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archives of civil and mechanical engineering 14 (2014) 425–432

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Original Research Article

Characteristics of surface layer of sintered stainless


steels after remelting using GTAW method

A. Wrońska *, A. Dudek
Czestochowa University of Technology, Institute of Materials Engineering, Al. Armii Krajowej 19,
42-200 Czestochowa, Poland

article info abstract

Article history: The study presents the results of the investigations concerning the effect of remelting using
Received 21 May 2013 gas tungsten arc welding (GTAW) process on the microstructure and selected properties of
Accepted 29 October 2013 the surface layer in sintered multi-phase steels obtained from powders of 304L and 434L
Available online 2 December 2013 steels. The effect of surface treatment was evaluated based on macro- and microstructural
observations, EDS analysis, X-ray phase analysis and measurements of surface roughness
Keywords: and microhardness. It was found that remelting of surface layer leads to elimination of open
Sintered stainless steel porosity and homogenization of the structure, which was confirmed by microscopic obser-
Surface remelting vations and microhardness tests. A cellular or mixed cellular and dendritic structure was
GTAW method formed in the remelted zone in the sinters. Growth of columnar crystals occurred along the
direction of heat transfer. Using the energy dispersive spectroscopy (EDS), the authors found
higher concentration of alloy elements in the intercellular zones compared to cell cores. X-
ray analysis demonstrated that the remelting used is conducive to formation of the
austenitic phase in the remelted material.
# 2013 Politechnika Wrocławska. Published by Elsevier Urban & Partner Sp. z o.o. All
rights reserved.

manufacturing of small products with complex shapes while


1. Introduction
maintaining high accuracy of the products. Moreover, powder
metallurgy is nearly a waste-free technology, which is highly
Stainless steels are a group of materials with particular desirable due to the depleted resources of raw materials and
properties. They are characterized by resistance to oxidation rising prices [2,3]. Regarding stainless steels, powder metallurgy
and corrosion and they also exhibit good mechanical properties allows for control over chemical composition and microstruc-
[1]. Recent years have seen increased application of stainless ture. This causes that, apart from the basic grades of ferritic and
steel manufactured using powder metallurgy technologies. austenitic steels, it is possible to easily obtain products with the
Although the prices of powders of stainless steels are higher microstructure typical of duplex stainless steel or products with
than the prices of semi-products made of conventionally a multi-phase structure [4,5].
manufactured steels, production of components from powders The basic criterion which should be met by sintered
is more economical. This results chiefly from easier automation stainless steels is resistance to chemical agents, whereas
and energy-efficiency of the process and opportunities of mechanical properties are treated as a secondary problem [2].

* Corresponding author. Tel.: +48 343250627; fax: +48 3250721.


E-mail addresses: agataw@wip.pcz.pl, agata.21@onet.eu (A. Wrońska), dudek@wip.pcz.pl (A. Dudek).
1644-9665/$ – see front matter # 2013 Politechnika Wrocławska. Published by Elsevier Urban & Partner Sp. z o.o. All rights reserved.
http://dx.doi.org/10.1016/j.acme.2013.10.011
426 archives of civil and mechanical engineering 14 (2014) 425–432

