The influence of ethylene glycol on the chemical interaction of PbTe and Pb₁₋ₓSnₓTe crystals with H₂O₂–HBr–ethylene glycol etching compositions
The process of cutting, mechanical and chemical treatment of the PbTe and Pb₁₋ₓSnₓTe crystal surface has been studied. The dependences of the chemical-mechanical polishing rate versus dilution of the base polishing etchant H₂O₂–HBr–ethylene glycol by the ethylene glycol have been determined. The sur...
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| Опубліковано в: : | Semiconductor Physics Quantum Electronics & Optoelectronics |
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Інститут фізики напівпровідників імені В.Є. Лашкарьова НАН України
2017
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| Цитувати: | The influence of ethylene glycol on the chemical interaction of PbTe and Pb₁₋ₓSnₓTe crystals with H₂O₂–HBr–ethylene glycol etching compositions / G.P. Malanych, V.M. Tomashyk, O.S. Lytvyn // Semiconductor Physics Quantum Electronics & Optoelectronics. — 2017. — Т. 20, № 1. — С. 91-95. — Бібліогр.: 10 назв. — англ. |
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Digital Library of Periodicals of National Academy of Sciences of Ukraine| _version_ | 1860295840067747840 |
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| author | Malanych, G.P. Tomashyk, V.M. Lytvyn, O.S. |
| author_facet | Malanych, G.P. Tomashyk, V.M. Lytvyn, O.S. |
| citation_txt | The influence of ethylene glycol on the chemical interaction of PbTe and Pb₁₋ₓSnₓTe crystals with H₂O₂–HBr–ethylene glycol etching compositions / G.P. Malanych, V.M. Tomashyk, O.S. Lytvyn // Semiconductor Physics Quantum Electronics & Optoelectronics. — 2017. — Т. 20, № 1. — С. 91-95. — Бібліогр.: 10 назв. — англ. |
| collection | DSpace DC |
| container_title | Semiconductor Physics Quantum Electronics & Optoelectronics |
| description | The process of cutting, mechanical and chemical treatment of the PbTe and Pb₁₋ₓSnₓTe crystal surface has been studied. The dependences of the chemical-mechanical polishing rate versus dilution of the base polishing etchant H₂O₂–HBr–ethylene glycol by the ethylene glycol have been determined. The surface states after chemical etching have been investigated using electron, metallographic, and atomic force microscopy, as well as X-ray microanalysis. It has been shown that the surface state is improved after chemical etching. Efficient methods for washing the samples after different types of PbTe and Pb₁₋ₓSnₓTe surface treatment (cutting the crystal, mechanical surface treatment, and chemical removal of the surface-damaged layer) have been developed.
|
| first_indexed | 2026-03-21T07:43:30Z |
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Semiconductor Physics, Quantum Electronics & Optoelectronics, 2017. V. 20, N 1. P. 91-95.
doi: https://doi.org/10.15407/spqeo20.01.091
© 2017, V. Lashkaryov Institute of Semiconductor Physics, National Academy of Sciences of Ukraine
91
PACS 81.65.Ps
The influence of ethylene glycol on the chemical interaction
of PbTe and Pb1–xSnxTe crystals with H2O2–HBr–ethylene glycol
etching compositions
G.P. Malanych1, V.M. Tomashyk1, O.S. Lytvyn1,2
1V. Lashkaryov Institute of Semiconductor Physics, National Academy of Sciences of Ukraine,
41, prospect Nauky, 03028 Kyiv;
E-mail: galya_malanich@mail.ru
2Borys Grinchenko Kyiv University,
18/2, Bulvarno-Kudriavska str., 04053 Kyiv
Abstract. The process of cutting, mechanical and chemical treatment of the PbTe and
Pb1–xSnxTe crystal surface has been studied. The dependences of the chemical-
mechanical polishing rate versus dilution of the base polishing etchant H2O2–HBr–
ethylene glycol by the ethylene glycol have been determined. The surface states after
chemical etching have been investigated using electron, metallographic and atomic force
microscopy as well as X-ray microanalysis. It has been shown that the surface state is
improved after chemical etching. Efficient methods for washing the samples after
different types of PbTe and Pb1–xSnxTe surface treatment (cutting the crystal, mechanical
surface treatment, chemical removing the surface damaged layer) have been developed.
Keywords: chemical etching, lead telluride, solid solutions, dissolution rate, chemical
dynamic polishing.
Manuscript received 31.10.16; revised version received 18.01.17; accepted for
publication 01.03.17; published online 05.04.17.
