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Thin film analysis

Advanced X-ray Workshop, S.N. Bose National Centre

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Thin Films Samples 1


Metal conductor paths (Cu, Al, AlSiCu) Insulators (SiO2, HfO2) in semiconductors Diffusion barriers (Si3N4, Ti/TiN) Semiconductors (SiGe, GaAs, InP) Active zones in lasers and LEDs (InGaN, AlGaAs, GaN) Hard coatings (TiN) Solar cells a.k.a photovoltaics (CuInSe2,CdS, CdTe, organic) Magnetic active layers (CoPtCr) Piezoelectrics(PMN-PT, PZT, PLZT, PbTiO3) Optical coatings Electro-optics (PLZT, PMN-PT) Magnetostrictives (FeGa) Fuel cells (YSZ, Gd-CeO2) Superconductors (MgB2, YBa2Cu3O7)
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Thin Films Samples 2


Electrolytes in batteries (LiPO3) Oxide electrodes (SrRuO3) Catalysts (MOFs, CeO2) Coatings (bathroom fixtures, corrosion prevention) Communication/band gap tuning (HEMTs...quantum wells) Thermoelectrics (Pb0.5Sn0.5Te) Energy storage (ultracapacitors using metal carbides) Energy harvesting/ energy conversion

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Advanced X-ray Workshop

Thin Film Characteristics


A thin film is a layer of material ranging from fractions of nanometers (monolayer) to several micrometers in thickness. Thin films can have different degree of crystallinity: from amorphous to single crystal.
Degree of order Amorphous Polycrytal. Single crystal Front-end SiGe Organic monolayer Magn. storage Nanoparticles in matrix Back-end (Semi.) Low-k oxides LEDs Oxyde Semi. Coatings

1 nm

10 nm

100 nm

1 m

Layer thickness

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Thin Film XRD Methods Parameters of Interest


Grazing incidence Diffraction (GIXRD)
depth dependent information phase identification lattice parameter microstructure (size/strain) residual stress

X-Ray Reflectometry
layer thickness composition roughness density porosity

Stress and Texture


orientation distribution orientation quantification residual stress epitaxial relationship

High-Resolution X-Ray Diffraction


thickness lattice parameter lattice mismatch composition strain & relaxation lateral structure mosaicity (crystallinity) defects
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Reciprocal Space Mapping


lattice parameter lattice mismatch composition orientation relaxation lateral structure

In-Plane GIXRD
IP-lattice parameter IP-crystallite size IP-orientation epitaxial relation

Advanced X-ray Workshop

Bruker Confidential

Thin Film XRD Methods Parameters of Interest


Grazing incidence Diffraction (GIXRD)
depth dependent information phase identification lattice parameter microstructure (size/strain) residual stress

X-Ray Reflectometry
layer thickness composition roughness density porosity

Stress and Texture


orientation distribution orientation quantification residual stress epitaxial relationship

High-Resolution X-Ray Diffraction


thickness lattice parameter lattice mismatch composition strain & relaxation lateral structure mosaicity (crystallinity) defects
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Reciprocal Space Mapping


lattice parameter lattice mismatch composition orientation relaxation lateral structure

In-Plane GIXRD
IP-lattice parameter IP-crystallite size IP-orientation epitaxial relation

Advanced X-ray Workshop

Bruker Confidential

What is X-ray Reflectometry (XRR)?


A surface-sensitive X-ray scattering technique
Non-destructive method Wavelength probes on nanometer scale Works for crystalline and amorphous materials

What does XRR provide?


Layer thickness 0.1 nm 1000 nm Material density < 1-2% Roughness of surfaces and interfaces < 3-5 nm

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Analytical tasks

Layer thickness

(electron density)

Chemical Composition

Roughness

Lateral structure

Specular XRR

Diffuse

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The specular XRR scattering geometry


z x

q=(0,0,qz)

Wavevector transfer has a non-zero component perpendicular to the sample surface

q z = 2k sin
ki kf
For Cu-K (=1.54)

q z = 2 / 140 [nm 1 ]

XRR probes the laterally averaged electron density

S (q z ) ( z ) exp( iq z z )dz
2
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( z ) = ( x, y , z )
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x, y

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The reflectivity from a substrate


(z) exp(iqz) T exp(iQz) R exp(-iqz) 0
Fresnel reflectivity

q Q rF (q ) = RF (q ) = q+Q
2
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with

Q = q 2 16 re
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Density dependency of the reflectivity


