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X-ray diffraction techniques for thin films

Rigaku Corporation Application Laboratory Takayuki Konya


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Todays contents (PM)


Introduction X-ray diffraction method
Out-of-Plane In-Plane Pole figure Reciprocal space mapping High resolution rocking curve

X-ray reflectivity

Advantage of X-ray diffraction (XRD) method Probed depth control by incidence angle Nondestructive Measurement under atmosphere pressure

What can we see?


(hkl) a,b,c Thickness, Density, Roughness d Phase Identification ? , Interface, transition layer, etc Crystal structure Crystal quality, lattice parameter, etc Crystal orientation Single: orientation relation of substrate & film Poly: preferred orientation
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What XRD reveals


Position and coordinate of reciprocal lattice points lattice constant crystal orientation lattice distortion

spread of reciprocal lattice points degree of orientation preferred

Shape of a reciprocal lattice distribution crystal perfection defects mosaicity

Structure parameters
Structure Parameter Thickness Layer Structure Density Roughness Phase ID Crystal System Lattice Crystal Constant Structure Crystal quality Preferred Orientation Orientation Relation Order 1~103nm Precision :~several % H2O~Heavy Metals 0.2~several nm ~several nm Precision : 0.05~0.00005nm Poly~Single, Perfect Crystals Random~Preferred Orientation ~Single Crystal Relation between Film & Substrate Analysis Method Xray Reflectivity Xray Reflectivity Xray Reflectivity In-Plane XRD Out-of-Plane XRD etc In-Plane XRD Out-of-Plane XRD etc In-Plane XRD Out-of-Plane XRD etc In-Plane XRD Out-of-Plane XRD etc Pole Figure ect Rocking Curve Reciprocal Space Map etc

Todays contents (PM)


Introduction X-ray diffraction method
Out-of-Plane In-Plane Pole figure Reciprocal space mapping High resolution rocking curve

X-ray reflectivity
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Todays contents (PM)


Introduction X-ray diffraction method
Out-of-Plane In-Plane Pole figure Reciprocal space mapping High resolution rocking curve

X-ray reflectivity
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Difference between Scan Modes


The orientation of observed crystal plane depends on scanning mode.
Out-of-Plane scan Film scan In-Plane scan

Observed plane is.. Observed plane is.. parallel to the surface

tilting (changing during a scan)

perpendicular to the surface


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What is In-Plane XRD?


The detector moves parallel to the surface. Diffracted x-ray Incident x-ray

Diffraction angle 2B
Reflected x-ray

Grazing incidence (fixed angle) Observing planes are perpendicular to the surface.
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Outward of In-Plane Attachment


Scanning motion is completely perpendicular to /2 scan.
/2 scan

In-Plane measurement (2/ scan)

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In-plane effect
100

Intensity (cps)

Intensity (cps)

80 60 40 20 0 20 30 40

022

1400

In Plane

1200 1000 800 600 400 200 0 20

111

Out of Plane

111 311
50 60

400133 422
70 80 90

220 113 004 331 224


30 40

2/ (degree)

2/ (degree)

50

60

70

80

90

111

In -Plane In-Plane

220 poly-Si Glass

Out -of-plane Out-of-plane

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Probed depth control ?


1 1000 0.1

extinction distance (nm)

100

0.01

0.001 10 0.0001 0.0 0.2 0.4 0.6 0.8 1.0 incident angle (degree)

Sample:Al Wavelength:1.54056CuK1
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Surface & Interface Structure


250

In-Plane In-Plane XRD XRD


Al(111) Al+Cu Incident angle 0.2 deg. 0.5 deg.

200

Intensity (cps)

150

Al ~300nm
Al(220) Al(311) Cu(220) Al(222)
60 70 80

Transition layer Al+Cu

100

50

Al+Cu Cu(111) Cu(200)

Cu SiO2 Si (substrate) Ta

0 30 40 50

2/(degree)

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Todays contents (PM)


Introduction Advantage of reciprocal lattice vector X-ray diffraction method
Out-of-Plane In-Plane Pole figure Reciprocal space mapping High resolution rocking curve

X-ray reflectivity
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Single crystal and random orientation

Single crystal

Fiber orientation

Random orientation

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Orientation conditions and pole figure


