Crystals Cd₁₋x ZnxTe – a promising material for non-cryogenic semiconductor detectors: preparations, structure defectness and electrophysical properties
Relationship between preparation conditions of the raw charge, crucible material, growth regimes and structure defectness and electrophysical properties of crystals Cd₁₋x ZnxTe has been studied. The crystals were grown both from the raw material which had been pre-synthesized in quartz ampoules and...
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Інститут фізики напівпровідників імені В.Є. Лашкарьова НАН України
1999
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| Цитувати: | Crystals Cd₁₋x ZnxTe – a promising material for non-cryogenic semiconductor detectors: preparations, structure defectness and electrophysical properties / L.V. Atroshchenko, S.N. Galkin, L.P. Gal’chinetskii, A.I. Lalayants, I.A. Rybalka, V.D. Ryzhikov, V.I. Silin, N.G. Starzhinskii // Semiconductor Physics Quantum Electronics & Optoelectronics. — 1999. — Т. 2, № 4. — С. 81-85. — Бібліогр.: 5 назв. — англ. |
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irk-123456789-1202592017-06-12T03:04:34Z Crystals Cd₁₋x ZnxTe – a promising material for non-cryogenic semiconductor detectors: preparations, structure defectness and electrophysical properties Atroshchenko, L.V. Galkin, S.N. Galchinetskii, L.P. Lalayants, A.I. Rybalka, I.A. Ryzhikov, V.D. Silin, V.I. Starzhinskii, N.G. Relationship between preparation conditions of the raw charge, crucible material, growth regimes and structure defectness and electrophysical properties of crystals Cd₁₋x ZnxTe has been studied. The crystals were grown both from the raw material which had been pre-synthesized in quartz ampoules and from the raw material synthesized from the elements directly in the growth furnace. It is shown that the best values of electric resistivity ρ (up to 10¹¹ Ohm⋅cm) and sensitivity to X-ray and gamma-radiation are obtained for crystals grown in crucibles of highly pure coal-graphite material from the pre-synthesized raw charge. Correlation has been established between values of ρ and crystal defectness: decrease of dislocation density by 10⁴ times led to 10⁷ times higher values of resistivity. Concentration of dislocation etching pits regularly decreased with higher purity of the raw material and optimization of crystal preparation technology. 1999 Article Crystals Cd₁₋x ZnxTe – a promising material for non-cryogenic semiconductor detectors: preparations, structure defectness and electrophysical properties / L.V. Atroshchenko, S.N. Galkin, L.P. Gal’chinetskii, A.I. Lalayants, I.A. Rybalka, V.D. Ryzhikov, V.I. Silin, N.G. Starzhinskii // Semiconductor Physics Quantum Electronics & Optoelectronics. — 1999. — Т. 2, № 4. — С. 81-85. — Бібліогр.: 5 назв. — англ. 1560-8034 PACS: 72.20, 78.30.A, F, 81.05.C, D, E, G, H http://dspace.nbuv.gov.ua/handle/123456789/120259 en Semiconductor Physics Quantum Electronics & Optoelectronics Інститут фізики напівпровідників імені В.Є. Лашкарьова НАН України |
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Relationship between preparation conditions of the raw charge, crucible material, growth regimes and structure defectness and electrophysical properties of crystals Cd₁₋x ZnxTe has been studied. The crystals were grown both from the raw material which had been pre-synthesized in quartz ampoules and from the raw material synthesized from the elements directly in the growth furnace. It is shown that the best values of electric resistivity ρ (up to 10¹¹ Ohm⋅cm) and sensitivity to X-ray and gamma-radiation are obtained for crystals grown in crucibles of highly pure coal-graphite material from the pre-synthesized raw charge. Correlation has been established between values of ρ and crystal defectness: decrease of dislocation density by 10⁴ times led to 10⁷ times higher values of resistivity.
