Introduction to ellipsometry

J.Ph.PIEL (PhD) Application Lab Manager SOPRALAB

EPFL October 7th 2008

OUTLINE : - Basic Theory - GES5 description - Data Analysis - Conclusion

EPFL October 7th 2008

I - BASIC THEORY Brief history of Ellipsometry Principle Physical meaning of and

EPFL October 7th 2008

For the 1st time Paul DRUDE use ellipsometry in 1888

Phase measurement

EPFL October 7th 2008

2000

Alexandre Rothen Published in 1945 a paper where the word Ellipsometer appears for the 1st time

Thickness sensitivity : 0.3 A

EPFL October 7th 2008

Bref Historique
Schematic representation of the mounting from Alexandre Rothen
(Rev. of scientifique instruments Feb 1945)

EPFL October 7th 2008

Few key people in ellipsometry area

Malus in 1808 : discovery of the polarisation of light by reflexion. Fresnel in 1823 : Wave theory of the light. Maxwell in 1873 : developpment of the Electrogmagnetic field theory. Drude in 1888 : Use of the extreme sensitivity of the ellipsometry to detect ultra thin layers (monolayer). Abeles in 1947 : Developpment of matrix formalism applied to thin layers stack. Rothe in 1945 : Introduction of the word : Ellipsometer Hauge, Azzam, Bashara in 1970 : description and developpement of different ellipsometer settings.

1980 : development of Personal Computer , automatisation of the EPFL October 7th 2008 technique. Industrial development of tools.

INTRODUCTION
ELLIPSOMETRY is a method based on measurement of the change of the polarisation state of light after reflection at non normal incidence on the surface to study -The measurement gives two independent angles: and - It is an absolute measurement: do not need any reference - It is a non-direct technique: does not give directly the physical parameters of the sample (thickness and index) - It is necessary to always use a model to describe the sample SPECTROSCOPIC ELLIPSOMETRY (SE) gives more comprehensive results since it studies material on a wide spectral range

EPFL October 7th 2008

PRINCIPLE OF SPECTROSCOPIC ELLIPSOMETRY

linear polarisation

Ei ES

EP

rp

Ei

Ep Es

0
Thin Film 1 (n1, k1, T1) Thin Film 2 (n2, k2, T2) Thin Film i (ni, ki, Ti) Substrate (ns, ks)

Er

rs

elliptical polarisation

Er

Ambient (n0, k0)

Ep.rp Es. rs

Ellipsometry measures the complex reflectance ratio :

=
EPFL October 7th 2008

rp rs

= tan .e j = f( ni, ki, Ti )

9

- After reflection on the sample, the extremity of the electric field vector describes an ellipse
p

rp
0

rs

- This ellipse is characterised by *the ellipticity Tan which is the ratio of the large axis to the small axis *the angle of rotation between the main axis and the P axis:
EPFL October 7th 2008 10

Extremity of the electric field vector descrives an ellipse

EPFL October 7th 2008

11

Physical meaning of and .

Those parameters give all relevant information about the polarization state of the light at a given wavelength.
However, and are not straightforwardly linked to the easiest geometrical features of the ellipse. - Tan gives exactly the angle of the first diagonal of the rectangle in which the ellipse is enclosed. - Cos gives roughly how fat is going to be the ellipse (shape). Its mathematically linked to the ratio of short axis to long axis of the ellipse in its fundamental frame.
40.
1

Tan (2)=Tan (2)Cos

0.5

: angle of rotation of the long axis of the ellipse

versus axis p
EPFL October 7th 2008

0.5

0.5

0.5

12
-

0
1

20.
1

40.
1

0.5

0.5

0.5

0.5

0.5

0.5

0.5

0.5

0.5

0.5

0.5

0.5

60.
1

80.
1

90.
1

0.5

0.5

0.5

0.5

0.5

0.5

0.5

0.5

0.5

0.5

0.5

0.5

Example of some different phase shift () for a given value.