1. Introduction
Single crystals of PbTe are used as material for
substrates when growing the PbTe/Pb1–xSnxTe
heterostructures that are key components in fabrication
of photodetectors and IR diode sources [1]. The quality
of detectors and substrates for epitaxy is directly related
to the quality of material itself (structural perfection and
purity of material) and processes used to produce them
(cutting ingots, polishing the crystal surface, and
metallic contact deposition). When fabricating detectors
and substrates, an important role is played by chemical
treatment of the crystal surface of PbTe and Pb1–xSnxTe
solid solutions. The main task of this chemical treatment
is elimination of the disturbed layer that is formed as a
result of previous mechanical processing as well as
acquisition of the high-clean surfaces maximally
structurally perfect and homogeneous in terms of their
chemical composition. These problems are successfully
solved using liquid-phase etching, in particular, applying
the method of chemical-mechanical polishing (CMP).
CMP process is realized as a result of the combined
effects of the chemical and mechanical factors and is
described approximately by the Preston equation [2, 3].
Semiconductor Physics, Quantum Electronics & Optoelectronics, 2017. V. 20, N 1. P. 91-95.
doi: https://doi.org/10.15407/spqeo20.01.091
© 2017, V. Lashkaryov Institute of Semiconductor Physics, National Academy of Sciences of Ukraine
92
In most cases, CMP is therefore employed with
polishing etchants. During this polishing, the reagents
oxidize or dissolve surface layers of the plates, and the
polishing member removes mechanically the interaction
products and microscopic particles of semiconductor.
The material removal, surface quality and geometrical
parameters of the plates to a considerable extent depend
on the polishing mixture composition, treatment
temperature, pressure on the plate and the material of the
polishing member. The etchant compositions for CMP
must correspond to a number of requirements: to have a
required etching rate without formation of insoluble or
poorly soluble reaction products; to be inert to the
material of the polishing member and equipment and to
be not too toxic [4].
Bromine solutions in organic and inorganic
solvents are most frequently used for the surface etching
of PbTe and Pb1–xSnxTe solid solutions. After
mechanical lapping of Pb1–xSnxTe (100) wafers, cut from
a Bridgman grown ingot, 2% Br2 solution in НBr were
used to remove residual lap damage before preferential
etching to develop defects and pits [5]. For polishing the
PbTe crystals, the solution of 5 vol.% Br2 + 95 vol.%
НBr was used, and etching was carried out for 1 min
followed by treatment with 30% KOH (t ≈ 40 °С) for
20 min and washing in bidistilled water [6].
Etching compositions based on elementary bromine
are characterized by high polishing rates. Some
problems appear with their preparation and composition
control, and their components are highly toxic.
Therefore, there is a necessity to search less toxic and
more technological etching compositions with low
dissolution rates of semiconductor surfaces. More
practical and promising are bromine-emerging etchant
compositions [7, 8], in which bromine is formed as a
result of the redox reaction of etchant components, for
example, Н2О2 and HBr.
This work is aimed to investigate CMP of PbTe
and Pb1–xSnxTe single crystal surfaces by bromine-
emerging etchant compositions based on aqueous
solutions of H2O2–HBr–solvent, to determine surface
quality after CMP using metallography, AFM and X-ray
microanalysis, and to optimize the polishing
compositions for formation of high quality surfaces of
the semiconductors mentioned above.
2. Experimental
In our experiments, the Bridgman-grown single crystals
of PbTe and Pb0.83Sn0.17Te and Pb0.8Sn0.2Te (II) solid
solutions as well as vapor-grown Pb0.8Sn0.2Te (I) single
crystals were used. The ingots were sliced into wafers
5×7×1.5 mm in dimensions by using a diamond wire
saw. The authors [9] have found that the depth of the
damaged layer for PbTe semiconductor monocrystalline
wafers is about 120 μm after diamond wheels cutting,
and it doesn’t depend on the nature of samples. It should
be noted that the damaged layer thickness is almost
independent from the surface crystallographic
orientation of the plates. The cutting-induced surface
deformation layer was partially removed by mechanical
grinding with aqueous suspensions of M10 to M5
abrasive powders. The polishing process was carried out
on a glass polisher, and working side plate was polished
for 2 min with an aqueous suspension of M10 abrasive,
and then – M5 abrasive. To remove the surface
contamination produced on the wafer surface at the
cutting and grinding stages, the wafers were rinsed in
warm distilled water containing surfactants, rinsed
several times with distilled water, and then dried in
flowing dry air. The damaged layer depth of
semiconductor wafers after polishing with abrasive
powder was amounted for M10 – 11…32 μm, and for
M5 – 7…26 μm [10]. The elimination rate of the surface
layer is different and depends on the nature of materials
and abrasive grit (Table).
