Structure perfection variations of Si crystals grown by Czochralski or floating zone methods after implantation of oxygen or neon atoms followed by annealing
Structure perfection of the silicon crystals grown by the Czochralski and floating zone methods after implantation with oxygen or neon fast iones followed by annealing at the temperatures T ~ 1050-1150 ⁰0C, when large SiOx precipitates were formed, was studied by means of various X-ray diffraction m...
Gespeichert in:
| Datum: | 1999 |
|---|---|
| Hauptverfasser: | , , , , , , , , , , , |
| Format: | Artikel |
| Sprache: | English |
| Veröffentlicht: |
Інститут фізики напівпровідників імені В.Є. Лашкарьова НАН України
1999
|
| Schriftenreihe: | Semiconductor Physics Quantum Electronics & Optoelectronics |
| Online Zugang: | https://nasplib.isofts.kiev.ua/handle/123456789/117934 |
| Tags: |
Tag hinzufügen
Keine Tags, Fügen Sie den ersten Tag hinzu!
|
| Назва журналу: | Digital Library of Periodicals of National Academy of Sciences of Ukraine |
| Zitieren: | Structure perfection variations of Si crystals grown by Czochralski or floating zone methods after implantation of oxygen or neon atoms followed by annealing / L.I. Datsenko, J. Auleytner, A. Misiuk, V.P. Klad'ko, V.F. Machulin, J. Bak-Misiuk, D. Zymierska, I.V. Antonova, V.M. Melnyk, V.P. Popov, T. Czosnyka, J. Choinski // Semiconductor Physics Quantum Electronics & Optoelectronics. — 1999. — Т. 2, № 1. — С. 56-61. — Бібліогр.: 9 назв. — англ. |
Institution
Digital Library of Periodicals of National Academy of Sciences of Ukraine| id |
nasplib_isofts_kiev_ua-123456789-117934 |
|---|---|
| record_format |
dspace |
| spelling |
nasplib_isofts_kiev_ua-123456789-1179342025-02-09T15:49:56Z Structure perfection variations of Si crystals grown by Czochralski or floating zone methods after implantation of oxygen or neon atoms followed by annealing Datsenko, L.I. Auleytner, J. Misiuk, A. Klad'ko, V.P. Machulin, V.F. Bak-Misiuk, J. Zymierska, D. Antonova, I.V. Melnyk, V.M. Popov, V.P. Czosnyka, T. Choinski, J. Structure perfection of the silicon crystals grown by the Czochralski and floating zone methods after implantation with oxygen or neon fast iones followed by annealing at the temperatures T ~ 1050-1150 ⁰0C, when large SiOx precipitates were formed, was studied by means of various X-ray diffraction methods. Considerable increments of integral reflectivities for different Bragg reflections of such samples in comparison with those calculated for a perfect crystal were detected. Broadening of the spatial intensity distribution curves for the Bragg-diffracted beams taken by a single crystal spectrometer as well as the maps of the diffuse isointensity distribution near a reciprocal lattice point, registered by the Philips high-resolution diffractometer, are shown. All of these diffraction effects related to creation of the SiOx precipitates formed on structural damages caused by implantation of oxygen or neon ions and subsequent annealing. Contrary to FZSi, where the appearence of SiOx precipitates was discovered due to intensive diffuse scattering near the layer contained the implanted oxygen ions only, in the case of CZSi samples with larger concentration of oxygen (up to 1*10¹⁸ at/cm³) such defects were formed not only near the burried layer, created by ions of oxygen or neon (with energy E = 4 MeV, dose 10¹⁴cm⁻²) but in a bulk of a crystal. Annealing of the FZSi crystals implanted by oxygen (E ~ 200 keV, dose ~ 10¹⁶-10¹⁷ cm⁻²) at enhanced hydrostatic pressure, additionally stimulated SiOx precipitation close to the implanted layer. 1999 Article Structure perfection variations of Si crystals grown by Czochralski or floating zone methods after implantation of oxygen or neon atoms followed by annealing / L.I. Datsenko, J. Auleytner, A. Misiuk, V.P. Klad'ko, V.F. Machulin, J. Bak-Misiuk, D. Zymierska, I.V. Antonova, V.M. Melnyk, V.P. Popov, T. Czosnyka, J. Choinski // Semiconductor Physics Quantum Electronics & Optoelectronics. — 1999. — Т. 2, № 1. — С. 56-61. — Бібліогр.: 9 назв. — англ. 1560-8034 PACS: 81.40.- Z,61.66. Bi https://nasplib.isofts.kiev.ua/handle/123456789/117934 en Semiconductor Physics Quantum Electronics & Optoelectronics application/pdf Інститут фізики напівпровідників імені В.Є. Лашкарьова НАН України |
