김 창수 ([email protected]) 한국표준과학연구원 (KRISS) 산업측정표준본부 2013 X-선 회절 측정클럽 개별워크샵 고분해능 XRD의 LED 소재분석 응용 2013. 8. 27
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6-X- 2013. 8. 27
’13
XRD - X- - HRXRD (High-Resolution XRD) - - LED : WPM
’13
- a, b, : angles
- 1
Indices of directions : [uvw]
/
b
c
a
1
1
- 2
Hexagonal
’13
(dhkl)
LiAl 0.24
Mn 1.76
O 4
.u .]
n = 2d sin
: X-
n : (1,2,3….)
d :
: Bragg
1+2
LiAl 0.24
Mn 1.76
O 4
.u .]
Perovskite Hexagonal Diamond Cubic
Bragg X-Ray Diffractometer (phase) : ICDD PDF cards
ICDD (International Center for Diffraction Data)
PDF ( Powder Diffraction File)
(residual stress), , /...
() XRD
/...
30 40 50 60 70 10
0
1
20000
40000
LED (Light Emitting Diode)
(High-resolution) X-
aL
aS
-150 -125 -100 -75 -50 -25 0 25 50 75 100 125 150
( = 10" )
X-ray Optics for High-resolution
- :
Channel Cut Crystal(CCC)
( : 1º = 3600")
Optics Resolution Intensity
X-Rays
CCC
XRD
- Triple Axis Difractometer (or Diffraction) : TAD Monochromator + Sample + Analyser
() :
: single/multi-layers, superlattices (MQWs)
- : scan
- (diffuse scattering)
- () :
’13
HRXRD /
Compound Semiconductor Data Storage Defence Displays
Electronics
Photonics
Semiconductor
(optoelectronics)
Epitaxial oxides : BZT, PZT, YBCO, BST, STO, PTO, ZnO ...
: GaMnAs, ZnMnSe, ZnMnTe,
ZnMnS, CdMnTe …
highly textured layers(AuCo/Si) …
’13
Schematic diagram for HRXRD
(rocking curve) :
Bragg intensity
’13
Rocking Curve – , FWHM
10 1
10 2
10 3
10 4
10 5
- layer thickness - lattice parameter - strain relaxation - layer composition
(FWHM) - crystalline quality -mosaic spread (dislocation density) - sample curvature
’13
X-ray source
( : (001) )
’13
FWHM(RC)
0
2000
4000
6000
4-b Ge (220)s monochromator
FWHM : Full Width at Half Maximum
X- – No. 1
6 - X- FWHM : 4b-Ge (044) monochromator - Full wafer mapping (FWHM) uniformity
10.9 10.9 10.7
11.0 10.1 10.7
6” Wafer (150mm)
4 bounce Ge(220)
3.9 4.1 3.9
3.6 4.1 4.4
4 bounce Ge(440)
6” Wafer (150mm)
25mm
25mm
– X-
DAD Rocking Curve - : AlxGa1-xAs/GaAs Epilayer
AlGaAs x = 0.25
Sf cos2
’13
’13
TAD /2 scan and RSM for AlxGa1-xN/GaN
- TAD /2 scan AlGaN (Al )
- TAD /2 scan
-2000 -1000 0 1000 2000
t = 1200 X = 0.12
TAD
DAD
GaN
Al composition (%) Thickness (nm)
RSMs for InxGa1-xN/GaN epilayers
TAD
GaN
In te
1 6 20
2 70 70
C-plane sapphire (substrate)
Semi-Insulating GaN : 2
AlxGa1-xN FWHM (arcsec)
GaN(002) ~ 300
GaN(102) ~ 780
60 mol/min
80 mol/min
100 mol/min
120 mol/min
In te
5.1463 5.1356 5.1249 5.1148
D (=2C13/C33)
AlGaN /
’13
RSM(Reciprocal space map) : GaN(105) TMAl
(μmol/min) 60 80 100 120
5.1512 5.1413 5.1319 5.1230
3.1689 3.1625 3.1565 3.1512
FWHM
(arcsec, ) 450 480 500 500
3.0 3.1 3.2 3.3 3.4 3.5 3.6 3.7 3.8 3.9 4.0 4.1
0.00
0.05
0.10
0.15
0.20
GaN (eV) 3.42
AlN (eV) 6.30
x (%) 17.7 21.5 25.6 29.1
I(AlGaN)/I(GaN) 1.19 0.44 0.20 0.08
• Bowing parameter (b) : 1.3 eV
GaN GaN
’13
- direction
of the GaN ReLP 1 2 3 4 5 6
0.08
0.09
0.10
0.11
0.12
0.13
0.14
0.15
0.16
0.17
0.18
3.1890
3.1893
3.1896
3.1899
3.1902
3.1905
3.1908
3.1911
W60
W45
o m
The degree of
Barrier thickness : 7.5 nm)
LT - PL
300 350 400 450 500 550 600 650 700 750 800
W60
W45
W30
W15
0.0
0.1
0.2
0.3
0.4
0.5
W60
W45W30W15
a ti o
’13
(Standard Test Method for Determining the Orientation of
a Semiconductive Single Crystal)
d1
: d1 = √d(0) 2 + d(90)
2
- d1 p (/ )
- (bending),
Reference edge
– GaN/Sapphire surface
(100)
x
y
z
(off-cut angle miscut angle)
[1] D. Lu, D.I. Florescu, D. S. Lee, V. Merai, J. C. Ramer, A. Parekh, and E. A. Armour, J. of Crystal Growth 272, 353 (2004).
