The Importance of Refractive Index When using Laser Diffraction · 2011. 10. 19. · Refractive...

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© 2011 HORIBA, Ltd. All rights reserved. The Importance of Refractive Index When using Laser Diffraction Mark Bumiller [email protected]

Transcript of The Importance of Refractive Index When using Laser Diffraction · 2011. 10. 19. · Refractive...

Page 1: The Importance of Refractive Index When using Laser Diffraction · 2011. 10. 19. · Refractive Index Refractive Index is defined by two components – Real and Imaginary RI = n +

© 2011 HORIBA, Ltd. All rights reserved.

The Importance of Refractive IndexWhen using Laser Diffraction

Mark [email protected]

Page 2: The Importance of Refractive Index When using Laser Diffraction · 2011. 10. 19. · Refractive Index Refractive Index is defined by two components – Real and Imaginary RI = n +

© 2011 HORIBA, Ltd. All rights reserved.

Fraunhofer Approximation

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Mie Theory

RI 1.60 – 0.0i, in water, RI 1.33

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Mie vs. Fraunhofer

1.E-04

1.E-03

1.E-02

1.E-01

1.E+00

1.E+01

1.E+02

1.E+03

1.E+04

1.E+05

0.01 0.1 1 10 100

Angle in degrees

Rel

ativ

e In

tens

ity

3.0 µm by Mie3.0 µm by Fraunhofer100.0 µm by Mie100.0 µm by Fraunhofer

100 μm

3 μm

Figure A.3 -- Comparison of scattering patterns of non-absorbing particles according to Fraunhofer and Mie calculations (Np = 1,59 – 0,0; nwater = 1,33;

wavelength = 633 nm)

Page 5: The Importance of Refractive Index When using Laser Diffraction · 2011. 10. 19. · Refractive Index Refractive Index is defined by two components – Real and Imaginary RI = n +

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Practical Application of Theory:Mie vs. Fraunhofer for Glass Beads

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Practical Application of Theory: Mie vs. Fraunhofer for CMP Slurry

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Influence of Particle Size on Angular Light Intensity Scattering Patterns

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Influence of Imaginary Parts of RI (Absorbancies)

Page 9: The Importance of Refractive Index When using Laser Diffraction · 2011. 10. 19. · Refractive Index Refractive Index is defined by two components – Real and Imaginary RI = n +

© 2011 HORIBA, Ltd. All rights reserved.

Refractive Index

Refractive Index is defined by two components –Real and Imaginary

RI = n + ik

Where:N = real component, velocity of light in a vacuum/ velocity

of light in the particle= c/vp

c = speed of light in vacuumVp= speed of light in particle (liquid, air)k = the extinction coefficient of the materiali = - 1

Page 10: The Importance of Refractive Index When using Laser Diffraction · 2011. 10. 19. · Refractive Index Refractive Index is defined by two components – Real and Imaginary RI = n +

© 2011 HORIBA, Ltd. All rights reserved.

RI: Real Component

Real component from published tables or measured using Snell’s Law

Light Path

nn

n sin = n sin

n sin = n sin

where:n = RI of air = angle of incidencen= RI of particle = angle of refraction

Page 11: The Importance of Refractive Index When using Laser Diffraction · 2011. 10. 19. · Refractive Index Refractive Index is defined by two components – Real and Imaginary RI = n +

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n is Frequency Dependent

Remember theLA-950 hastwo light sourcesRed = 650 nmBlue = 405 nm

In this example1.53 vs. 1.51Not very important

Could matter forsub-micron pigments

1.531.51

Sellmeier equation

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RI: Imaginary Component Imaginary component (k) in Mie equation is the

extinction coefficient of the particle. Reduction of transmission of optical radiation caused by absorption and scattering of light.

Light Path

Particle

Absorption coefficient () = reciprocal distance light penetrates surface & be attenuated to 1/e of original intensity, about 37%. Opaque particles have high coefficient.

k = Where:

k = the extinction coefficient = the absorption coefficient = the wavelength of light used

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RI: Imaginary Component

100%

Intensity

1 / e = 37%

d Distance into medium

1 / d = k = ( Example: for a value of k = 0.1 k = [] = 0.05 x [1 / d] = 0.1 = k d = 0.05 / 0.1 = 0.5 micron

Page 14: The Importance of Refractive Index When using Laser Diffraction · 2011. 10. 19. · Refractive Index Refractive Index is defined by two components – Real and Imaginary RI = n +

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RI: Imaginary Component For transparent particles use 0 for the imaginary

component For slightly opaque materials use 0.01 or 0.1 For opaque materials use 1.0 or higher Values can exceed 1.0 (see below*)

*http://www.ee.byu.edu/photonics/opticalconstants.phtml

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© 2011 HORIBA, Ltd. All rights reserved.