| institution |
Digital Library of Periodicals of National Academy of Sciences of Ukraine |
| collection |
DSpace DC |
| language |
English |
| description |
Structure perfection of the silicon crystals grown by the Czochralski and floating zone methods after implantation with oxygen or neon fast iones followed by annealing at the temperatures T ~ 1050-1150 ⁰0C, when large SiOx precipitates were formed, was studied by means of various X-ray diffraction methods. Considerable increments of integral reflectivities for different Bragg reflections of such samples in comparison with those calculated for a perfect crystal were detected. Broadening of the spatial intensity distribution curves for the Bragg-diffracted beams taken by a single crystal spectrometer as well as the maps of the diffuse isointensity distribution near a reciprocal lattice point, registered by the Philips high-resolution diffractometer, are shown. All of these diffraction effects related to creation of the SiOx precipitates formed on structural damages caused by implantation of oxygen or neon ions and subsequent annealing. Contrary to FZSi, where the appearence of SiOx precipitates was discovered due to intensive diffuse scattering near the layer contained the implanted oxygen ions only, in the case of CZSi samples with larger concentration of oxygen (up to 1*10¹⁸ at/cm³) such defects were formed not only near the burried layer, created by ions of oxygen or neon (with energy E = 4 MeV, dose 10¹⁴cm⁻²) but in a bulk of a crystal. Annealing of the FZSi crystals implanted by oxygen (E ~ 200 keV, dose ~ 10¹⁶-10¹⁷ cm⁻²) at enhanced hydrostatic pressure, additionally stimulated SiOx precipitation close to the implanted layer. |
| format |
Article |
| author |
Datsenko, L.I. Auleytner, J. Misiuk, A. Klad'ko, V.P. Machulin, V.F. Bak-Misiuk, J. Zymierska, D. Antonova, I.V. Melnyk, V.M. Popov, V.P. Czosnyka, T. Choinski, J. |
| spellingShingle |
Datsenko, L.I. Auleytner, J. Misiuk, A. Klad'ko, V.P. Machulin, V.F. Bak-Misiuk, J. Zymierska, D. Antonova, I.V. Melnyk, V.M. Popov, V.P. Czosnyka, T. Choinski, J. Structure perfection variations of Si crystals grown by Czochralski or floating zone methods after implantation of oxygen or neon atoms followed by annealing Semiconductor Physics Quantum Electronics & Optoelectronics |
| author_facet |
Datsenko, L.I. Auleytner, J. Misiuk, A. Klad'ko, V.P. Machulin, V.F. Bak-Misiuk, J. Zymierska, D. Antonova, I.V. Melnyk, V.M. Popov, V.P. Czosnyka, T. Choinski, J. |
| author_sort |
Datsenko, L.I. |
| title |
Structure perfection variations of Si crystals grown by Czochralski or floating zone methods after implantation of oxygen or neon atoms followed by annealing |
| title_short |
Structure perfection variations of Si crystals grown by Czochralski or floating zone methods after implantation of oxygen or neon atoms followed by annealing |
| title_full |
Structure perfection variations of Si crystals grown by Czochralski or floating zone methods after implantation of oxygen or neon atoms followed by annealing |
| title_fullStr |
Structure perfection variations of Si crystals grown by Czochralski or floating zone methods after implantation of oxygen or neon atoms followed by annealing |
| title_full_unstemmed |
Structure perfection variations of Si crystals grown by Czochralski or floating zone methods after implantation of oxygen or neon atoms followed by annealing |
| title_sort |
structure perfection variations of si crystals grown by czochralski or floating zone methods after implantation of oxygen or neon atoms followed by annealing |
| publisher |
Інститут фізики напівпровідників імені В.Є. Лашкарьова НАН України |
| publishDate |
1999 |
| url |
https://nasplib.isofts.kiev.ua/handle/123456789/117934 |
| citation_txt |