On those graphics, the long axis is the ellipse is represented and it has to be compared with the diagonal of the rectangle. Because is fixed, the ellipse is enclosed in the same rectangle for each graphic. EPFL Modification of change both angle of inclination and ellipticity. October 7th 2008

13

II - GES5 DESCRIPTION Physical description Jones Formalism Mathematical treatment of the signal Example
14

EPFL October 7th 2008

Goniometer

Microspots

Polariser Arm

Analyser Arm

Mapping rho/theta Sample

EPFL October 7th 2008

15

EPFL October 7th 2008

16

EPFL October 7th 2008

17

SPECTROSCOPIC ELLIPSOMETER

Goniometer
A P

Xe Lamp

Optical Fiber

Photo Multiplier Tube

Scanninig channel

C.C.D. channel

EPFL October 7th 2008

18

Schematics of dispersion elements

Spectrograph
Entrance Fiber

Multichannel Detector

Grating : fixed

Spectrometer

Entrance Fiber Grating : rotating

PMT

EPFL October 7th 2008 NIR detector

Prism : rotating

19

GENERAL GES5 DESCRIPTION: - Xenon Lamp:75 W, Short arc, High brilliance

- MgF2 Rotating Polarizer MgF2 : 6 Hz - Adjustable Analyzer - Goniometer from 7 up to 90 - Microspots : spot size : 400 m - High resolution way : -Spectral range : 190 nm up to 2000 nm- resolution < 0.5 nm - double monochromator: prism + grating - Photon counting PMT -High speed way : - Spectral range : 190 nm up to 1700 nm - Measurement duration : few seconds - Fixed grating spectrograph - CCD (1024x64 pixels)and OMA NIR (256 pixels) detectors
EPFL October 7th 2008 20

Jones Formalism

BUT : Jones formalism can only work if there is no depolarisation effects induced by the material
EPFL October 7th 2008 21

Optical system with no depolarisation effects is characterized by this following Jones Matrix :

2X2 complex Matrix

EPFL October 7th 2008

22

If the material is isotrope :

Ellipsometric Angles and measured simultaneously

EPFL October 7th 2008

23

Jones Matrix for a Linear Polarizer : Rotation Matix :

1 Px = 0

0 0
sin cos

P =

cos sin

General expression for a polarizer where the main axis is oriented with an angle P =R(-).Px.R()

EPFL October 7th 2008

24

I = Edp . Edp* + Eds . Eds* I (t) = I0 . ( 1 + Cos 2 (t) + Sin 2 (t) ) A : Angle between Analyser and plane of Incidence. EPFL October 7 2008 (t) : Angle between Polariseur and plane of Incidence.
th

25

Edp Eds

1 0 Cos A Sin A rp 0 Cos P - Sin P 1 0 0 0 -Sin A Cos A 0

Rotation

Ep Es

rs Sin P Cos P 0 0
Rotation

Detector Analyser

Sample

Polariser Lamp

I = Edp . Edp* + Eds . Eds* I = I0 . ( 1 + Cos 2 P(t) + Sin 2 P(t) ) A : Angle between Analyser axis and Plane of Incidence. P(t) : Angle between Polarizer axis and Plane of Incidence.
EPFL October 7th 2008 26

HADAMART TRANSFORM

Intensity

S1 = I ( P )dP
0

S 2 = I ( P )dP

4
4 3

S3 =
S4 =

I ( P )dP
2

S1

S2

S3

S4

S1

I ( P )dP
4

Time
[S1 - S2 -S3 + S4 ] = 2 I0
EPFL October 7th 2008

[S1 + S2 - S3 - S4 ] = 2 I0

0 =

[S1 + S2 + S3 + S4 ]

27

CALCULATION OF THE ELLIPSOMETRIC PARAMETERS 0 = = Tan 2 - Tan 2 A Tan 2 + Tan 2 A Cos 2 A Tan 2 + Tan 2 A = 2 Cos . Tan . Tan A Tan 2 + Tan 2 A

Tan = Tan A . 1 - 2

1+ 1 -

Cos =
EPFL October 7th 2008

28

DUV UV
EPFL October 7th 2008

VISIBLE

NIR
29

ELLIPSOMETRIC MEASUREMENT

RESULTS ANALYSIS

Physical Model Tan Experimental Measurement Cos

Estimated sample structure

- Film Stack and structure - Material n, k, dispersion - Composition Fraction of Mixture

Non direct technique.

