionized water. After the solution is boiling, 10 ml of 1% sodium citrate

(0.22 g of trisodium citrate, C6H5Na307, dissolved in 22 mL of H2O) is added into it. The color of

solution gradually turns gray in a few minutes. The mixture solution is kept boiling for 1 hour.

Then the production containing silver nanoparticles is irradiated by an intensive laser beam (532

nm, 393 mJ/cm2) for about 30 minutes. The silver nanoparticles are melted by the laser beam to

form the nanoparticles at about 8-10 nanometers. These nanoparticles are used as seeds for

further synthesis. After the same amount and concentration of AgNO3 solution is boiled again,

8.3 ml of seeds solution and 10 ml of 1% sodium citrate are added into them. Keeping boiling

for 1 hour, the mixture solution is cooled to the room temperature. The Ag nanoparticles in the

solution are finally filtered with 100 nm filters and used for the nano-PIV measurement.

Hitachi S 3500 SEM (Scanning Electron Microscope) is used to characterize the actual

morphologies of silver nanoparticles. The nanoparticles have spherical shapes. The diameters of

those nanoparticles are approximately 35 nm. The silver nanoparticles used in the experiments

are measured, shown in Figure 4. The size distribution of nanoparticles is counted, shown in

Figure 5.

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Figure 4. Morphologies of dry silver nanoparticles record by SEM. The bar represents 100nm.

Figure 5. The size distribution of silver nanoparticles measured by SEM

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Figure 6. Size distribution of silver nanoparticles in solution measured by DLS

Size distribution of the nanoparticles is recorded by a dynamic light scattering (DLS) system
(Brookhaven Instruments BI-2000SM goniometer equipped with a PCI BI-9000AT digital
correlator). The laser wavelength is 633 nm. The detector is located at the scattering angle of 90º.
The DLS provides the hydrodynamic size distribution of the particles in the solution by the
autocorrelation calculation of the Brownian motion of particles. Sizes distribution of Ag
nanoparticles is shown in figure 6. The diameter for most nanoparticles is ~52.1 nm. There are
also minor proportions in the size distribution. Especially the nanoparticles less than 10 nm in
the solution are common for the synthesis process. In addition, the sizes of particles obtained
from DLS are always greater than those from electron microscopes due to hydrodynamic effects
in the water [31].

3.2 Far-field Nanoparticle Observation

The prepared nanoparticle solutions can be examined using a standard dark field microscopy.

Shown in Figure 7(a), the silver nanoparticles were recorded with an exposure time of 3.3 ms

under the illumination of white light. The image under the illumination of a single laser pulse

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(532nm, 10ns duration) was shown in Figure 7(b). The sizes of spots in the images represented

the silver nanoparticles is nearly ~ 0.5 µm.

(a) (b)

Figure 7. Dark field images of Ag nanoparticles illuminated by (a) a white light source.

Exposure time for the camera is 4 ms. (b) a laser pulse at 532nm, exposure time equals to the

pulse duration of laser, which is about 10ns. The bar is 2µm.

Following the analysis used in µPIV, the final sizes of spots recorded by CCD can be estimated

by the following equation [15],

1/2
  1  
2

de   M 2 d p2  5.95  ( M  1)2  2    (3)


  2 NA  

where de is the final imaged particle diameter, M is image magnification (100 ×), dp is the

particle diameter (~35 nm), λ is the light wavelength (500 nm or 532 nm), , NA is the numerical

aperture of objective lens (1.4). So the final imaged particle diameter of silver nanoparticles is

~0.55pixles in the images, which corresponding to 0.55 µm in the images.

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3.3 Velocity Measurement

(a) (b)

Figure 8. (a) The diagram of nano-PIV setup used dark field illumination, (b) the schematics of

the micro channel.

(a)

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(b)

(c)

Figure 9. Experimental measurement of nanoparticle movement in a micro channel using white

light dark- field illumination. (a) Image of nanoparticles at an exposure of 2 milliseconds and

Instantaneous velocity map of the flow (in m/s). Flow speed is 0.01ml/sec, (b) Flow speed is

0.08ml/sec, (c) flow speed is 0.16ml/sec.

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A far field plasmonic enhanced nano-Particle Image Velocimetry (nPIV) has been demonstrated

by integrating the common PIV technique with the single nanoparticle tracking technique. As

shown in Figure 8, a laser or white light source has been focused on a micro channel (shown in

Figure 8 B) by a dark field condenser. The flow seeded with nanoparticles has been pumped

through the channel using syringe pump. A fast camera (TSI- HS650) with an image intensifier

has been used to capture scattering light from the nanoparticles. The movement of the flow is

accompanied by the displacement of the seeding particles. Since only the scattering light from

the nanoparticles can be detected by the camera, it is straightforward to locate those

nanoparticles. By comparing two consecutive images of the flow field with auto-/cross-

correlation technique, we can follow the movement of the nanoparticles so that a 2D velocity

profile has been obtained as shown in Figure 9. The flow velocity is about 0.5 mm/s.

4. Conclusions

In this paper, a novel far-field plasmonic resonance enhanced nanoparticle-seeded Particle Image

Velocimetry (nPIV) has been demonstrated to measure the velocity in a micro channel.

Calculations based on Discrete Dipole Approximation are conducted to optimize light scattering

from chemically synthesized silver nanoparticles. Optimum scattering wavelength is specified

for the nanoparticles in two media: water and air. The diffraction-limited plasmonic resonance

enhanced images of silver nanoparticles at different diameters have been recorded. By using

standard PIV techniques, the velocity profiles within the micro channel have been determined

from the images. Velocity of 0.5mm/s has been successfully measured by the technique.

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5. Acknowledgements

The work is supported by the University of Tennessee and Joint Directed Research Direction

(JDRD) of the Science Alliance.

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