Concentration of dislocation etching pits regularly decreased with higher purity of the raw material and optimization of crystal preparation technology. |
| format |
Article |
| author |
Atroshchenko, L.V. Galkin, S.N. Galchinetskii, L.P. Lalayants, A.I. Rybalka, I.A. Ryzhikov, V.D. Silin, V.I. Starzhinskii, N.G. |
| spellingShingle |
Atroshchenko, L.V. Galkin, S.N. Galchinetskii, L.P. Lalayants, A.I. Rybalka, I.A. Ryzhikov, V.D. Silin, V.I. Starzhinskii, N.G. Crystals Cd₁₋x ZnxTe – a promising material for non-cryogenic semiconductor detectors: preparations, structure defectness and electrophysical properties Semiconductor Physics Quantum Electronics & Optoelectronics |
| author_facet |
Atroshchenko, L.V. Galkin, S.N. Galchinetskii, L.P. Lalayants, A.I. Rybalka, I.A. Ryzhikov, V.D. Silin, V.I. Starzhinskii, N.G. |
| author_sort |
Atroshchenko, L.V. |
| title |
Crystals Cd₁₋x ZnxTe – a promising material for non-cryogenic semiconductor detectors: preparations, structure defectness and electrophysical properties |
| title_short |
Crystals Cd₁₋x ZnxTe – a promising material for non-cryogenic semiconductor detectors: preparations, structure defectness and electrophysical properties |
| title_full |
Crystals Cd₁₋x ZnxTe – a promising material for non-cryogenic semiconductor detectors: preparations, structure defectness and electrophysical properties |
| title_fullStr |
Crystals Cd₁₋x ZnxTe – a promising material for non-cryogenic semiconductor detectors: preparations, structure defectness and electrophysical properties |
| title_full_unstemmed |
Crystals Cd₁₋x ZnxTe – a promising material for non-cryogenic semiconductor detectors: preparations, structure defectness and electrophysical properties |
| title_sort |
crystals cd₁₋x znxte – a promising material for non-cryogenic semiconductor detectors: preparations, structure defectness and electrophysical properties |
| publisher |
Інститут фізики напівпровідників імені В.Є. Лашкарьова НАН України |
| publishDate |
1999 |
| url |
http://dspace.nbuv.gov.ua/handle/123456789/120259 |
| citation_txt |
Crystals Cd₁₋x ZnxTe – a promising material for non-cryogenic semiconductor detectors: preparations, structure defectness and electrophysical properties / L.V. Atroshchenko, S.N. Galkin, L.P. Gal’chinetskii, A.I. Lalayants, I.A. Rybalka, V.D. Ryzhikov, V.I. Silin, N.G. Starzhinskii // Semiconductor Physics Quantum Electronics & Optoelectronics. — 1999. — Т. 2, № 4. — С. 81-85. — Бібліогр.: 5 назв. — англ. |
| series |
Semiconductor Physics Quantum Electronics & Optoelectronics |
| work_keys_str_mv |
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81© 1999, Institute of Semiconductor Physics, National Academy of Sciences of Ukraine
Semiconductor Physics, Quantum Electronics & Optoelectronics. 1999. V. 2, N 4. P. 81-85.
1. Introduction
Among semiconductor materials with wide band gap, much
attention has been paid to CdTe and Cd1-xZnxTe as room-
temperature detectors of X-ray and gamma-radiation. They
have high atomic number (~ 50), high density (> 6 g/cm3)
and relatively high carrier mobility. It has been shown that
formation of solid solutions CdTe-ZnTe is accompanied by
broadening of the band gap, increase of resistivity (by more
than an order of magnitude), and improved stability of spectral
characteristics as compared with CdTe [1]. A general problem
for semiconductor materials based on AIIBVI compounds is
the difficulty of growing structurally perfect crystals charac-
terized by high degree of chemical purity and stoichiometry.
Requirements to the structural perfectness of crystals
Cd1-xZnxTe are very high, because practically all their princi-
pal electrophysical and optical characteristics are strongly
structure-dependent.