Structure perfection variations of Si crystals grown by Czochralski or floating zone methods after implantation of oxygen or neon atoms followed by annealing / L.I. Datsenko, J. Auleytner, A. Misiuk, V.P. Klad'ko, V.F. Machulin, J. Bak-Misiuk, D. Zymierska, I.V. Antonova, V.M. Melnyk, V.P. Popov, T. Czosnyka, J. Choinski // Semiconductor Physics Quantum Electronics & Optoelectronics. — 1999. — Т. 2, № 1. — С. 56-61. — Бібліогр.: 9 назв. — англ. |
| series |
Semiconductor Physics Quantum Electronics & Optoelectronics |
| work_keys_str_mv |
AT datsenkoli structureperfectionvariationsofsicrystalsgrownbyczochralskiorfloatingzonemethodsafterimplantationofoxygenorneonatomsfollowedbyannealing AT auleytnerj structureperfectionvariationsofsicrystalsgrownbyczochralskiorfloatingzonemethodsafterimplantationofoxygenorneonatomsfollowedbyannealing AT misiuka structureperfectionvariationsofsicrystalsgrownbyczochralskiorfloatingzonemethodsafterimplantationofoxygenorneonatomsfollowedbyannealing AT kladkovp structureperfectionvariationsofsicrystalsgrownbyczochralskiorfloatingzonemethodsafterimplantationofoxygenorneonatomsfollowedbyannealing AT machulinvf structureperfectionvariationsofsicrystalsgrownbyczochralskiorfloatingzonemethodsafterimplantationofoxygenorneonatomsfollowedbyannealing AT bakmisiukj structureperfectionvariationsofsicrystalsgrownbyczochralskiorfloatingzonemethodsafterimplantationofoxygenorneonatomsfollowedbyannealing AT zymierskad structureperfectionvariationsofsicrystalsgrownbyczochralskiorfloatingzonemethodsafterimplantationofoxygenorneonatomsfollowedbyannealing AT antonovaiv structureperfectionvariationsofsicrystalsgrownbyczochralskiorfloatingzonemethodsafterimplantationofoxygenorneonatomsfollowedbyannealing AT melnykvm structureperfectionvariationsofsicrystalsgrownbyczochralskiorfloatingzonemethodsafterimplantationofoxygenorneonatomsfollowedbyannealing AT popovvp structureperfectionvariationsofsicrystalsgrownbyczochralskiorfloatingzonemethodsafterimplantationofoxygenorneonatomsfollowedbyannealing AT czosnykat structureperfectionvariationsofsicrystalsgrownbyczochralskiorfloatingzonemethodsafterimplantationofoxygenorneonatomsfollowedbyannealing AT choinskij structureperfectionvariationsofsicrystalsgrownbyczochralskiorfloatingzonemethodsafterimplantationofoxygenorneonatomsfollowedbyannealing |
| first_indexed |
2025-11-27T15:38:10Z |
| last_indexed |
2025-11-27T15:38:10Z |
| _version_ |
1849958484453359616 |
| fulltext |
5 6 © 1999, Institute of Semiconductor Physics, National Academy of Sciences of Ukraine
Semiconductor Physics, Quantum Electronics & Optoelectronics. 1999. V. 2, N 1. P. 56-61.
1. Introduction
The SiO
x
precipitates surrounded by system of disloca-
tion loops appearing in silicon crystals containing oxy-
gen impurity due to solid solution decay at high temper-
atures play an important role as intrinsic gettering cen-
tres for cleaning active zones of semiconductor devices
from undesirable impurities [1]. Usually, these defects
are formed on various initial structure distortions (asso-
ciations of various point defects) existing in as-grown
crystals after preliminary low temperature treatment [2].
Structure distortions induced in crystals by irradiation
with various particles (neutrons, atoms, electrons) of high
energy or during technological processes of active impu-
rity implantation can also play the role of such centres
[3, 4]. Therefore, it is interesting to make clear an effect
of implantation of silicon crystals with oxygen because
just this impurity play an important role in creation of
initial stages of large SiO
x
precipitates. It is known [5]
that the processes of SiO
x
formation in a silicon con-
taining oxygen can considerably change the integral char-
acteristics of structure perfection of a crystal, namely:
its reflectivity, the Debye-Waller factor, coeficient of ex-
tinction. Analysing character of these parameter varia-
tions, one can judge of the structural transformation in
a crystal and determine the character of existing defects.
