positron beam studies of defects in...
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Positron Beam Studies of Defects in SemiconductorsPositron Beam Studies of Defects in Semiconductors
R. Krause-Rehberg, F. Börner, F. Redmann, J. Gebauer, S. Eichler
Universität Halle, FB Physik
� The development of the technique
� Recent progress: lateral and depth resolution enhancement
� Example: The Rp/2 effect in Si
� Future developments
Martin-Luther-Universität Halle
Martin-Luther-Universität
Halle-Wittenberg
Monoenergetic positrons by moderation
Martin-Luther-Universität Halle
� positron annihilation was very successful in defect identification in last decades
� semiconductor technology: thin layers (epitaxy, ion implantation)
� broad energy distribution due to β+ decay
� some surfaces: negative workfunction ⇒ moderation (rather unefficient)
Energy distribution after β+ decayEffect of moderation
Conventional positron beam technique
Martin-Luther-Universität Halle
� positron beam can be made from monoenergetic positrons
� often: magnetically guided for simplicity
� disadvantage: no simple lifetime measurements and bad lateral resolution
� defect studies by Doppler-broadening spectroscopy
� characterization of defects only by line-shape parameters or positron diffusion length
Information from Doppler-broadening spectroscopy
Martin-Luther-Universität Halle
� S parameter does not contain all information
� W parameter determined by annihilation with core electrons ⇒ chemical sensitivity
� R parameter was invented in 1978
S. Mantl, W. Triftshäuser, Phys. Rev. B 17 (1978) 1645
� this parameter was revitalized by the S-W-plotL. Liszkay et al., Appl. Phys. Lett. 64 (1994) 1380
506 508 510 512 514 516 518 5200,0
0,2
0,4
0,6
0,8
1,0
defect-free
defect-riche+ annihilationin GaAs
AS
norm
aliz
ed in
tens
ity
γ energy (keV)
514 515
AW
b d b
b d b
S S S SR
W W W W
− −= =− −
S. Eichler, PhD Thesis, 1997
Ion implantation in Si
0 .92
0 .96
0 .96 0 .98 1 .00
1 .00
1 .04
M e an p o s itro n d ep th (µ m )
P o sitro n e n erg y (ke V )
d e fec t
su r face I
su r face II
b u lk
B :S i 5 0 , 1 5 0 , 3 0 0 k e V
1 ·1 0 cm1 4 -2
re fe re n ce
2 ·1 0 c m1 6 -2
0 1 0 2 0 3 0 4 0
0 0 .59 1 .92 3 .83 6 .24
S pa
ram
eter
W parameter
S. Eichler, PhD Thesis, 1997
.××
4 0 0 6 0 0 8 0 0 1 0 00 1 2 00
1 .00
1 .02
1 .04
1 .06
1 .08
1 .10
S i:S i 5×1 0 cm1 4 -2
S i:S i 1×1 0 cm1 5 -2
annea ling tem pera tu re (K )
norm
aliz
edla
yer
Spa
ram
eter
Complex defect reactions show up in S-W-plot
Martin-Luther-Universität Halle
� defects of self-implantation of Cz-Si (300 keV) show a complex annealing behavior
� during annealing: defect reactions take place
� oxygen-vacancy complexes are formed and grow further
� although more detailed information by S-W-plot: positron lifetime absolutely essential
for determination of open-volume and trapping fraction
Ion implantation in Cz-Si
� coincident detection of second annihilation γ quantum:strong reduction of background
� high-momentum region accessible
� comparison with theoretically calculated spectra:
information on chemical environment of annihilation site
Doppler-coincidence spectroscopy
Martin-Luther-Universität Halle
(Gebauer, unpublished)
E1+E2= 2 m0 c2
=1022 keV
500 505 510 515 520 525
10-5
10-4
10-3
10-2
10-1
100
Rel
ativ
e in
tens
ity
γ-ray energy [keV]