The present work was focussed on studying effects of
preparation conditions of crystals Cd1-xZnxTe upon concen-
tration of electrically active structural defects in this material
and X-ray sensitivity of detectors made on its base.
2. Experimental procedure
We studied a set of crystals Cd1-xZnxTe (32 mm in diameter)
grown by Bridgman method in vertical compression furnaces
under inert gas (argon) pressure from 3.5 to 5.5 MPa. Crystal
growth regimes are presented in Table 1.
In this work, crystals Cd1-xZnxTe were grown using raw
materials pre-synthesized in a quartz ampoule, as well as
those synthesized from elements (Cd,Zn,Te) directly in the
growth equipment.
During growth of certain crystals (No. 9-12) gas samples
were taken to analyze concentration of oxygen-containing
impurities in the atmosphere of the growth furnace. Carbon
oxide content at different growth stages varied from 0.1 to 3
vol. %. Concentration of oxygen and water vapor in the
initial argon did not exceed 1⋅10-3 vol. %. It could be con-
cluded that in the growth furnace carbon oxide was formed
from the air desorbed from the construction material, and its
removal was necessary.
Quality and uniformity of the properties and structure of
the grown crystals was determined by several independent
PACS: 72.20, 78.30.A, F, 81.05.C, D, E, G, H
Crystals Cd1-xZnxTe – a promising material for
non-cryogenic semiconductor detectors: preparations,
structure defectness and electrophysical properties
L.V. Atroshchenko, S.N. Galkin, L.P. Gal’chinetskii, A.I. Lalayants, I.A. Rybalka, V.D. Ryzhikov,
V.I. Silin, N.G. Starzhinskii
STC for Radiation Instruments, Concern «Institute for Single Crystals», NAS of Ukraine,
60 Lenin Ave.,310001 Kharkov, Ukraine.
Tel. (0572) 321379 fax (0572) 32130, E-mail:root@stcri.kharkov.ua
Abstract. Relationship between preparation conditions of the raw charge, crucible material, growth
regimes and structure defectness and electrophysical properties of crystals Cd1-xZnxTe has been studied.
The crystals were grown both from the raw material which had been pre-synthesized in quartz ampoules
and from the raw material synthesized from the elements directly in the growth furnace. It is shown that
the best values of electric resistivity ρ (up to 1011 Ohm⋅cm) and sensitivity to X-ray and gamma-
radiation are obtained for crystals grown in crucibles of highly pure coal-graphite material from the pre-
synthesized raw charge. Correlation has been established between values of ρ and crystal defectness:
decrease of dislocation density by 104 times led to 107 times higher values of resistivity.
Concentration of dislocation etching pits regularly decreased with higher purity of the raw material and
optimization of crystal preparation technology.
Keywords: preparation conditions, structure defectness, electric resistivity, dislocation density, semi-
conductor detectors.
Paper received 19.10.99; revised manuscript received 15.12.99; accepted for publication 17.12.99.
L.V. Atroshchenko et al.: Crystals Cd1-xZnxTe – a promising material for...
82 SQO, 2(4), 1999
methods: selective chemical etching on dislocations, IR
microscopy, IR spectroscopy, measurements of resistivity
and gamma-sensitivity. The etching agent used for detec-
tion of dislocations in crystals Cd1-xZnxTe was the same as
that commonly used for CdTe crystals and had the following
composition [2]: 10 ml (10 ml of conc. HNO3 + 20 ml H2O +
4g K2Cr2O7) + 10 mg AgNO3.
Studies of crystals in IR spectral region (0.75-1.2 µm)
were carried out in transmitted light using a MIK-4 micro-
scope (amplifications from 44x to 1200x). Measurements of
resistivity ρ were carried out using samples of 5×5×2 mm3
after chemical etching and application of contacts on the
5x5 mm2 area. Gamma- and X-ray sensitivity of detectors
based on crystals Cd1-xZnxTe were studied using radionuc-
lides Cs-137 and Am-241, as well as X-ray sources
IRI and RAPAN-200 (U = 20-200 kV, I ≤ 5 µA). Elemental
analysis of the raw material and crystals grown from it was
carried out using a VRA-30 X-ray fluorescent spectrometer
with accuracy of ± 0.4 at.%.