The unprocessed side of the wafers prepared in
such manner was then glued with picein to silica
substrates. The residual picein was removed from the
surface of the specimens and substrates by rinsing with
organic solvents: acetone, toluene, and ethanol. Next, the
cutting- and grinding-induced surface deformed layer
was removed from the surface of all the crystals by CMP
[8] using a bromine-emerging H2O2–HBr–ethylene
glycol etchant at the dissolution rate ≈170 μm/min. The
CMP process was performed at Т = 293…295 K on a
glass wheel covered with cloth. The etchant was
constantly fed at the rate 2…3 mL/min.
Etchants were prepared using aqueous solutions of
48% HBr, 35% Н2О2, and ethylene glycol (EG). All the
chemicals were of extra pure or reagent grade. The
starting chemicals were mixed in appropriate volume
ratios (that is, the etchant composition was expressed as
a volume percent). All solutions were aged before the
etching and were allowed to stand for 120 min to
provide the reaction between the given etchant
components:
H2O2 + 2HBr = Br2+ 2H2O. (1)
After chemical etching, the wafers were rapidly
withdrawn from the etchant and at once rinsed to fully
remove the residual etchant and reaction products from
the surface. According to the proposed technique, the
rinsing process comprised several steps (30 s in each
solution), as represented by the following scheme:
Н2O (dist.) → 15% NaOH → Н2O (dist.)
→ HCl (conc.) → Н2O (dist.). (2)
After rinsing, the samples were dried in flowing
dry air.
The dissolution rate was determined via the
decrease in wafer thickness by using a 1 MIGP multiturn
timer with the accuracy of ±0.5 μm. Four samples were
dissolved simultaneously, and the deviation in thickness
measurements did not exceed 5%. The surface
microstructure of the PbTe samples and Pb1–xSnxTe solid
solutions after various abrasive and chemical treatment
Semiconductor Physics, Quantum Electronics & Optoelectronics, 2017. V. 20, N 1. P. 91-95.
doi: https://doi.org/10.15407/spqeo20.01.091
© 2017, V. Lashkaryov Institute of Semiconductor Physics, National Academy of Sciences of Ukraine
93
steps was studied using optical microscopy and electron
probe microanalysis. Surfaces were examined in white
light on the MIM-7 metallurgical microscope fitted with
an eTREK DCM800 digital video camera (8 Mpix) and
JEOL JCM-5000 NeoScope benchtop scanning electron
microscope. The quality of polished surfaces was
assessed by atomic force microscopy (AFM) by using
intermittent contact mode imaging with the NanoScope
IIIa Dimension 3000TM scanning probe microscope
(Digital Instruments, USA). The elemental composition
of the wafer surfaces was determined using scanning
electron microscopy being based on Zeiss EVO 50 XVP
equipped with an INCA450 energy dispersive X-ray
spectrometer system, which included an
INCAPentaFET×3 detector and HKL Channel-5
backscattered electron diffraction system (Oxford
Instruments).
3. Results and discussion
Correct selection of etchant compositions that are used at
the abrasive chemical treatment for CMP is an important
condition for obtaining high quality polished surfaces of
semiconductor materials. When using the base polishing
etchant to form polishing compositions for CMP, it was
taken into account that the rate of material removal at the
expense of mechanical component action should be
several times higher than that of chemical dynamic
polishing (CDP). It was shown that in the concentration
regions of the H2O2–HBr–EG system (in vol.%)
(2–10) H2O2:(48–98) HBr:(0–50) EG the polishing
compositions for CDP of the PbTe and Pb1–xSnxTe are
formed [7]. A base solution (B) with a composition in
the EG enriched region was therefore selected from the
investigated range. The rate of CDP of the PbTe and
Pb1–xSnxTe in this etchant is equal to ≈7 µm/min. But
when using CMP, the polishing rate increased and
reached 170 µm/min (Fig. 1). Some quantity of the
viscous component was added to the base solution B to
diminish the polishing rate and to improve the surface
properties. It is clear from Fig. 1 that the increase of
added EG quantity to etchant B leads to a decrease in
the CMP rate of the PbTe and Pb1–xSnxTe mono-
crystalline plate. Using the dependences from Fig. 1, it
is possible to select a required CMP rate within the
region from 20 to 170 µm/min by changing the ratio of
base etchant B to EG.