with coincidence
without
K.G. Lynn et al., Phys. Rev. Lett. 38 (1977) 241
M. Alatalo et al., Rev. B 51 (1995) 4176.
� Doppler spectra show only minor changes
� difference or ratio plots: characteristic elemental features
� a single atom in direct neighborhood of a vacancy leaves its mark (VGa-TeAs in GaAs:Te)
� chemical senistivity of DOBS is a real advantage over lifetime spectroscopy
Doppler-coincidence spectroscopy in GaAs
Martin-Luther-Universität Halle
J. Gebauer et al., Phys. Rev. B 60 (1999) 1464
0 10 20 30
0,5
1,0
1,5
Electron momentum pL (10
-3 m
0c)
Te Ga As Si
Rat
io t
o d
efec
t-fr
ee G
aAs
0,8
1,0
10 20 30
0,8
1,0
VGa
-SiGa
Vacancy in GaAs:Te
Experiment
VGa
-SiGa
VGa
-TeAs
VGa
VAs
Theory
Electron momentum pL (10-3 m
0c)
Rat
io t
o d
efec
t-fr
ee G
aAs
0 10 20 3010-6
1x10-5
1x10-4
10-3
10-2
Elemental Si Ga As Te
ρ (p
) [1
03 (m
0c)-1]
Electron momentum pL (10-3 m
0c)
Martin-Luther-Universität Halle
Positron lifetime spectroscopy using monoenergetic positrons
� positron lifetime measurement more difficult
� a system of chopper and bunchers: short
pulses of monoenergetic positrons
� problems with sidepeaks are solved
� another system: Tsukuba
� more systems under construction
Schödelbauer et al., NIM 34 (1988) 258Kögel et al.,
Mat. Sci. Forum 175 (1995) 107
n-type Si
Munich system
� Semiconductor devices nm-sized ⇒ Positron microscopes and microprobes required
� However: positron diffusion length is fundamental limit for lateral resolution
� no sense to improve resolution below 500 nm
Improvement of lateral resolution
Martin-Luther-Universität Halle
H. Greif et al., Appl. Phys. Lett., 71 (1997) 2115
Bonn Positron Microprobe Munich Positron Microscope
W. Triftshäuser et al., NIM B 130 (1997) 265
� for 3D-imaging of defects: depth resolution must also be improved
� positron implantation profile rather broad compared to L+ at energies > 10 keV
� Makhov function roughly describes this profile
Improvement of depth resolution
Martin-Luther-Universität Halle
−=
− m
m
m
z
z
z
mzEzP
00
1
),(
� idea: stepwise removal of surface and
measurement with small e+ energy
� chemical etching:
N.B. Chilton and M. Fujinami, AIP Conf. Proc. 303 (1994) 25H. Kauppinen, C. Corbel, K. Skog, K. Saarinen, T. Laine, P. Hautojärvi, P. Desgardin and E. Ntsoenzok, Phys. Rev. B 55 (1997) 9598F. Börner, S. Eichler, A. Polity, R. Krause-Rehberg, R. Hammer and M. Jurisch, Appl. Surf. Sci. 149 (1999) 151P.J. Simpson, M. Spooner, H. Xia and A.P. Knights, J. Appl. Phys. 85 (1999) 1765
P.G. Coleman and A.P. Knights, Appl. Surf. Sci. 149 (1999) 82
� another idea: surface removal by ion sputtering
� test structure: a-Si/SiO2/c-Si
� sputter conditions:
Improvement of depth resolution by ion sputtering
Martin-Luther-Universität Halle
4 8 5 n m
6 0 0 n m
a -S i
c -S i
S iO 2
A r rad ia tio n
Θ
� Ar+ of 2.5 keV at 60° angle
� 2×10-6 Torr (3 ×10-4 Pa)
� about 3 nm / min
0 2 4 6 8 1 0 1 2 0 .9 0
0 .9 5
1 .0 0
1 .0 5
1 .1 0
S p u tte r s tep
S surf
/S re
f
0 .8
1 .0
1 .2
1 .4
1 .6
1 .8
2 .0
W su
rf /W
ref
c -S i su bstra te S iO 2 (60 0 n m ) a-S i (4 85 nm ) S i o x id e
0 .9 2
0 .9 4
0 .9 6
0 .9 8
1 .0 0
1 .0 2
1 .0 4
S/S
bulk
at 2
.5 k
eV
0 .9 2
0 .9 4
0 .9 6
0 .9 8
1 .0 0
1 .0 2
1 .0 4
S/S
bulk
0 .0 0 .2 0 .4 0 .6 0 .8 1 .0 1 .2
1 .0
1 .2
1 .4
1 .6
1 .8
D ep th ( µ m )
W/W
bulk
at 2
.5 k
eV
1 .0
1 .2
1 .4
1 .6
1 .8
W/W
bulk
c -S i s u b s tra te S iO 2 (6 0 0 n m ) a -S i (4 8 5 n m )
S i o x id e
Surface parameters
Please visit our Poster: „Improved depth resolution of slow positron method- detailed determination of defect profiles“ presented by F. Börner
Martin-Luther-Universität Halle
Defects in high-energy self-implanted Si The Rp/2 effect
� after high-energy (3.5 MeV) self-implantation of Si (5 ×1015 cm-2) and RTA annealing
(900°C, 30s): two new gettering zones appear at Rp and Rp/2 (Rp = projected range of Si+)
� visible by SIMS profiling after intentional Cu contamination
0 1 2 3 41015
1016
1017
Cu
conc
entr
atio
n (c
m-3)
Depth (µm)
RpRp/2
SIMS
� at Rp: gettering by interstitial-type
dislocation loops (formed by excess
interstitials during RTA)
� no defects visible by TEM at Rp/2
� What type are these defects?