3. Results and discussion
To obtain structurally perfect crystals by Bridgman method,
one should minimize negative effects of the atmosphere in
the growth furnace, crucible material, variations of the el-
emental composition due to thermal dissociation, as well as
of possible contamination of the crystal by construction
materials.
Accounting for peculiar features of the AIIBVI crystal
growth by this method, the crucible material should meet
the following requirements:
- thermal stability up to 1500 K;
- non-wettability by the Cd1-xZnxTe melt;
- chemical inertness with respect to Cd1-xZnxTe and the
initial elemental components;
- thermal expansion coefficient of the crucible material
should be lower than that of the crystal;
- low gas penetrability;
- high mechanical strength.
Table 1. Conditions and results of experiments of Cd1-xZnxTe crystal growth
Experi- Raw charge Material of crucible Growth rate, Melt eva- R,Ohm⋅cm
ment № mm/hour poration, %
1 3N Graphite 5 7.5 -
2 - // - - // - 3 9 -
3 - // - - // - 3 9 -
4 - // - - // - 2.8 4.5 -
5 - // - Pyrographite, thermal
expansion coefficient 2.8 - -
< 5⋅10-6 К-1
6 Cd+Zn+Te - // - 1.54 0.7 103
Qualification 6N,
synthesis in autoclave
7 - // - - // - 1.54 0.9 103
8 - // - - // - 1.35 1 104
9 - // - - // - 1.35 1 104
10 Cd0.8Zn0.2Te - // - 2.6 1 105
Qualification 6N,
synthesis in quartz
ampoule
11 - // - - // - 3 1.9 109
12 - // - - // - 2.6 0.7 1010
13 Cuts of 1-5 crystals - // - 2.6 3.5 1010
14 Cd0.8Zn0.2Te - // - 2.6 - 5⋅1010
Qualification 6N,
synthesis in quartz
ampoule
L.V. Atroshchenko et al.: Crystals Cd1-xZnxTe – a promising material for...
83SQO, 2(4), 1999
At present, boron nitride is often considered as a prom-
ising material in this respect [3]; however, the use of this
material is limited by its high cost.
To work out the main technological regimes, we carried
out a set of crystal growth experiments in graphite crucibles
25 mm in diameter (No. 1-5, Table 1).
For growth of crystals No. 6-14 32 mm in diameter (Table 1)
we used crucibles of highly pure coal-graphite material with
thermal expansion coefficient not more than 5.7⋅10-6 K-1.
The use of such material allowed to decrease the carry-over
of the raw charge due to melt evaporation from 9% to 0.7%
as compared with the graphite crucibles. It was also possi-
ble to avoid crystal deformation during cooling, and the
crystal could be easily removed from the crucible.
To study the effects of the raw charge composition upon
composition and electrophysical properties of crystals
Cd1-xZnxTe, three kinds of raw materials for charge were
used.
At the first stage of working out of the growth regimes
(crystals No. 1-5) raw material of 3N qualification was used.
In this crystals, we analyzed only the melt evaporation and
the degree of structural perfection, which was not high.
At the second stage (crystals No. 6-9) elementary Cd,
Zn, Te of 6N qualification were used as raw charge after
appropriate purification. It was established that, during syn-
thesis of the charge from elements directly in the growth
furnace, there was chemical interaction with the crucible
and other construction parts made of carbon, yielding CTe,
CTe2, CdC, ZnC and similar compounds. These caused con-
tamination of the melt by reaction products and to the pres-
ence of carbon-containing inclusions in the crystal struc-
ture, as well as to high concentration of growth disloca-
tions, low optical uniformity and decreased values of ρ
(Table 1).