The aim of this paper was the investigation of structure
perfection variations in a crystal by means of different
X-ray diffraction methods after annealing the samples
implanted by accelerated ions of chemically active oxy-
PACS: 81.40.- Z,61.66. Bi
Structure perfection variations of Si crystals grown by
Czochralski or floating zone methods after implantation
of oxygen or neon atoms followed by annealing
L. I. Datsenko1, J. Auleytner2, A. Misiuk3, V. P. Klad�ko1, V. F. Machulin1, J. B¹k-Misiuk2,
D. ¯ymierska2, I. V. Antonova4, V. M. Melnyk1, V. P. Popov4, T. Czosnyka5 and J. Choiñski5
1 Institute of Semiconductor Physics, National Academy of Sciences of Ukraine, Kyiv, 252028, Ukraine
2 Institute of Physics, al. Lotników 32/46, 02-668 Warsaw, Poland
3 Institute of Electron Technology, al. Lotników 32/46, 02-668 Warsaw, Poland
4 Institute of Semiconductor Physics, RAS, Nauki prosp., 13 , 630090 Novosibirsk, Russia
5 Heavy Ion Laboratory of Warsaw University, V. Pasteura 5a, 02-093 Warsaw, Poland
Abstract. Structure perfection of the silicon crystals grown by the Czochralski and floating zone
methods after implantation with oxygen or neon fast iones followed by annealing at the tempera-
tures T ~ 1050-1150 0C, when large SiO
x
precipitates were formed, was studied by means of vari-
ous X-ray diffraction methods. Considerable increments of integral reflectivities for different Bragg
reflections of such samples in comparison with those calculated for a perfect crystal were detected.
Broadening of the spatial intensity distribution curves for the Bragg-diffracted beams taken by a
single crystal spectrometer as well as the maps of the diffuse isointensity distribution near a recip-
rocal lattice point, registered by the Philips high-resolution diffractometer, are shown. All of these
diffraction effects related to creation of the SiO
x
precipitates formed on structural damages caused
by implantation of oxygen or neon ions and subsequent annealing. Contrary to FZSi, where the
appearence of SiO
x
precipitates was discovered due to intensive diffuse scattering near the layer
contained the implanted oxygen ions only, in the case of CZSi samples with larger concentration of
oxygen (up to 1*1018 at/cm3) such defects were formed not only near the burried layer, created by
ions of oxygen or neon (with energy E = 4 MeV, dose 1014cm-2) but in a bulk of a crystal. Annealing
of the FZSi crystals implanted by oxygen (E ~ 200 keV, dose ~ 1016-1017 cm-2) at enhanced hydro-
static pressure, additionally stimulated SiO
x
precipitation close to the implanted layer.
Keywords: Czochralski and floating zone silicon, SiO
x
precipitates, radiation damages, oxygen and
neon ions, Bragg-diffraction of X-ray, reflectivity, Debye-Waller static factor.
Paper received 26.02.99; revised manuscript received 04.05.99; accepted for publication 24.05.99.
L. I. Datsenko et al.: Structure perfection variations of Si crystals grown by ...
57SQO, 2(1), 1999
gen or neutral atoms (neon) having approximate mass-
es. For this purpose, Si crystals grown by Czochralski
and floating zone methods, containing different quanti-
ty of �grown-in� oxygen atoms, were used. Thus, the
process of oxygen solid solution decay was investigated
in the samples with radiation defects (with or almost
without �grown-in� interstitial oxygen atoms).
2. Materials and methods
Three Si samples of the first series I, samples 1, 2, and 3,
of (100) surface orientation and of thickness about
3,0 mm, containing rather high concentration C
0
of oxy-
gen (up to ~ 10 18 cm -3) were grown by Czochralski meth-
od (CzSi). The samples 2 and 3 were irradiated with neon
and oxygen ion beams of energy 4 MeV/u and dose
1014 particles/cm2 from the Warsaw Cyclotron [6]. The
implantation was performed by uniformly defocused
beam at room temperature. The sample 1 was kept as a
reference one. The implanted CzSi samples were next an-
nealed at 1050 0C for 5h in the atmosphere consisting of
argon (80 %) and oxygen (20 %) to create SiO
x
precipi-
tates on the radiation damages. The annealed samples
are noted as 1′, 2′ and 3′. Because of a large concentra-
tion of oxygen in CzSi, SiO
x
precipitates were formed
not only near the surface subjected to irradiation but in
the bulk of these crystals.