TEM image by P. Werner, MPI Halle
Interstitial type
[1,2]
Vacancy type
[3,4]
[1] R. A. Brown, et al., J. Appl. Phys. 84 (1998) 2459[2] J. Xu, et al., Appl. Phys. Lett. 74 (1999) 997[3] R. Kögler, et al., Appl. Phys. Lett. 75 (1999) 1279[4] A. Peeva, et al., NIM B 161 (2000) 1090
Martin-Luther-Universität Halle
Investigation of the Rp/2 effect
by conventional VEPAS
� the defect layers are expected in a
depth of 1.7 µm and 2.8 µm corresponding
to E+= 18 and 25 keV
� implantation profile too broad to
discriminate between the two zones
� simulation of S(E) curve gives the same
result for assumed blue and yellow
defect profile (solid line in upper panel)
� furthermore: small effect only
� no conclusions about origin of Rp/2 effect
possible
0 1 2 3 4 5 6 0 .0 0
0 .0 1
0 .0 2
0 .9 4
0 .9 6
0 .9 8
1 .0 0
1 7
1 10 ×
1 10 ×
1 8
P(z
,E)
D e p th ( µ m )
P o sitron e n e rg y (k e V )
40 35 30 25 20 15 10 0
S/S
bulk
defe
ct d
ensi
ty (
cm -3
)
re fe ren ce im p lanted andan nea led + C u
18 keV25 keV
Martin-Luther-Universität Halle
Getter centers after high-energy self-implantation in Si
0,95
1,00
1,05
1,10
1,15
W/W
ref a
t 7.5
keV
0,995
1,000
1,005
1,010
1,015
S/S
ref a
t 10
keV
0 1 2 3 4 5 6
1016
1017
PositronAnnihilation
SIMS
Cu
dens
ity (
cm-3)
Depth (µm)
TEM
surface RpRp/2
0 1 2 3 4 5 6
1.000
1.005
1.010
1.015
Rp/2 R
p
Depth (µm)
S/S re
f
0.95 1.00 1.05 1.10
surface
running parameter:depth
Rp/2R
p
bulk
W/W
Please visit our Poster: „Impurity gettering in high-energy ion-implanted siliconat Rp/2 by vacancy-type defects“
� the depth-enhanced VEPAS show clearly open-volume
defects at Rp/2 and Rp
� they must be different (see S-W-plot)
� �normal� behavior of W parameter at Rp but high value at
Rp/2: Cu decorates the vacancy-type defect
Doppler-coincidence and lifetime spectroscopy
Martin-Luther-Universität Halle
0 2 4 6 8
0
200
400
600
-60
-40
-20
0
20
0 8 16 24 32
Cu
γ energy (difference to 511 keV)
RTA-annealed
RTA-annealed +Cu contaminated
pL (10-3 m
0c)
as-implanted
Dif
fere
nce
to b
ulk
Si (
a.u.
)
0 1 2 3 4200
250
300
350
400
450
RpR
p/2
τbulk
τ def (
ps)
Depth (µm)
60
80
100
after annealingCu contaminated
Inte
nsity
(%
)
� Doppler-coincidence shows the existence of Cu
at the annihilation site
� lifetime spectroscopy needed for size of open
volume
� at Rp/2: τd=450 ps
� at Rp: τd=320 ps
� lifetimes independent of
copper contamination
� intensities behave
different
� Conclusions
� Rp/2: small vacancy clusters are getter centres
� Rp: positrons are trapped by dislocation loops; trap density
decreases during Cu diffusion; no copper close to the positron
trap
Martin-Luther-Universität Halle
Positron microprobe at LLNL
� Positrons generated by LINAC; twofold re-moderation and bunching system
� E+ = 1�50 keV
� spot about 1 µm
� 107 e+/s expected
Martin-Luther-Universität Halle
Research reactorFRM-II, Munich
Photos: 4-July-2000 (source: internet)
experimental hall
reactor vessel moderator tank
construction site
� positron source by a nuclear
reaction: 113Cd(n,γ)114Cd
� three γ rays → pair production
� continuous positron beam
� ≈1010 slow e+/s expected
Martin-Luther-Universität Halle
Positron source at an Free-Electron Laser
� electron beam at FEL is bunched (length: ≈ 1 ps repetition time: ≈ 100ns)
� beam energy: > 50 MeV power: > 50 kW
� two such systems under construction in Germany: DESY (Hamburg) & ELBE (Rossendorf)
p sn s ≈
� in September 1999: Workshop at DESY (40 participants / 11 European countries):
� Agreement: �EPOS � European Positron Source for Applied Research�
� Conceptual Report now available (done by 20 scientists / 8 countries)
p o ssib lee so u rce+
p ossib lee so urce+
Please visit our Poster: „EPOS - A European Positron Source for Applied Research “
Martin-Luther-Universität Halle
Future developments
� positron beam technique now widely accepted as unique tool for defect
detection
� important: combination of Doppler broadening with positron lifetime
spectroscopy
� powerful: comparison Doppler-coincidence spectroscopy ⇔ theory
� new: - 3D-imaging of defects
- direct observation of defect kinetics in real time
� needed: - focused high-brightness positron beams operated as
user-dedicated facilities- more efficient moderators
This presentation can be found as pdf-file at our Webpage:
http://www.ep3.uni-halle.de/positrons