The higher the electron density (z) of a material the higher the critical angle

c
The higher the electron density, the more intensity is scattered at higher angles

c r 2

This limits the accessible angular range for light materials like softmatter films

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Influence of Roughness Waviness


small inclinations of the surface normal on a large scale of some 100 nm broadening of the specular reflected beam reflected intensity

The broadening of the specular reflected beam decreases the It does not contains any information about internal sample
structure

Samples should have a flat surface


waviness

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Influence of Roughness Microscopic Roughness


large inclinations of the surface normal on an atomic scale of a few nanometers leads to diffuse reflection of the incident beam the intensity of the specular reflected beam decreases

microscopic roughness

waviness

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Influence of Roughness
Roughness decreases the reflected intensity dramatically XRR is highly sensitive to roughness Roughness causes diffuse scattering

The interface roughness should not be larger than 2-3 nm.

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XRR from single layer on substrate: Thickness fringes


The interference of the waves reflected from the interfaces causes oscillations of period

q z = 2 / d
The minimal observable thickness is limited by the maximal measurable range The maximal observable thickness is limited by the instrumental resolution The sample should have thicknesses observable with the instrumental setup.

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Thickness fringes Amplitude


Amplitude of the thickness fringes increases with increasing density contrast XRR is quite sensitive to variations of the electron density

The sample should have a good contrast in the electron density.

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XRR from multilayers

10

10

-1

2 - layer system 10 nm Ag 60 nm Au Si - substrat

Reflectivity

10

-2

10

-3

10

-4

10

-5

10

-6

0,0

0,5

1,0

1,5

2,0

2,5

3,0

Incidence angle []

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X-ray Reflectometry in Practise Demands on Sample Properties


Golden Rule: You should be able to see your reflection on the surface of the sample! Flat and lateral homogeneous - not structured Sample roughness < 5nm Good contrast in electron density for layered samples Length of at least 3-5 mm in beam direction

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Simplest Setup for XRR

Reasonable resolution requires slit of 50-100 m Intensity is on the order of 107 cps Full energy spectrum creates high background
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Principle of the Gbel Mirror

Goebel mirror Parabola

X-ray source

Sample

Mirror converts 0.35 into a parallel beam of 1.2 mm Integrated intensity >109 cps Mainly K-radiation is reflected

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The standard XRR setup for thin films

Slits can be easily exchanged to tune resolution A reasonable resolution requires a slit size of 0.1 0.2 mm Integrated intensity 2x108 cps
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Reflectometry with different slits

1e7

1e6

1e5

Int. [cps]

with 0.6 mm slit with 0.1 mm slit ~ 5 min ~ 6.5 h

1e4

1000

100

2/[]

Use slits to balance flux and resolution


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XRR setup for very thin layers

Full beam on primary side Soller with resolution down to 0.1 Integrated intensity 8x108 cps
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Limits of X-Ray Reflectometry Thin layers Example: LaZrO on Si


1*10 1*10 1*10 Intensity [au] 1*10 1*10 1*10 1*10 1*10 1*10
0

-1

-2

-3

-4

6.7 nm LaZrO Si (111)

-5

-6

-7

-8

6 2 []

10

12

14

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XRR with an analyzer crystal

Analyzer crystal improves the resolution:

1-bounce Ge(220) 3-bounce Ge(220)

Analyzer crystal separates K1, suppresses diffuse scattering and fluorescence Crystal can accept the full incident beam Integrated intensity 3x107 cps (for a 3-bounce analyzer)
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XRR setup for thick layers

Monochromator crystal:

4-bounce Ge
Analyzer crystal:

1-bounce Ge(220s) 3-bounce Ge(220s)

Monochromator cystals provide highly parallel and monochromatic beam Crystals can accept the full incident beam Integrated intensity 105 - 106 cps
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Limits of X-ray Reflectometry Thick layers example: SiO2 on Si

1e4

1000

Int. [au]

1014 nm SiO2:H Si

100

10 5 0.11 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1.0 1.1

2 []
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Resolution of differents setups


For Cu-K radiation: 1.54 Values for were obtained by scanning the direct beam Obtained from the rough estimation d / 2
Tube side GM + 1.2mm GM + 0.2mm 2xGe(220a) GM 2xGe(220a) 4xGe(220s) 4xGe(440s) Detector side 0.2 soller 0.2mm slits 0.2mm slits 3xGe(220s) 3xGe(220s) 3xGe(220s) 3xGe(220s) [deg] 0.06 0.029 0.026 0.013 0.01 0.006 < 0.006 dmax [nm] 73 150 170 340 440 735 > 735
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Geometrical corrections The footprint

d : beam width L : sample length || beam D : illuminated area

L
D = d / sin

Footprint of the beam on surface: Beam matches the sample size at: Below B the intensity is reduced by:
Advanced X-ray Workshop