Refractive Index EffectMost pronounced when:

Particles are spherical Particles are transparent RI of particle is close to RI of fluid Particle size is close to wavelength of light source

Least pronounced when:

Particles are not spherical Particles are opaque RI of particle is larger than RI of the fluid Particle size is much larger than wavelength of the light source

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© 2011 HORIBA, Ltd. All rights reserved.

Older HORIBA Software: RI Kernels

If n = 1.33 (water) and n’ = 1.60 (particle)

Relative refractive index (RRI) : 1.60/1.33 = 1.203Transparent particles: k = 0Kernel function:120-000rri

Particles somewhat opaque: then k > 0KERNEL function: 120-020rriIf powder, relative index:n = 1.0 (air) and n’ = 1.60 (particle), RRI: 1.60/1.0 = 1.60Kernel function: 160-000rri or 160-020rri

Suspending medium

n n

particle

Page 17: The Importance of Refractive Index When using Laser Diffraction · 2011. 10. 19. · Refractive Index Refractive Index is defined by two components – Real and Imaginary RI = n +

© 2011 HORIBA, Ltd. All rights reserved.

Practical Approach

Measure sample onceChange RIDoes result change significantly?No: stop worryingYes: keep workingFor LA-950 users: determine real

component, vary imaginary component to minimize residual R value.

Oops, gave the plot away

Page 18: The Importance of Refractive Index When using Laser Diffraction · 2011. 10. 19. · Refractive Index Refractive Index is defined by two components – Real and Imaginary RI = n +

© 2011 HORIBA, Ltd. All rights reserved.

Abbe Refractometer

Dissolve sample at different concentrations

Plot conc. vs. RI Extrapolate to infinite

concentration

0 0.2 0.4 0.6 0.8 1.0

1.8

1.6

1.5

1.4

1.3

Concentration

Ref

ract

ive

Inde

x

Page 19: The Importance of Refractive Index When using Laser Diffraction · 2011. 10. 19. · Refractive Index Refractive Index is defined by two components – Real and Imaginary RI = n +

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Becke Lines

Bright line is called the Becke line and will always occur closest to the substance with a higher refractive index

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Becke Line Test

A particle that has greater refractive index than its surroundings will refract light inward like a crude lens.

A particle that has lower refractive index than its surroundings will refract light outward like a crude diverging lens.

As you move away from the thin section (raising the objective or lowering the stage),the Becke Line appears to move into the material with greater refractive index.

Page 21: The Importance of Refractive Index When using Laser Diffraction · 2011. 10. 19. · Refractive Index Refractive Index is defined by two components – Real and Imaginary RI = n +

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Becke Line Test

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Luxpop.com

Note RI is dependent on wavelength of light.Can adjust RI for red &blue light, but only needto for small, absorbingparticles.

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RI of Polymershttp://www.texloc.com/closet/cl_refractiveindex.html

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Google Search

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Mixtures

Larsen, E.S., Berman, H., The Microscopic Determination of the Non-Opaque Minerals, Second Edition, United States Department of the Interior, Geological Survey Bulletin 848, 1934, US Government Printing Office, Washington, DC.

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Mixtures

Page 27: The Importance of Refractive Index When using Laser Diffraction · 2011. 10. 19. · Refractive Index Refractive Index is defined by two components – Real and Imaginary RI = n +

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AnisotropyAlso called birefringenceMany crystals have different RI as inspected throughdifferent planes.Use average, consider flow alignment

I would rather eat French food

Page 28: The Importance of Refractive Index When using Laser Diffraction · 2011. 10. 19. · Refractive Index Refractive Index is defined by two components – Real and Imaginary RI = n +

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Uniaxial vs. Biaxial Materials

where no and ne are the refractive indices for polarizations perpendicular (ordinary) and parallel (extraordinary) to the axis of anisotropy respectively.

Biaxial birefringence, also known as trirefringence, describes an anisotropic material that has more than one axis of anisotropy

3 Elert, Glenn. "Refraction". The Physics Hypertextbook. http://hypertextbook.com/physics/waves/refraction/.

Page 29: The Importance of Refractive Index When using Laser Diffraction · 2011. 10. 19. · Refractive Index Refractive Index is defined by two components – Real and Imaginary RI = n +

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Scary Example: Is the Small Peak Real?

Starch sample

Low imaginary

Page 30: The Importance of Refractive Index When using Laser Diffraction · 2011. 10. 19. · Refractive Index Refractive Index is defined by two components – Real and Imaginary RI = n +

© 2011 HORIBA, Ltd. All rights reserved.

Scary Example: Is the Small Peak Real?

Starch sampleHigh imaginary

Page 31: The Importance of Refractive Index When using Laser Diffraction · 2011. 10. 19. · Refractive Index Refractive Index is defined by two components – Real and Imaginary RI = n +

© 2011 HORIBA, Ltd. All rights reserved.