[2] A. Nakamura, N. Yanagita, T. Murata, K. Hoshino, and K. Tadatomo, phys. Stat. sol. (c) 5 (6), 2007 (2008).
’13
6” – Spec.
(
Spec1))
1 2 3
1. Core cylinder mm 15 200 100 150 200 200
2. Core cylinder mm 15 200 100 100 100 100
3. 1) % 15 25 40 50 45 45
4. Lineage mm 10 0 0 0 0 0
5. Bubble / 10 0 0 0 0 0
6. Twin - 5 0 0 0 0 0
7. EPD /cm2 10 1000 <1000 <1000 <500 <500
8. FWHM arcsec 10 20 <12 <12 <12 <12
XRD
9.Orientation
C degree 5 ±0.05 ±0.05 ±0.025 ±0.025 ±0.025 XRD
A degree 5 ±0.1 ±0.1 ±0.1 ±0.1 ±0.1 XRD
34
• /
•
•
-
= 2d1·sin(PE/2) sin( - p- PE/2)
= a·sin( - b) :
)(
)(
(certification procedure)
1 u(δ1) 0.00091 0.99587 0.09077 7
2 u(φP) 0.0316 -0.00032 0.00354 34
3 u(ω) 0.00013 1 1 ∞
uc(δ)
U 0.0022 0.0004 T/ (k=2.36/2.0)
- -
36
- X-ray source : Mo (50 kV, 200mA)
- Sample : 4” (001) Sapphire wafer
- center area 2”
- X-ray source-sample distance: 1600 mm
- X-ray film
- 12kW
- X-ray film cassette
set-up
X-ray source
Lang Camera
Sample 4B
37
Dislocations image broadening : , ↔
Sample - 6” wafer (1 t)
Sample 4B - 4” wafer (0.6 t)
’13
- : (LED )
10 : 2010. 9
- : 10
’13
X XRD LED XRD - GaN - (WPM ) HRXRD : - / - /
’11
X- (X-Ray Metrology)
’13
XRD - X- - HRXRD (High-Resolution XRD) - - LED : WPM
’13
- a, b, : angles
- 1
Indices of directions : [uvw]
/
b
c
a
1
1
- 2
Hexagonal
’13
(dhkl)
LiAl 0.24
Mn 1.76
O 4
.u .]
n = 2d sin
: X-
n : (1,2,3….)
d :
: Bragg
1+2
LiAl 0.24
Mn 1.76
O 4
.u .]
Perovskite Hexagonal Diamond Cubic
Bragg X-Ray Diffractometer (phase) : ICDD PDF cards
ICDD (International Center for Diffraction Data)
PDF ( Powder Diffraction File)
(residual stress), , /...
() XRD
/...
30 40 50 60 70 10
0
1
20000
40000
LED (Light Emitting Diode)
(High-resolution) X-
aL
aS
-150 -125 -100 -75 -50 -25 0 25 50 75 100 125 150
( = 10" )
X-ray Optics for High-resolution
- :
Channel Cut Crystal(CCC)
( : 1º = 3600")
Optics Resolution Intensity
X-Rays
CCC
XRD
- Triple Axis Difractometer (or Diffraction) : TAD Monochromator + Sample + Analyser
() :
: single/multi-layers, superlattices (MQWs)
- : scan
- (diffuse scattering)
- () :
’13
HRXRD /
Compound Semiconductor Data Storage Defence Displays
Electronics
Photonics
Semiconductor
(optoelectronics)
Epitaxial oxides : BZT, PZT, YBCO, BST, STO, PTO, ZnO ...