Six Si samples of the second (II) series, (1 - 6 ), were
grown by the floating zone (FZ) method and had low
oxygen concentrations (up to C
o
~ 1016 cm-3 ). All of them
had (111) orientation and were subjected to implantation
with oxygen ions of 200 keV energy and doses 1016 ÷
1017 cm-2. Local maximum concentration C
ol
in the
burried layer situated on the depth close to 0,4 µm
(thickness ∆t ~ 0.09 µm) was estimated to reach 4 ×1021 ÷
4 ×1022 cm-3.
Then the samples 1 - 6 of the second series were an-
nealed at 1130 °C in the argon atmosphere using high
hydrostatic pressure P (up to 12 kbar). It was done to
promote the process of SiO
x
formation [7] in the near-
surface layer containing implanted oxygen ions. The tech-
nological parameters of annealing of the FZSi crystals
are given in the Table 1.
Structure perfection changes were investigated by
means of a set of X-ray diffractometrical methods based
on the Bragg case of diffraction [7]. For characterization
of the structure state (appearence of distortions connected
with defects) the increments ∆R
i
of the measured integral
reflectivities R
i
for different Bragg diffraction maxima
after various treatments (implantation with oxygen or
neon ions or annealing), relatively to the values R
i
p ,
calculated for a perfect crystal, were used :
∆R
i
= R
i
� R
i
p = R
i
p L + 2LR
i
k . (1 )
Here: R
i
k is the kinematical reflectivity for an ideal-
mosaic crystal. Thus, analysing the ∆R
i
increments, one
could determine the static Debye-Waller factors L after
Fig. 1. Spatial intensity distributions (SID) of the Bragg diffracted beams of AgKα radiation in the samples (the first series) after
irradiation by high energy ions (E = 4MeV/u, dose 1014 particles/cm2) and annealing (1050 0C, 5 h). Non-implanted sample � 1′,
sample implanted with neon � 2′ and oxygen � 3′ ions.
0,00 0,01 0,02 0,03 0,04 0,05
0
1
2
3'
2'
1'
t , cm
I
/
I
0
*1
0
5 ,
a
rb
.u
n
its
L. I. Datsenko et al.: Structure perfection variations of Si crystals grown by ...
5 8 SQO, 2(1), 1999
various treatments of the samples. More exact expression
for the ∆R
i
can be obtained from the De-Marco and
Weiss formulae [8] which were successfully used for
experimental data interpretation [5].
Additionally, the spatial intensity distribution (SID)
of diffracted beams in a real space by single crystal
spectrometer and two-dimensional maps of the diffuse
intensity countors near the reciprocal lattice point were
obtained by a Philips high-resolution diffractometer. The
last method was used, however, for investigation of the
FzSi only. Both of these methods permitted us to judge
qualitatively the structural state of the samples.
3. Results and discussion
Let us start with discussion of the results obtained for
samples of the first series. In Fig. 1 the SID as a function
of the depth scattering, t, is presented. For the sample 3`
Number of the sample Type of
treatment
Ion dose
(cm-2)
Annealing parameters
(temperature, pressure,
duration)
1 implanted only 1016 -
2 implanted and annealed 1016 11300C,1 bar,10 h
+11300C,12 kbar,5 h
3 the same 1017 11300C,1 bar,5 h
4 the same 1017 11300C,12 kbar,5 h
5 the same 1016 11300C,6 kbar,5 h
6 the same 1016 11300C,1 bar,10 h
Table 1. The technological parameters of annealing the FZSi samples (second series).