B = arcsin( d / L)
B = sin( ) / sin( B )
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Geometrical corrections The footprint

Beamsize : 200 m

Sample size reduces the reflected intensity at small angles Sample must be sufficiently large for XRR
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Controlling the footprint The Knife Edge Collimator

The KEC allows the removal of the footprint effect by making the probed

area smaller than the sample size For higher angles, the KEC needs to be lifted from the surface to gain flux The measurement with KEC will be upscaled to the curve without KEC
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Controlling the footprint The Knife Edge Collimator


with KEC without KEC
10
8

Measurement with KEC must be performed up to at least 2B The high-angle measurement without KEC must have an overlap with the KEC measurement to rescale the data properly

10
7

Intensity

10

10

10

0,0

0,5

1,0

1,5

2,0

2 [deg]

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Evaluation of Sample Fitting Procedure

Sample Model parameterized by {p1,pN}

XRR Simulation

Comparison with Experiment, 2 cost function

Minimization of 2 using Genetic Algorithm, Levenberg-Marquardt, Simplex, Simulated Annealing, etc. in view of {p1..pN}

Tolerance

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Amorphous HfO2 film Ultra thin films

[degees]

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XRR on MEMS Ru/SiN film

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GMR Heterostructure 8 Layers

Sample courtesy of Dr. Schug, IBM Mainz

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Thin Film XRD Methods Parameters of Interest


Grazing incidence Diffraction (GIXRD)
depth dependent information phase identification lattice parameter microstructure (size/strain) residual stress

X-Ray Reflectometry
layer thickness composition roughness density porosity

Stress and Texture


orientation distribution orientation quantification residual stress epitaxial relationship

High-Resolution X-Ray Diffraction


thickness lattice parameter lattice mismatch composition strain & relaxation lateral structure mosaicity (crystallinity) defects
14-15/12/2011

Reciprocal Space Mapping


lattice parameter lattice mismatch composition orientation relaxation lateral structure

In-Plane GIXRD
IP-lattice parameter IP-crystallite size IP-orientation epitaxial relation

Advanced X-ray Workshop

Bruker Confidential

37

Remarks for Coatings


For coatings (few microns down to sub-micron range), the Bragg-Brentano geometry (BB) is still the best configuration. This is basically the classical powder diffraction case and BB will offer the best grain statistic and the easiest instrumental function characterization. Providing that the preferred orientation is weak, quantitative phase analysis or microstructure investigation (size/strain) are quite easy to perform. Limitations of the BB set-up: If the substrate is a single crystal, the huge intensity from the substrate peak will emphasize all minor peaks originating from the energy spectrum of the tube and other aberrations (K, tube tails, Ni absorption edge, W lines,) with the consequence that a significant part of the scan wont be usable.

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Polycrystalline Thin Films Constrains


Even if a layer is polycrystalline, several characteristics differentiate a polycrystalline thin film with a loosed powder: Due to the limited layer thickness, the grain statistics is limited. The classical BB geometry might fail in providing necessary peak intensity for further analysis. An alternative is then to go for GIXRD. The confinement of the grains into a limited volume very often causes preferred orientation and the quantitative phase analysis might become impossible. The grain interaction during growth can also induce residual stress. A composition gradient through the layer may also appear during the growth.

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Grazing Incidence X-Ray Diffraction Instrumental Set-up Requirements


GIXRD requires a parallel-beam set-up A parallel beam Goebel mirror (mostly Cu radiation is used) A small slit would also work, at the cost of intensity A stage able to precisely adjust the sample height (z-alignment) A parallel beam attachement on secondary side (Soller plate collimator, defining the instrumental resolution) A 0-D detector (e.g. scintillation counter or LYNXEYE in 0-D mode)

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Grazing incidence diffraction Ag2Te thin film on glass

13000 12000 11000 10000

Bragg-Brentano geometry

13000

Grazing incidence geometry

12000

11000

10000

9000

Lin (Counts)

Lin (Counts)

8000

7000

GIXRD emphasizes the signal of the Ag2Te nanocrystallites, and the glass substrate signal is reduced
9000 8000 7000 6000 5000 4000