Scary Example: Is the Small Peak Real?

Starch sampleZero imaginary

?

The oldsecondaryscatteringtrick

Page 32: The Importance of Refractive Index When using Laser Diffraction · 2011. 10. 19. · Refractive Index Refractive Index is defined by two components – Real and Imaginary RI = n +

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Effect of RI: Cement

Fixed absorbance, vary real Fixed real, vary absorbance

Page 33: The Importance of Refractive Index When using Laser Diffraction · 2011. 10. 19. · Refractive Index Refractive Index is defined by two components – Real and Imaginary RI = n +

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Chi Square and R Parameter

yi The measured scattered light at each channel (i) of the detector.y (xi) The calculated scattered light at each channel (i) of the detector based on the chosen refractive index kernel and reported particle size distribution.σi The standard deviation of the scattered light intensity at each channel (i) ofthe detector. A larger σi indicates lower reliability of the signal on a given detector.N The number of detectors used for the calculation

Page 34: The Importance of Refractive Index When using Laser Diffraction · 2011. 10. 19. · Refractive Index Refractive Index is defined by two components – Real and Imaginary RI = n +

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Using R Value for i

Page 35: The Importance of Refractive Index When using Laser Diffraction · 2011. 10. 19. · Refractive Index Refractive Index is defined by two components – Real and Imaginary RI = n +

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Changing RI

Page 36: The Importance of Refractive Index When using Laser Diffraction · 2011. 10. 19. · Refractive Index Refractive Index is defined by two components – Real and Imaginary RI = n +

© 2011 HORIBA, Ltd. All rights reserved.

Changing RI

Page 37: The Importance of Refractive Index When using Laser Diffraction · 2011. 10. 19. · Refractive Index Refractive Index is defined by two components – Real and Imaginary RI = n +

© 2011 HORIBA, Ltd. All rights reserved.

Changing RI

Page 38: The Importance of Refractive Index When using Laser Diffraction · 2011. 10. 19. · Refractive Index Refractive Index is defined by two components – Real and Imaginary RI = n +

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Using R Value for i

Page 39: The Importance of Refractive Index When using Laser Diffraction · 2011. 10. 19. · Refractive Index Refractive Index is defined by two components – Real and Imaginary RI = n +

© 2011 HORIBA, Ltd. All rights reserved.

Using R Value for i

Real component = 1.57 via Becke lineVary imaginary component, minimize Chi square & R parameter

Page 40: The Importance of Refractive Index When using Laser Diffraction · 2011. 10. 19. · Refractive Index Refractive Index is defined by two components – Real and Imaginary RI = n +

© 2011 HORIBA, Ltd. All rights reserved.

Automation by Method Expert Analytical conditions Calculation conditions

View Method Expert webinar TE004 in Download Center

Page 41: The Importance of Refractive Index When using Laser Diffraction · 2011. 10. 19. · Refractive Index Refractive Index is defined by two components – Real and Imaginary RI = n +

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Automated RI ComputationReal part studyNeed to fix imaginary partSet up to 5 real partsSoftware will compute all RI and display R parameter

variation with RI selection

Page 42: The Importance of Refractive Index When using Laser Diffraction · 2011. 10. 19. · Refractive Index Refractive Index is defined by two components – Real and Imaginary RI = n +

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Automated RI Computation

Page 43: The Importance of Refractive Index When using Laser Diffraction · 2011. 10. 19. · Refractive Index Refractive Index is defined by two components – Real and Imaginary RI = n +

© 2011 HORIBA, Ltd. All rights reserved.

Automated RI Computation

Page 44: The Importance of Refractive Index When using Laser Diffraction · 2011. 10. 19. · Refractive Index Refractive Index is defined by two components – Real and Imaginary RI = n +

© 2011 HORIBA, Ltd. All rights reserved.

Automated RI Computation Imaginary part studyNeed to fix real partSet up to 5 imaginary partsSoftware will compute all RI and display R parameter

variation with RI selection

Page 45: The Importance of Refractive Index When using Laser Diffraction · 2011. 10. 19. · Refractive Index Refractive Index is defined by two components – Real and Imaginary RI = n +

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Automated RI Computation

Imaginary study

Page 46: The Importance of Refractive Index When using Laser Diffraction · 2011. 10. 19. · Refractive Index Refractive Index is defined by two components – Real and Imaginary RI = n +

© 2011 HORIBA, Ltd. All rights reserved.

Summary

Measure sample, recalculate w/different RI –see how important it is

Use one of the described approaches to determine the real component

Recalculate using different imaginary component

Choose result that minimizes R parameter, but also check if result makes sense

You wish you had Method Expert by your side

Page 47: The Importance of Refractive Index When using Laser Diffraction · 2011. 10. 19. · Refractive Index Refractive Index is defined by two components – Real and Imaginary RI = n +

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