One of the advantages of the developed polishing
compositions except for the low polishing rates is their
pH that is equal to 6–7. It allows us to avoid interaction
of the etchants with the surface of the polishing member.
This factor has a great importance as in the majority of
cases the etchants can destroy the material of the
polishing member due their high acidity or alkalinity and
introduce additional impurities on the surfaces of
semiconductor plates. It should be noted that the
semiconductor surface after CMP in etchants containing
from 0 up to 60 vol.% of EG acquired high quality.
Further dilution of the stock solution (70 vol.% of EG)
deteriorated the surface quality: a white translucent film
appeared on the surface.
Using the methods of metallographic analysis and
electron microscopy, the sample surfaces were compared
after cutting, polishing and CMP to assess the impact of
etching processes on surface quality of semiconductor
crystals, in particular, on reducing the damaged layer.
The microstructure of the PbTe and Pb1–xSnxTe solid
solution surfaces after their treatment according to the
developed method is characterized by a high quality and
good mirror brightness.
Analysis of the obtained results shows that at the
same improvement of lead telluride surface there is a
clear difference between topography after mechanical
treatment (Figs. 2a and 2b), which reveals the surface
traces after string cutting, scratches from abrasive grains
and microcracks of surface even after its treatment with
polishing etchant (Fig. 2c) (different size of
microroughnesses and surface nature).
Table. The elimination rate of the PbTe and Pb1–xSnxTe
single crystal surfaces layer during mechanical treatment
with free abrasives.
The rate of surface layer
elimination, µm/min Semiconductor
М 10 М 5
PbTe ~ 60.0 ~ 13.5
Pb0.83Sn0.17Te ~ 80.0 ~ 20.0
Pb0.8Sn0.2Te (ІІ) ~ 95.0 ~ 24.0
Pb0.8Sn0.2Te (ІІ) ~ 68.5 ~ 21.0
0 10 20 30 40 50 60 70
0
50
100
150
200
0
50
100
150
200
4
3
2
1
III
B EGB : EG, vol.%
v,
µ
m
/m
in
Fig. 1. Dependences of the CMP rate of the PbTe (1),
Pb0.83Sn0.17Te (2), Pb0.8Sn0.2Te (I) (3) and Pb0.8Sn0.2Te (II) (4)
versus volume ratio of base etchant B (H2O2–HBr–EG) and
viscous organic component – ethylene glycol (I – polishing and
II – unpolishing solutions).
Semiconductor Physics, Quantum Electronics & Optoelectronics, 2017. V. 20, N 1. P. 91-95.
doi: https://doi.org/10.15407/spqeo20.01.091
© 2017, V. Lashkaryov Institute of Semiconductor Physics, National Academy of Sciences of Ukraine
94
The surface microstructure of the samples under
investigation was examined after each abrasive and
chemical treatment step (cutting, grinding, CMP) using
optical and electron microscopy techniques. AFM
characterization was only carried out for polished
surfaces with the best microstructure, that is, for the
surfaces treated with the most promising etchant
mixtures. Fig. 3 shows a three-dimensional AFM image
of the surface of the PbTe single crystal after CMP with
a bromine-emerging Н2О2–HBr–EG etchant. The AFM
data demonstrate that the average surface roughness Ra
of all our samples does not exceed 4 nm. CMP of the
surface of the PbTe and Pb1–xSnxTe crystals with the
proposed etchant mixtures produces a surface
microprofile with Rz = 5…11 nm. Thus, one can obtain
high-quality polished PbTe and Pb1–xSnxTe surfaces with
tailored parameters satisfying the requirements
(roughness value Rz ≤ 40 nm) for polished surfaces of
semiconductor materials [4].
Using X-ray microanalysis, we checked the
presence of oxygen and carbon, as well as possible
contamination with chemical compounds present in the
etchant and rinsing solutions. Oxygen was not detected
immediately after treatment with polishing etchants but
was found after prolonged storage of the samples (for
about two months) in air. The absence of Br, Cl, and Na
on the surface of the studied samples suggests that an
adequate rinsing procedure was used.