Experimental Measurement

No

Need the use of models to interpret the measurements and to get physical parameters of the layers

=
Model Simulation ?

Yes

Ti , ni , ki

EPFL October 7th 2008

REAL SAMPLE STRUCTURE

30

III - DATA ANALYSIS Which physical parameters can we get ? Sensisitivy of the technique Description of the main models used How to describe optical properties of the materials.
31

EPFL October 7th 2008

Which physical parameters can we get ?

- Mechanical thickness of each layer : Monolayer sensitivity (<0.01 A) up to 50 m. - Refractive index versus wavelength : n() Allow to characterize the quality of the layer and the process. - Extinction coefficient versus wavelength : k(). Measure the attenuation of light in the material. Allow to characterize the quality of the layer and the process. Surface and Interface characterization. Layer inhomogeneity characterization.

- In case of metallic or activated doping material: resistivity and doping concentration characterization using Drude Model. In case of porous material: porosity, pore size distribution and Young modulus EPFL October 7th 2008 32 characterization using Kelvin model.

Spectroscopic ellipsometry sensitiviy

Phase variation : is extremelly sensitive to ultra thin layers

Angle of incidence: 75
EPFL October 7th 2008 33

Spectroscopic ellipsometry sensitiviy

Sensitivity could reach 0.01 A or 1 picometer

0nm

10 A

EPFL October 7th 2008

34

Angle of incidence: 75

Description of the main models used

EPFL October 7th 2008

35

2 media model : Substrat alone

Fresnel equation and Snell-Descartes law: rp = (ns.cos0 n0.coss)/(ns.cos0 + ns.cos1) and
0 Ambiant : air Substrat ns = s - i.ks

rs= (n0.cos0 - ns.coss)/(ns.cos0 + ns.cos1) with = rp/ rs = Tan.exp(i.)

Direct inversion of the ellipsometric parameters to get substrate indices

ns = sin0.(1 + ((1-)/(1+))2.Tan20)1/2
EPFL October 7th 2008 36

2 media model : Substrat alone

Silicium
EPFL October 7th 2008

Angle of incidence 75
37

3 media model : one layer on known substrate

EPFL October 7th 2008

38

3 media model : one layer on known substrate

Native oxide (SiO2) on Silicon
SiO2 Sicr 30.8

EPFL October 7th 2008

39

3 media model : one layer on known substrate

SiO2 1200

SiO2 layer on silicon

Sicr

EPFL October 7th 2008

40

3 media model : one layer on known substrate

Thick SiO2 layer on Silicon
SiO2 Sicr 1,9838m

EPFL October 7th 2008

41

3 media model : one layer on known substrate

Rp et Rs are periodic function Same periods Idem for Tan and Cos

If a =75 Period=/(nb2-0.93)0.5 For SiO2 film nb =1.5 Period = /2.3 At =450 nm, period = 200 nm
EPFL October 7th 2008

Sensitivity to : In this case variation de 360 for a period = 200 nm sensitivity given by instrument: 5.10-2 Thickness sensitivity : 0.01 A
42

Multilayer stack

EPFL October 7th 2008

43

Multilayer stack
Interface relations : Fresnel Propagation inside the layer : Interferences

EPFL October 7th 2008

44

How to describe optical properties of the materials

Index library Effective medium mixing laws Dispersion law Harmonic oscillators laws Drude laws