Number of
the crystal
220 440 660 880
∆R i 107 L 220 ∆R i 107 L 440 ∆R i 107 L 660 ∆R i 107 L 880
1 2,5 - 3,3 - 7,3 0.018 2,7 0.03
2 18,0 0.002 23,0 0.01 11,0 0.028 5,3 0.07
3 8,4 0.001 3,6 0.002 6,5 0.016 1,7 0.02
1′ 121,0 0.01 48,0 0.02 20,0 0.05 4,2 0.05
2′ 68,0 0.006 32,0 0.015 15,0 0.04 2,7 0.035
3′ 156,0 0.013 67,0 0.032 23,7 0.06 4,4 0.056
Table 2. Integral perfection characteristics of the first series samples, i.e., increments of reflectivities ∆∆∆∆∆R
i
and Debye-Waller static
factors L for as grown (1), irradiated (2, 3) and annealed (1′′′′′, 2′′′′′,3′′′′′) crystals measured for 220, 440, 660, 880 Bragg reflections of
AgKααααα radiation.
Notes: The Czochralski grown Si samples: (1) � as grown, (2) � implanted with neon ions, and (3) � implanted with
oxygen ions respectively. Figures 1′, 2′, 3′ designate the same crystals annealed at 1050 °C for 5 h. The depthes of X-
ray penetrating in Si under the Bragg diffraction conditions (extinction length Λ) are equal to 50, 71, 120, 205 µm for
220, 440, 660 and 880 reflections of AgKα radiation, respectively.
L. I. Datsenko et al.: Structure perfection variations of Si crystals grown by ...
59SQO, 2(1), 1999
irradiated with the oxygen ions the noticeable broaden-
ing of the curve in comparison with those of the samples
1′ and 2′ is seen indicating more intensive X-ray diffuse
scattering on the SiO
x
precipitates formed during anneal-
ing just near the surface of the sample. One can see also
less intensive tails of diffuse scattering for the samples 1′
and 2′. It means that during annealing the SiO
x
precipi-
tates were formed not only on the radiation damages
created by the Ne ions, but also in the bulk of non-irra-
diated sample 1′.
The results of the reflectivity increment measurements
after irradiation of the CzSi samples and their successive
annealing are given in Table 2. An enhancement of the
R
i
is seen
for the irradiated samples (2, 3) due to creation
of distorted zones near the surface where the accelerated
ions stoped. The most noticeable distortions were creat-
ed in the case of the neutral neon atoms which did not
interact chemically with the silicon matrix. For both of
the samples 2 and 3 the largest ∆R
i
changes were re-
vealed for the Bragg reflections of low orders (220 and
440) for which the depths of diffraction maximum for-
mation (extinction length, Λ) are equal 50µm and 71 µm,
respectively. It may mean that the damaged zones af-
fecting the ∆R
i
changes were situated somewhere between
the surface and these depths.
More drastic changes of the ∆R
i
were discovered in
the samples 1′, 2′ and 3′ of the first series after their an-
nealing at 1050 °C for 5 hours, probably due to inten-
sive SiO
x
precipitates appearing. The largest R
i
incre-
ment, 156 ·10-7, characterises the sample 3′ irradiated
with oxygen. This result is in agreement with the the SID
for the the Bragg diffracted beam presented in Fig. 1
where the largest broadening of the curve 3′ is shown.
So, one can suppose that the oxygen ions created higher
local concentration of this impurity and, therefore, more
favourable conditions for oxygen solid solution decay
during annealing of the crystal as comparing with the
case of neon ions.
Let us consider now the results obtained after anneal-
ing of the FZSi samples, implanted by oxygen (series II).
At first we analyse peculiarities of the SID for the Bragg
diffracted beams in the samples 1 - 4, presented in Fig. 2.
The broadest curve corresponds to the sample 2 subject-
ed not only to implantation with oxygen ions but an-
nealings, too (see Table 1). Its large width is connected
perhaps with strong diffuse scattering on SiO
x
precipi-
tates appeared during high temperature annealings. The
other curves (e.g., 3 and 4), taken from the samples sub-
jected to various annealings (of not so long duration as
for the sample 2), are narrower. The peak value of the
relative intensity I / I
0
, is however, higher in the sample 2
than in as-implanted sample 1 due to contribution of
diffuse scattering on SiO
x
precipitates appearing in def-
fects of complex annealing near 1130 °C.