4. Conclusion
The CMP process of the PbTe, Pb0,83Sn0,17Te and
Pb0,8Sn0,2Te solid solutions surfaces with the H2O2–HBr–
EG bromine-emerging etchants has been investigated. It
has been shown that etchant compositions based on
aqueous solutions of the H2O2–HBr–solvent systems with
ethylene glycol as a solvent completely meet the
requirements for CMP etchants. The surface roughness of
the single crystals of PbTe and Pb1–xSnxTe solid solutions
after their treatment by using the CMP method including
the developed etchant compositions does not exceed
40 nm. The compositions of the polishing etchants for the
various surface treatments of the above semiconductor
materials were optimized.
a) b) c)
Fig. 2. Microstructure of PbTe surface (metallographic microscope МIМ-7 with digital video camcorder eTREK DCM800
(8 Mpix)): (a) after string cutting, (b) after abrasive polishing М5, (c) after chemical-mechanical polishing with Н2О2–НBr–ЕG
etchant.
a) b)
Fig. 3. (a) Three-dimensional AFM image of the PbTe surface after CMP with a H2O2–HBr–EG polishing solution, (b) surface
roughness profile.
Semiconductor Physics, Quantum Electronics & Optoelectronics, 2017. V. 20, N 1. P. 91-95.
doi: https://doi.org/10.15407/spqeo20.01.091
© 2017, V. Lashkaryov Institute of Semiconductor Physics, National Academy of Sciences of Ukraine
95
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|
| id | nasplib_isofts_kiev_ua-123456789-214906 |
| institution | Digital Library of Periodicals of National Academy of Sciences of Ukraine |
| issn | 1560-8034 |
| language | English |
| last_indexed | 2026-03-21T07:43:30Z |
| publishDate | 2017 |
| publisher | Інститут фізики напівпровідників імені В.Є. Лашкарьова НАН України |
| record_format | dspace |
| spelling | Malanych, G.P. Tomashyk, V.M. Lytvyn, O.S. 2026-03-03T11:04:48Z 2017 The influence of ethylene glycol on the chemical interaction of PbTe and Pb₁₋ₓSnₓTe crystals with H₂O₂–HBr–ethylene glycol etching compositions / G.P. Malanych, V.M. Tomashyk, O.S. Lytvyn // Semiconductor Physics Quantum Electronics & Optoelectronics. — 2017. — Т. 20, № 1. — С. 91-95. — Бібліогр.: 10 назв. — англ. 1560-8034 PACS: 81.65.Ps https://nasplib.isofts.kiev.ua/handle/123456789/214906 https://doi.org/10.15407/spqeo20.01.091 The process of cutting, mechanical and chemical treatment of the PbTe and Pb₁₋ₓSnₓTe crystal surface has been studied. The dependences of the chemical-mechanical polishing rate versus dilution of the base polishing etchant H₂O₂–HBr–ethylene glycol by the ethylene glycol have been determined. The surface states after chemical etching have been investigated using electron, metallographic, and atomic force microscopy, as well as X-ray microanalysis. It has been shown that the surface state is improved after chemical etching. Efficient methods for washing the samples after different types of PbTe and Pb₁₋ₓSnₓTe surface treatment (cutting the crystal, mechanical surface treatment, and chemical removal of the surface-damaged layer) have been developed. en Інститут фізики напівпровідників імені В.Є. Лашкарьова НАН України Semiconductor Physics Quantum Electronics & Optoelectronics The influence of ethylene glycol on the chemical interaction of PbTe and Pb₁₋ₓSnₓTe crystals with H₂O₂–HBr–ethylene glycol etching compositions Article published earlier |
| spellingShingle | The influence of ethylene glycol on the chemical interaction of PbTe and Pb₁₋ₓSnₓTe crystals with H₂O₂–HBr–ethylene glycol etching compositions Malanych, G.P. Tomashyk, V.M. Lytvyn, O.S. |
| title | The influence of ethylene glycol on the chemical interaction of PbTe and Pb₁₋ₓSnₓTe crystals with H₂O₂–HBr–ethylene glycol etching compositions |
| title_full | The influence of ethylene glycol on the chemical interaction of PbTe and Pb₁₋ₓSnₓTe crystals with H₂O₂–HBr–ethylene glycol etching compositions |
| title_fullStr | The influence of ethylene glycol on the chemical interaction of PbTe and Pb₁₋ₓSnₓTe crystals with H₂O₂–HBr–ethylene glycol etching compositions |
| title_full_unstemmed | The influence of ethylene glycol on the chemical interaction of PbTe and Pb₁₋ₓSnₓTe crystals with H₂O₂–HBr–ethylene glycol etching compositions |
| title_short | The influence of ethylene glycol on the chemical interaction of PbTe and Pb₁₋ₓSnₓTe crystals with H₂O₂–HBr–ethylene glycol etching compositions |
| title_sort | influence of ethylene glycol on the chemical interaction of pbte and pb₁₋ₓsnₓte crystals with h₂o₂–hbr–ethylene glycol etching compositions |
| url | https://nasplib.isofts.kiev.ua/handle/123456789/214906 |
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