: GaMnAs, ZnMnSe, ZnMnTe,
ZnMnS, CdMnTe …
highly textured layers(AuCo/Si) …
’13
Schematic diagram for HRXRD
(rocking curve) :
Bragg intensity
’13
Rocking Curve – , FWHM
10 1
10 2
10 3
10 4
10 5
- layer thickness - lattice parameter - strain relaxation - layer composition
(FWHM) - crystalline quality -mosaic spread (dislocation density) - sample curvature
’13
X-ray source
( : (001) )
’13
FWHM(RC)
0
2000
4000
6000
4-b Ge (220)s monochromator
FWHM : Full Width at Half Maximum
X- – No. 1
6 - X- FWHM : 4b-Ge (044) monochromator - Full wafer mapping (FWHM) uniformity
10.9 10.9 10.7
11.0 10.1 10.7
6” Wafer (150mm)
4 bounce Ge(220)
3.9 4.1 3.9
3.6 4.1 4.4
4 bounce Ge(440)
6” Wafer (150mm)
25mm
25mm
– X-
DAD Rocking Curve - : AlxGa1-xAs/GaAs Epilayer
AlGaAs x = 0.25
Sf cos2
’13
’13
TAD /2 scan and RSM for AlxGa1-xN/GaN
- TAD /2 scan AlGaN (Al )
- TAD /2 scan
-2000 -1000 0 1000 2000
t = 1200 X = 0.12
TAD
DAD
GaN
Al composition (%) Thickness (nm)
RSMs for InxGa1-xN/GaN epilayers
TAD
GaN
In te
1 6 20
2 70 70
C-plane sapphire (substrate)
Semi-Insulating GaN : 2
AlxGa1-xN FWHM (arcsec)
GaN(002) ~ 300
GaN(102) ~ 780
60 mol/min
80 mol/min
100 mol/min
120 mol/min
In te
5.1463 5.1356 5.1249 5.1148
D (=2C13/C33)
AlGaN /
’13
RSM(Reciprocal space map) : GaN(105) TMAl
(μmol/min) 60 80 100 120
5.1512 5.1413 5.1319 5.1230
3.1689 3.1625 3.1565 3.1512
FWHM
(arcsec, ) 450 480 500 500
3.0 3.1 3.2 3.3 3.4 3.5 3.6 3.7 3.8 3.9 4.0 4.1
0.00
0.05
0.10
0.15
0.20
GaN (eV) 3.42
AlN (eV) 6.30
x (%) 17.7 21.5 25.6 29.1
I(AlGaN)/I(GaN) 1.19 0.44 0.20 0.08
• Bowing parameter (b) : 1.3 eV
GaN GaN
’13
- direction
of the GaN ReLP 1 2 3 4 5 6
0.08
0.09
0.10
0.11
0.12
0.13
0.14
0.15
0.16
0.17
0.18
3.1890
3.1893
3.1896
3.1899
3.1902
3.1905
3.1908
3.1911
W60
W45
o m
The degree of
Barrier thickness : 7.5 nm)
LT - PL
300 350 400 450 500 550 600 650 700 750 800
W60
W45
W30
W15
0.0
0.1
0.2
0.3
0.4
0.5
W60
W45W30W15
a ti o
’13
(Standard Test Method for Determining the Orientation of
a Semiconductive Single Crystal)
d1
: d1 = √d(0) 2 + d(90)
2
- d1 p (/ )
- (bending),
Reference edge
– GaN/Sapphire surface
(100)
x
y
z
(off-cut angle miscut angle)
[1] D. Lu, D.I. Florescu, D. S. Lee, V. Merai, J. C. Ramer, A. Parekh, and E. A. Armour, J. of Crystal Growth 272, 353 (2004).
[2] A. Nakamura, N. Yanagita, T. Murata, K. Hoshino, and K. Tadatomo, phys. Stat. sol. (c) 5 (6), 2007 (2008).
’13
6” – Spec.
(
Spec1))
1 2 3
1. Core cylinder mm 15 200 100 150 200 200
2. Core cylinder mm 15 200 100 100 100 100
3. 1) % 15 25 40 50 45 45
4. Lineage mm 10 0 0 0 0 0
5. Bubble / 10 0 0 0 0 0
6. Twin - 5 0 0 0 0 0
7. EPD /cm2 10 1000 <1000 <1000 <500 <500
8. FWHM arcsec 10 20 <12 <12 <12 <12
XRD
9.Orientation
C degree 5 ±0.05 ±0.05 ±0.025 ±0.025 ±0.025 XRD
A degree 5 ±0.1 ±0.1 ±0.1 ±0.1 ±0.1 XRD
34
• /
•
•
-
= 2d1·sin(PE/2) sin( - p- PE/2)
= a·sin( - b) :
)(
)(
(certification procedure)
1 u(δ1) 0.00091 0.99587 0.09077 7
2 u(φP) 0.0316 -0.00032 0.00354 34
3 u(ω) 0.00013 1 1 ∞
uc(δ)
U 0.0022 0.0004 T/ (k=2.36/2.0)
- -
36
- X-ray source : Mo (50 kV, 200mA)
- Sample : 4” (001) Sapphire wafer
- center area 2”
- X-ray source-sample distance: 1600 mm
- X-ray film
- 12kW
- X-ray film cassette
set-up
X-ray source
Lang Camera
Sample 4B
37
Dislocations image broadening : , ↔
Sample - 6” wafer (1 t)
Sample 4B - 4” wafer (0.6 t)
’13
- : (LED )
10 : 2010. 9
- : 10
’13
X XRD LED XRD - GaN - (WPM ) HRXRD : - / - /
’11
X- (X-Ray Metrology)
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