The maps of two-dimensional distribution of diffuse
scattering intensities near the 333 reciprocal point given
in Fig. 3, confirm in general, the above interpretation of
SID. Really, the as-implanted sample 1 of series II
Fig. 2. Spatial intensity distributions (SID) variations for the samples of second series implanted with oxygen and annealed
(symbols are given in Table 1). (1) sample implanted with oxygen only. I
0
is the intensity for incident beams.
0,000 0,002 0,004 0,006 0,008 0,010
0
1
2
3
4
3
2
1
t , cm
I
/
I 0
*
1
0
5 ,
a
rb
.u
n
it
s
L. I. Datsenko et al.: Structure perfection variations of Si crystals grown by ...
6 0 SQO, 2(1), 1999
Fig. 4. Integral reflectivity increments ∆R
i
versus the diffrac-
tion vector H ~ (h2 + k2 + l2)1/2 for the FZSi crystals after im-
plantation with oxygen and annealing. The numbers of sam-
ples correspond to those in Table 1.
(Fig. 3A) shows the existence of two reciprocal points
(one of them relates to the upper thin (~ 0,3 µm) layer
near the implanted surface). Subsequent annealing of
the FZSi samples 2, 3 resulted in disappearing the
discussed second point and in forming the broad pictures
of diffuse scattering on SiO
x
precipitates (Fig. 3C).
Now let us discuss the curves of the integral reflectiv-
ity increments ∆R
i
versus a diffraction vector H taken
for the 111, 333, 444, 555, and 777 Bragg reflections in
the samples 1 - 6 of the second series after various treat-
ments (Fig. 4.). Besides these curves, the dotted graph
for the extinction length Λ (the depth of diffracted beam
penetration) as a functoin of H is also given for relative
comparison with the depth of scattering. It can be seen
that the main changes in scattering process occured just
for the low orders (111 or 333) reflections. It means that
the process of oxygen solid solution decay takes place
just closely to the implanted layer where the local con-
centration C
0l
of oxygen could reach level of 1021 or 1022
at/cm3.
The sample 1 of the second series is characterised by
very high increment of reflectivity, ∆R
i
, for the 111 re-
flection (curve 1 in Fig. 4). The reason of such large chang-
es in R
i
in this sample consists mainly in elastic bending
a crystal [9] due to presence of the oxygen burried layer
near the implanted surface. Thus, for this sample, the
Debye-Waller factor, L, hardly could be calculated from
the formula (1). Annealing of the sample 2 (see Table 1)
resulted in more considerable increment of ∆R
i
than that
of the sample 1 due to appearence of SiO
x
precipitates
closely to implanted zone and in relaxation of elastic
strains. For this sample the volume part of SiO
x
precipi-
tates r
0
, being estimated from the value of ∆R
i
(r
0
≈ 2L = 0,036), is the largest among the other crystals
because this sample was annealed for 15 h in total at
1130 0C and additionally it was treated under high pres-
sure (P = 12 kbar).
Concerning an influence of high pressure on the ∆R
i
increments (Fig. 4), the results for the samples 3 and 4
Fig. 3. Maps of the diffuse scattering taken near 333 reciprocal
lattice point for CuKα1
radiation in the samples of the II series
subjected to implantation with oxygen ions of energy E ~
~ 200keV, dose 1016 - 1017 at/cm2 and followed annealing (see
table 1). The axes are marked in λ/2d units, where λ is wave-
length and d interplanar distance.
A � after implantation with O only (dose 1017 cm-2),
C � implanted with O, dose 1016 cm-2 and annealed at 11300C,
1 bar, 10 h + 1130 0C, 12 kbar, 5 h.
0 2 4 6 8 10 12
0
1
2
3
6
5
777555444333111
∆R
i=
(R
i -
R
ip
)
*
1
0
5
,
a
rb
.u
n
.
H =(h
2+k
2+ l
2)1/2 , arb.un.
0
100
200
300
400
500
600
3
4
2
1
Λ
σ , µ m
L. I. Datsenko et al.: Structure perfection variations of Si crystals grown by ...
61SQO, 2(1), 1999
should be compared. It is easy to see that ∆R
i
(4) > ∆R
i
(3)
because the first of them was annealed during the same
time (5 h) but under higher pressure (P = 12 kbar). So,
creation of SiO
x
precipitates has been more noticeably
manifested under an influence of hydrostatic pressure.