6000

5000

4000

3000
3000

2000
2000

1000
1000

0
0 5 10 20 30 40 50 60 70 80 90

10

20

30

40

50

60

70

80

90

2-Theta - Scale

2-Theta - Scale

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GIXRD The Footprint


Footprint of the beam on surface: The all idea of GIXRD is to increase the number of diffracting crystallites (low incident angle) and increase the flux density (Goebel mirror). Depending on the sample length, the layer density and the expected penetration depth, an incident angle is chosen and remains fixed during the data collection. d : beam width L : sample length || beam D : illuminated area

L
42

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GIXRD Data collection


A detector scan (or 2 scan) is performed. The use of a Soller plates collimator maintains a good resolution in 2 (given by the acceptance of the Soller plates) while getting diffraction signal from the whole footprint on the sample.

Soller plates collimator defines the instrumental resolution! Available: 0,1, 0,2, 0,3, 0,4

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Grazing Incidence Diffraction Phase ID depth profile


LYNXEYE 0D Gbel mirror

Equatorial soller

XYZ stage

Incident angle Theta=0.2 to few degrees

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Grazing Incidence Diffraction Phase ID depth profile

At 0,2 deg incident angle, only Mo layer is detected. At higher incident angle, the YH2 layer is reached and starts to diffract.

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Combination of GIXRD with IP-GIXRD

Standard GIXRD or socalled coplanar geometry

In-plane GIXRD or so-called non-coplanar geometry

The idea remains the same: optimizing the grain statistic when looking at different grain orientations
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ULTRA-GID Coplanar vs. Non-Coplanar Diffraction


Coplanar diffraction
(hkl) // sample surface ULTRA-GID @ 0

D 2IP-GID f

Non-coplanar diffraction
In-Plane GID (hkl) sample surface ULTRA-GID @ 90

i i

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XRR on Si/SiO2/Si

LEPTOS results 100,3 nm SiO2 14,7 nm Si

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Coplanar GIXRD on Si/SiO2/Si

TOPAS results Cubic Si a=5.41285 A 9 nm normal crystallite size

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Non-coplanar GIXRD on Si/SiO2/Si

TOPAS results Cubic Si a=5.41285 A 14 nm lateral crystallite size

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XRR on ZrO2/Si
LEPTOS results 3,2 nm ZrO2

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Coplanar GIXRD on ZrO2

TOPAS results Tetragonal ZrO2 a=3,5658 A c=5,1614 A 3,4 nm normal crystallite size

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Non-coplanar GIXRD on ZrO2

TOPAS results Tetragonal ZrO2 a=3,5994 A c=5,18424 A 30,4 nm lateral crystallite size

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Thin Film XRD Methods Parameters of Interest


Grazing incidence Diffraction (GIXRD)
depth dependent information phase identification lattice parameter microstructure (size/strain) residual stress

X-Ray Reflectometry
layer thickness composition roughness density porosity

Stress and Texture


orientation distribution orientation quantification residual stress epitaxial relationship

High-Resolution X-Ray Diffraction


thickness lattice parameter lattice mismatch composition strain & relaxation lateral structure mosaicity (crystallinity) defects
14-15/12/2011

Reciprocal Space Mapping


lattice parameter lattice mismatch composition orientation relaxation lateral structure

In-Plane GIXRD
IP-lattice parameter IP-crystallite size IP-orientation epitaxial relation

Advanced X-ray Workshop

Bruker Confidential

54

Residual stress analysis on thin TiN layer The multiple (hkl) approach
The conventional sin2 method using (i) a unique (hkl) Bragg condition and (ii) different sample orientations with respect to the incident beam (iso- or side-inclination mode) has not been successful due to the weak diffracted intensity. For layer thicknesses around 20 nm, the only geometry were intensity is significant enough for further analysis is GIXRD. Using small angle of incidence the effective sampling volume is confined in the surface region resulting higher diffracted intensities than conventional diffraction methods. By measuring lattice strain using different hkl reflections (the incidence angle is kept constant while the detector is moved along the 2 circle) the direction of the diffraction vector can be varied without tilting the specimen physically: under such conditions the inclination angle is equal to hkl = hkl -

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Experiments with D8 ADVANCE Configuration of the diffractometer


Goniometer Measurement circle Tube Tube power Primary optics Sample stage Secondary optics Detector D8 ADVANCE Theta/Theta 560 mm 2.2 kW Cu long fine focus 40 kV / 40 mA Focusing Goebel mirror (*) 0,4 mm exit slit XYZ stage with vacuum chuck 0,4 deg equatorial Soller slit Scintillation counter or LYNXEYE in 0D mode