(111) pole figure
=90=0

(220) pole figure


=90=0

Random orientation

=90

=270

=90

=270

=180 =90=0

=180

=70.5
=90

=90=0

=35.3

{111} fiber orientation

=90

=270

=270

=180 =90=0

=180 =90=0

(111) single crystal

=90

=270

=90

=270

=180

=180

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Todays contents (PM)


Introduction Advantage of reciprocal lattice vector X-ray diffraction method
Out-of-Plane In-Plane Pole figure Reciprocal space mapping High resolution rocking curve

X-ray reflectivity
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Reciprocal space mapping


Diffraction intensity distribution is plotted on reciprocal space.
2/ ghkl ko
/ 2

kg

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Epitaxial layer structures


Relaxation
00l cubic[112]

Strain
00l

Misorientation
substrate[001] 00l cubic[112] film[001] tetragonal[112]

hh0

hh0

hh0

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Reciprocal space mapping


Mosaic spread
GaAs115

qy/-1

AlGaAs115

Broadening in direction of sample rotation

Mismatch (strained)

qx/-1

Broadening in direction of radial scan


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Todays contents (PM)


Introduction Advantage of reciprocal lattice vector X-ray diffraction method
Out-of-Plane In-Plane Pole figure Reciprocal space mapping High resolution rocking curve

X-ray reflectivity
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High- resolution rocking curve


The differences of lattice spacing between the substrate and epitaxial films are observed. Thickness and composition ratio of epitaxial films (when the degree of relaxation is known. ) 2/ kg K g log(I ) hkl ko 2/
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When the sample has multilayer structure


Complicated oscillation composed of oscillation from each layer is observed.
10 10 10 Reflectivity 10 10 10 10
-1

(004)

-2

GeSi GeSi

Si

-3

-4

-5

-6

GexSi(1-x) 50nm GexSi(1-x) 300nm Six=0.015 substrate x=0.050 x=0.015

-7

-2000

-1000

1000

Deviation Angle (arcseconds)

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When the sample has superlattice structure


Satellite peaks are observed.
10-1 10-2 10-3 Reflectivity 10-4 10-5 10-6 10-7 10-8 -8000 -4000 0 4000 8000

0 -1 -3 -2 1

GaAs

(004)

3 4 GaAs 5nm InxGa(1-x)As 5nm GaAs substrate 10L

Deviation Angle (arcseconds)

x=0.200
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How to interpret the profile


Si substrate

(004)

10 10

-1

SiGe mismatch

-2

SiGe mismatch
-3

Reflectivity

10 Oscillation period -4 SiGe thickness 10 10 10 10


-5

GexSi(1-x) 50nm x=0.050 GexSi(1-x) 300nm x=0.015 Si substrate

Intensity

-6

-7

Oscillation period SiGe thickness

-2000

-1000

1000

diffraction angle (eco arcsec.) Deviation A ng le (arcs nds )


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Todays contents (PM)


Introduction X-ray diffraction method
Out-of-Plane In-Plane Pole figure Reciprocal space mapping High resolution rocking curve

X-ray reflectivity
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What reflectivity reveals


X-ray reflectivity nondestructively reveals - layer structure of multi layers - thickness (1 to 1000nm) - density as an absolute value - surface and interface roughness
Interface roughness thickness layer 1 thickness layer 2 substrate density

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How to interpret the profile


Critical angle c Density
10
0

roughness 1 roughness 2 density 1layer 1 thickness1 roughness 3 density 2layer 2 thickness2

10

-1

Reflectivity

10

-2

Period of oscillation Thickness

density 3

substrate

10

-3

Amplitude of -4 oscillation -5 Contrast of density 10


10 0 2 4 2/ (degree)

Decay of amplitude Interface roughness Decay of reflectivity Surface roughness


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X-ray reflectivity measurement of TiN film


10 10 10
0 -1

Simulation Experimental

-2

Reflectivity

10 10 10 10 10

-3

TiN SiO2 Si
density 3 (g/cm ) 3.680 2.900 2.260 Thickness (nm) 1.230 8.400 127.700 substrate

-4

-5

-6

-7

0.0

0.5

1.0

1.5

2.0

Layer TiN TiN SiO2 Si

Roughness (nm) 1.420 1.000 0.220

Grancing angle (degree)

Coating Coatinglayer layer

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