The same conclusion could be drawn from comparison
of the ∆R
i
for the samples 5 and 6 (∆R
i
(5) > ∆R
i
(6)),
though the time of treatment was longer for the sample
6. However, comparing the increments of R
i
for the sam-
ples 2 and 4 treated under pressure p = 12 kbar by the
same time (5 h) one can conclude that ∆R
i
(2) > ∆R
i
(4)
because the first of these samples was annealed addition-
ally for 10 h, though this preannealing was carried out
at ambient pressure (P = 1 bar).
4. Conclusion remarks
Structure perfection of the Czochralski grown silicon
crystals and of silicon crystals obtained by floating zone
method subjected to implantation of oxygen and neon
ions and then to annealing at the temperatures, where
intensive silicon-oxygen solid solution decay takes place,
was studied. Noticeable changes of the increments of in-
tegral reflectivities for the Bragg diffracted beams of the
hard X-ray radiation and considerable broadening of the
spatial intensity distribution curves as well as maps of
isointensive diffuse countors near a reciprocal lattice
point after the mentioned annealings of both types of
crystals in comparison with a perfect crystal were estab-
lished. Contrary to FZSi, where intensive diffuse scat-
tering caused by appearance of SiO
x
precipitates near
the oxygen-implanted layer was detected only, in the case
of CZSi those defects were formed not approximately to
the damaged layer but through the bulk. Preferential cre-
ation of SiO
x
precipitates was discovered, however, near
the zone of radiation damages caused by high energetic
ions of neon and oxygen, especially in the last case. One
can suppose that chemically active impurity introduced
in silicon matrix creates more favourable conditions for
following appearence of SiO
x
precipitates at high tem-
peratures.
It was shown that annealing of the implanted FZSi
crystals at enhanced hydrostatic pressure in argon at-
mosphere additionally stimulated the diffuse scattering
intensity due to formation of the mentioned precipitates
during process of oxygen solid solution decay close to
the implanted layer. Changes of character different dif-
fraction phenomena are better displayed after such treat-
ments. These changes manifest themselves more distinctly
under higher hydrostatic pressure.
References
1. A. Borghesi, B. Pivac, A. Sassella, A. Stella, Oxygen precipitates
in silicon // J.Appl.Phys.,77, pp.4169-4244 (1995).
2. V. M. Babich, N. I. Bletskan, E. F. Venger, Kislorod v monokri-
stallakh kremniya (in Russian) Kiev., Interpress LTD Publishing
company (1997).p. 239.
3. X.-T. Meng. Radiation-enhanced oxygen precipitates in neutron-
transmutation-doped floating zone silicon // Phys.Stat.Sol.(a).,
129(2), pp.K131-K136 (1992).
4. T. Hallberg, J. L. Lindstrom, Enhanced oxygen precipitates in
electron irradiated Si // J.Appl.Phys., 72(11). pp.5130-5138 (1992).
5. L. Datsenko, A. Misiuk, V. Machulin, V. Khrupa, Vliyaniye tem-
peratury, hydrostaticheskogo szhatia i drugich fisicheskikh fac-
torov na evolyutsiyu structur pri pretsipitatsii kisloroda v krem-
nii, Poverchnost // Rentgenovskie, neutronnie i synchrotronniye
issledovaniya, 10, pp.122-137 (1998).
6. D. ¯ymierska, D. Klinger, J. Auleytner, T. Czosnyka, L. Datsen-
ko. Studies of the near- surface layers of silicon crystals implant-
ed with fast ions // Nucl. Instr. and Meth., B 146. pp.350-355 (1998).
7. L. Datsenko, A. Misiuk, J. Härtwig, A. Briginetz, V. I. Khrupa,
Influence of preannealing on perfection of CzSi crystals subjected
to high pressure treatment // Acta Phys.Polonica, 86(4). pp.585-
590 (1994).
8. J. J. De Marco, R. J. Weiss, The integrated intensities of perfect
crystals, 19(1). pp.68-72 (1965).
9. L. I. Datsenko, V. B. Molodkin, M. E. Osinovski, Dynam-
icheskoye rasseyanie rentgenovskich luchey realnymi kristallami
(in Russian), Naukova dumka publishing company, Kyiv, (1988).
|