(*) A focusing Goebel mirror gives a lower penetration depth resolution, but a higher flux on the sample surface. If the customer has a focusing mirror for capillary measurements, he can definitely use it for GIXRD.
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Residual stress analysis on thin films GIXRD scan on a 25 nm TiN layer


GIXRD on Sample 1A : phase ID
[2,0,0] [2,2,2] [4,0,0] [3,3,1] [4,2,0] [ 1, 1, 1] [ 2, 2, 0] [ 3, 1, 1]

370 360 350 340 330 320 310 300 290 280 270 260 250 240 230

TiN osbornite

Lin (Cps)

220 210 200 190 180 170 160 150 140 130 120 110 100 90 80 70 60 50 40 30 20 10

30

40

50

60

70

80

90

100

110

120

[4,2,2]

130

140

[5,1,1]

150

2-Theta - Scale
Commander Sample ID - File: GID@0,3245.raw - Type: Detec tor Scan - Start: 30.000000 - End: 146.00000 0 - Step: 0.100000 - Step time: 40. s - Temp.: 25 C (Room) - Time Started: 0 s - 2-Theta: Operations: Import 03-065-4085 (I) - Osbornite, syn - TiN0.98 - Y: 99.90 % - d x by: 1. - WL: 1.5406 - Cubic - a 4.24190 - b 4.24190 - c 4.24190 - alpha 90.000 - beta 90.000 - gamma 90.000 - Face-centered - Fm-3m (225)

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Residual stress analysis on thin films The refraction effect


The refraction of the incident beam and diffracted beam i at the surface of the specimen causes a positive shift between the measured peak position 2 and the true Bragg angle 2 Brhkl: 2 hkl = 2 2 Brhkl, where 2Brhkl = t- i
Qhkl hkl
Surf. normal

Measuring geometry in GIXRD experiment: the angle of incidence, t the refraction angle, i the incidence angle of the diffracted beam 14-15/12/2011 Advanced X-ray Workshop 58

Residual stress analysis on thin films XRR scan for critical angle determination

C= 0.311

From Leptos fit: 25 nm TiN layer

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Residual Stress Analysis on Thin Films Data Treatment LEPTOS

Evaluation of the peak K1position

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Residual Stress Analysis on Thin Films Data Treatment LEPTOS

Peak shift due to the refraction effect

n=1--i, where sin2c=2 and =(/4)

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Residual Stress Analysis on Thin Films Data Treatment LEPTOS

-4,7 0.5 GPa

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Stress Gradient Multiple (hkl) Approach

1600 1500 1400 1300 1200 1100 1000 900 800 700 600

Incident angle from 0,5 to 3,5

Q(hkl)

(hkl)

Detector scan

Sqrt (Cps)

500 400 300

1,2m TiCrN on Fe

200

100

10

0 31 40 50 60 70 80 90 100 110 120 130 140 150

2-Theta - Scale
File: TiCrN_0.50deg.raw - Type: 2Th alone - Start: 30.000 - End: 150.000 - Step: 0.0 50 - Step ti me: 60. s - Theta: 0.500 Y + 5.0 mm - File: TiCrN_1.25deg.ra w - Type: Detector Scan - Start: 30.000 - End: 150.000 - Step: 0.050 - Step time: 60. s - Theta: 1.250 Y + 10.0 mm - File: TiCrN_2.00deg.raw - Type: Detector Scan - Start: 30.000 - End: 150.000 - Step: 0.050 - Step time: 60. s - Theta: 2. 000 Y + 15.0 mm - File: TiCrN_2.75deg.raw - Type: Detector Scan - Start: 30.000 - End: 150.000 - Step: 0.050 - Step time: 60. s - Theta: 2. 750 Y + 20.0 mm - File: TiCrN_3.50deg.raw - Type: Detector Scan - Start: 30.000 - End: 150.000 - Step: 0.050 - Step time: 60. s - Theta: 3. 500

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Stress Gradient Multiple (hkl) Approach


Incident angle from 0,5 to 3,5

1,2m TiCrN on Fe
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Higher stress at the surface


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Texture analysis on thin films


Pt layer on Si Point focus, Polycap and scintillation counter (311) texture of platinum recorded at 81.6 using a 7 grid 30 min measurement time The fiber texture is apparent

min

max min

max min

max

Simulation using MULTEX software


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Texture analysis on thin films


TiN pole figure simulation using MULTEX Point focus, POLYCAP and scintillation counter
(422)

(220)

(111)

As measured

Simulated Residual

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