EPFL October 7th 2008

45

Index Library
3 main type of materials: Dielectric : transparent in the visible range but absorbing in the UV and have absorbing band in the IR. Transparent materials : Oxides (SiO2, TiO2) Fluorides (MgF2) Optical filters, Anti reflective coatings, dielectric mirror (lasers). Semi-conductors dispersives laws extremelly rich in the visible range linked to the band structures. Could be metallic in the IR. Silicon : Si; Germanium : Ge; Gallium arsenide : GaAs; Gallium nitride: GaN; Carbon Silicon SiC (blue diode); Metal highly absorbing in the visible. Infrared mirrors :Au, Al, Cu Magnetic Materials : Co, Ni, Fe, Gd Handbook of Optical Constants from Palick SOPRA library EPFL October 7th 2008 Direct measurements on bulk materials

46

Effective medium model

EPFL October 7th 2008

47

Popular effective medium model

EPFL October 7th 2008

48

Interface and Surface roughness treated by Effective medium Model

EPFL October 7th 2008

49

Limits of the effective medium model

- Model is convenient for physical or mechanical mixing. Ex : Porous material with inclusion of void. - Model is not convenient for chemical mixing Ex : Inclusion of atom in elementary cells or variable atomic concentration Ex : Si(1-x)Gex. - Model is not applicable when the size of inhomogeneities exceed few hundredth (1/100) of the wavelenght of the beam.

EPFL October 7th 2008

50

Dispersion Law
Sellmeier law :
( A 1) ( ) = 1 + ( B)
2 r 2
2 1 0 2

( ) =
i
2 3

A . A . + n( ) = A + A A
2 2

B B k ( ) = n( ) .(B . + + )
2 3 1 3

SiNx example

Cauchy law :
n = A+ B

k=

k =0 for transparent materials

EPFL October 7th 2008

51

Harmonic Oscillators
Absorption band in the measured spectral range Lorentz oscillators
A . . ( L ) = ( L ) + .
2 2 2 0 r 2 2 2 2 0 2

A. . = ( L ) + .
3 i 2 2 2 2 0

SiO2 in the Infrared range

A: Intensity. L0: Middle wavelength.

: Oscillator width.
4 absorption peaks

EPFL October 7th 2008

52

Harmonic Oscillators
100 nm of an absorbing layer on Silicon substrate

EPFL October 7 2008

Spectroscopic Ellipsometry data th

Indices of the layer

53

Drude Law
4.0 3.5 3.0 2.5

Indices are fitted using Drude law :

N() doped Silicon
N() undoped silicon
2 p 1 ( ) = 2 2
2 p 2 ( ) = ( 2 2 )

n, k

2.0 1.5 1.0 0.5 0.0 2 4 6 8 10 12 14 16

Measure and Drude law fit on doped silicon k() doped Silicon
k() undoped Silicon
Wavelength ( m)

p : Plama frequency : diffusion frequency

Semi conductors indices are sensitive to the doping level in the IR range
EPFL October 7th 2008 54

Drude Law
Spectroscopic ellipsometry fit gives :
Plasma frequency p and Diffusion Frequency Material Conductivity
2 p = 0

Carrier Density Carrier Mobility

N = m*

2 0 p

e2

e m*

N =1.6 1019 at./cm3

For the sample corresponding to the previous measurement : EPFL October 7th 2008

= 104 cm2 V-1 s-1 = 264 -1 cm-1

55

Conclusion

EPFL October 7th 2008

56

The measurement gives two independent angles: and - Absolute measurement: do not need any reference. - Extremely sensitive to very thin layers (less than a monolayer). - fast : get the full spectrum (190 nm up 1700 nm) in few seconds - Non-direct technique: does not give directly the physical parameters of the sample (thickness and index) - Need to use a model to describe the sample. Determination of : but also :

Thickness Refractive index : n Extinction coefficient : k Molecular bounds

EPFL October 7th 2008

Porosity Resistivity

57