Typical microstructure of crystals grown from the raw
charge synthesized from the elements directly in the growth
furnace is shown in Fig. 1a. On the cross-section normal to
the growth direction (orientation is arbitrary) there are non-
uniformly distributed dark etching figures in the shape of
isoscales triangle or trapezium. This is in full agreement with
the scheme of theoretically constructed configuration of
dislocation etching pits in crystals CdTe [2]. Purity of the
material (nature and amount of admixtures) has a decisive
influence upon formation of etching figures, i.e., the proc-
ess of selective etching of the surfaces of the studied crys-
tals is related to segregation of admixtures or the Cottrell
atmosphere on dislocations. The obtained etching figures
appear to be growth dislocations decorated with admixtures.
In areas of their highest concentration, density of etching
figures reached ~ 4⋅105 cm-2. We also observed small inclu-
sions of spherical shape, concentration of which reached
~ 5⋅106 cm-2; their nature remained unclear.
By means of IR microscopy, in such crystals Cd1-xZnxTe
inclusions of elongated shape were detected, which were
orientated along the growth direction. Their size could reach
0.8-1 mm.
We have determined that the best values of resistivity
(up to 1011 Ohm⋅cm) and sensitivity to X-ray and gamma-
radiation are obtained in crystals grown from the raw charge
which had been pre-synthesized in quartz ampoules. Typical
microstructure of crystals grown from the raw charge which
had been pre-synthesized in quartz ampoules is shown in
Fig. 1b. Large ρ values allow to increase the electric field and
to decrease charge collection time, or to decrease the leak-
age current and the accompanying noise.
Fig. 2 shows the output signal of the Cd1-xZnxTe based
detectors as a function of the dose rate of X-ray radia-
tion (E ~ 100 keV) and the bias voltage Ub (curves 1-3). It
was found that X-ray sensitivity of detectors of this type are
proportional to ρ and Ub , and at Ub = 200 V X-ray sensi-
tivity is by an order of magnitude higher as compared with
scintielectronic detectors based on ZnSe(Te) that is one of
the best scintillators (curve 4). These data show that detec-
tors based on Cd1-xZnxTe are very promising for their cur-
rent mode applications in introscopic and dosimetric sys-
tems of high sensitivity.
Average growth dislocation density in these crystals did
Fig. 1a. Cross-section microstructure for a crystal grown from the
raw materials synthesized from the elements directly in the growth
furnace.
Fig. 1b. Cross-section microstructure for a crystal grown from the raw
charge which had been pre-synthesized in quartz ampoules.
100 µµµµµm
L.V. Atroshchenko et al.: Crystals Cd1-xZnxTe – a promising material for...
84 SQO, 2(4), 1999
not exceed 2⋅10-2 cm-2, and inclusions of extra phases were
not observed. A correlation was found between values of ρ
and defectness of the crystals. When growth dislocation
density decreased by 104 times, ρ became 107 times higher.
Dislocations in all studied crystals detected by selective
chemical etching were decorated, which suggested that these
were due to the presence of admixtures. Concentration of
dislocation etching pits regularly decreased with higher
purity of the raw material and optimization of the growth
technology.
The composition of crystals was uniform up to 0.4-0.5
from the ingot «nose». Zn content in the «nose» part of the
ingot was 5-12% higher than in the initial mixture of the
components. Similar deviations of composition of crystals
Cd1-xZnxTe were observed in [4,5].
Besides, X-ray fluorescent analysis data (Table 2 and
Fig. 3) show that only composition from the «nose» part of
the ingots belongs to the quasibinary section CdTe – ZnTe
of the ternary diagram of state.
IR transmission spectra of some of the studied crystals
are presented in Fig. 3. It is shown that for crystals of high
electric conductivity absorption by the free carriers can be
observed, which is characterized by a featureless spectrum
described by the λ p law (1.5 < p < 3.5). For crystals of low
electrical conductivity absorption on the free carriers is not
observed. Absorption in the 2000- 3800 cm-1 region can ap-
parently be ascribed to the valence vibrations of hydroxyl
groups as well as to CO– groups. For crystals grown
from the raw material that had been pre-synthesized in
quartz ampoules, optical transmittance in the 500-1500
cm-1 region was not less than 66%.
Our studies have shown that, for 60 keV gamma-radia-
tion (Am-241), the signal-to-noise ratio in these crystals was
1/3-1/4 at the bias voltage of 200 V. The lifetime of carriers
multiplied by their mobility (a value that determines, along-
side with the resistivity, the ability of the detector material to
maintain and to enable the detection of ionizing charges)
was not less than 8⋅10-5 cm2/V.
Fig. 2. Output signal, A, as function of dose rate, P, of X-ray radiation
for detectors based on Cd1-xZnxTe (1-3) and a scintielectronic detec-
tor of «scintillator-photodiode» type (4).
No. 13
No. 14
Te
Cd
Zn
50 40
50
60
n
n
t
t
Fig. 3. Composition of the grown crystals Сd1-xZnxTe (No. 13 and
No. 14) on the ternary diagram of state Zn-Cd-Te.
Fig. 4. IR transmission spectra of crystals Cd1-xZnxTe.
0 50 100 150 200 250 300
0
0.5
1.0
1.5
2.0
2.5
3.0
3.5
4.0
4.5
5.0
5.5
6.0
(1)
U =50
V
(2)
U =100
V
(3)
U =200
V
(4)
PD+ZnSe(Te)
P, R/h
A
,
a.
u.
Table 2. Results of chemical analysis of content of the main
components in crystals Cd1-xZnxTe over the ingot length.
N Number Content of element,at. %
of crystal Cd Zn Te
1. 13 (nose) 46.97 2.99 50.04
2. 13 (2) 46.32 3.00 50.68
3. 13 (3) 46.58 2.92 50.50
4. 13 (tail) 40.80 2.81 56.39
5. 14 (nose) 40.74 8.98 50.28
6. 14 (2) 38.52 8.74 52.74
7. 14 (tail) 41.92 5.64 52.44
70 70
60 60
50 50
40 40
30 30
20 20
10 10
0 0
11
7
14
6
4000 3000 2000 1000
Wave number, cm
Tr
an
sm
is
si
on
, %
-1
L.V. Atroshchenko et al.: Crystals Cd1-xZnxTe – a promising material for...
85SQO, 2(4), 1999
Conclusions
Results of our studies show that the use of Bridgman method
under pressure is a promising way to obtain crystals Cd1-
xZnxTe with high values of electrophysical parameters and
high sensitivity to ionizing radiation, even for crystals of
small diameter. Synthesis of raw charge in this case should
be carried out in quartz ampoules under vacuum.
Acknowledgments
The authors are grateful to Dr.V. Kutniy and Dr.A. Rybka for
their having taken part in discussion of the results of this
work.
This work was carried out with financial support of the
Lawrence Livermore National Laboratory.
References
1. F.P. Doty, J.E. Butler et al.Properties of CdZnTe crystals grown
by a high pressure Bridgman method// J. Vac. Sci. Technol. 10.
N4, pp.358-363, 1992.
2. M. Jnoue, J. Teramoto, S. Takayanagi. Etch pits and polarity in
CdTe crystals// J. Appl. Phys. 33. N8, pp.2578-2582, 1962.
3. H.F. Glass, A.J. Socha, C.L. Parfeniuk, D.W. Baccen. Improve-
ments in production of CdZnTe crystals grown by the Bridgman
method // J. Crystal Growth. 184/185, p.1035, 1998.
4. Atsuko Ebina, Kasuyuki Saito, Tadashi Tacahashi. Crystals grown
of ZnCd1-x Te solid solution and their optical properties at the
photon energies of the lowest band-gap region// J. Appl. Phys. 44.
N 8(2), pp.3659-3662, 1973.
5. J. Karniewich, T. Majchrak. The directional solidification of
ZnxСd1-xTe from tellurium solvent// In book: 6 Int. Conf. for
Crystal Growth, Moscow, B 3, p.311, 1980.
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