Therefore, striving for obtaining a surface layer with the best standard). The average diameters of 304L and 434L steel
possible properties should be a top priority. The main factor powder grains were 10.87 mm and 14.89 mm, respectively. The
that contributes to corrosion in these steels is open porosity three different mixtures of the powders were prepared, with
[5,6]. Pores that are generated on the surface of sinters the following composition: 80% 304L:20% 434L (sinter A), 50%
enlarged the surface which is exposed to the effect of 304L:50% 434L (sinter B), 20% 304L:80% 434L (sinter C), which
aggressive environments. Moreover, if pores are connected was subjected to uniaxial compaction at 720 MPa. The
with each other by means of channels, there is a substantial moulded pieces were sintered at the temperature of 1250 8C
risk of edge corrosion caused by formation of local concentra- for 30 min in the dissociated ammonia medium and cooled
tion cells [7,8]. Consequently, steel ability to form a passive down with cooling rate of 0.5 8C/s. Chemical composition of
layer is reduced. An additional factor that reduces anti- the powders used and the obtained sinters were given in
corrosion properties in multi-phase steels is non-homogeneity Table 1.
of the microstructure. Open porosity was determined on the unetched metallo-
Sintered corrosion-resistant steels are currently used in graphic cross-sections using Axiovert 25 optical microscope
various areas of the industry. However, their main customer is and ImageJ computer software for image analysis. Five images
the automotive sector. Sintered ferritic-austenitic steels are were analyzed for each sample. Porosity of the sinters A, B and
used to manufacture the car parts such as components of C was, respectively: 5.11  0.77%; 14.71  1.34%; 3.06  0.7%.
exhaust system and branched pipes, holders of mirrors, parts The microstructure of duplex stainless steels after sintering
of windscreen wipers, etc. [2,9]. Considering economic factors, in the conditions adopted in the study was more complex and
one profitable method of processing that ensures improved quite different than the microstructure of conventionally
properties of surface layer in corrosion-resistant sintered steel manufactured duplex steels. The main factors which may
is remelting with focused heat sources. The most of previous impact on the microstructure of sinters are chemical compo-
publications on surface remelting of stainless steels have sition, sintering atmosphere and cooling rate. In studies
focused on solid materials [10–12]. Furthermore, few studies [19,20], authors obtained very complex microstructures in
were written on laser alloying of surface layer in corrosion- 316L+430L steels after sintering in nitrogen (95%N2 + 5%H2)
resistant sintered steel [13,14]. The authors of the present and slow cooling (5 8C/s). The formation of typical duplex
study discuss the opportunities for using a cheap and popular microstructure is possible by application of rapid cooling [3,8]
method of gas tungsten arc welding (GTAW) for modification or secondary heat treatments. In this study the typical
of surface layer in sintered ferritic-austenitic steels. Modifica- austenitic-ferritic microstructure was not observed. Sinters
tion of the surface of metallic materials through exposure to were characterized by a multiphase microstructure which
the effect of electrical arc allows for obtaining of a fragmented comprised, austenite and martensite. Fig. 1 presents micro-
but uniform microstructure in the surface layer and it structures of the sinters in the initial state after etching.
improves functional properties such as resistance to friction The SEM-EDS analysis was used in order to evaluate the
wear and corrosion resistance, which has been demonstrated distribution of alloying elements in different phases in the
in previous studies [15,16]. Regarding sintered stainless steels, sinters. It can be concluded from Fig. 1 and Table 2 that the
the use of GTAW method allows for obtaining a uniform sintered stainless steels in the initial state were inhomoge-
surface which is free of empty spaces, has cellular structure neous not only in the microstructural context but also that the
and good quality of the surface [17,18]. chemical composition of a and g phases differed significantly.
This study discusses the effectiveness of remelting of the This can be explained by the diffusional process and migration
surface layer in ferritic-austenitic sinters (304L+434L) using the of Cr and Ni during sintering. This phenomenon leads to
GTAW method. The analysis focused on the microstructure different phase transformations depending on chemical
and selected properties of the obtained remelted layers. composition during the cooling process [21–23].
The sinters were remelted using a welding method (GTAW).
The layout of GTAW apparatus was presented in the study [18].
2. Material and methods
Remelting of the sample surface occurred at constant
scanning rate (340 mm/min) and current intensity of 30, 35
The aim of the study was to investigate microstructural and 40 A. Based on the macroscopic examinations of the
changes and selected properties of surface layer in sintered remelted surface, optimum current intensity was set at 35 A.
ferritic-austenitic steels after arc remelting. The specimens for The criteria used were: measurable width and depth of
the examinations were made of the water-atomized powders remelted track and good surface quality. Table 3 presents
of steels (304L and 434L according to PN-EN ISO 10088-1:2007 the parameters used in the remelting process.

Table 1 – Chemical composition of the steel powders 304L and 434L and sinters 304L-434L (wt%).
Powder grade Cr C Ni Si Mn Mo N O S Fe
304L 18.9 0.013 11.2 0.9 0.1 – 0.02 0.28 0.005 Balance
434L 16.2 0.015 – 0.8 0.1 0.98 – – – Balance
Sinter A 18.36 0.0134 8.96 0.88 0.1 0.196 0.016 0.224 0.004 Balance
Sinter B 17.55 0.014 5.6 0.85 0.1 0.49 0.01 0.14 0.0025 Balance
Sinter C 16.74 0.015 2.24 0.82 0.1 0.78 0.004 0.056 0.001 Balance
archives of civil and mechanical engineering 14 (2014) 425–432 427

Analysis of chemical composition was carried out on


surface sections using scanning electron microscope Jeol
JSM5400 with an EDS device.
An X-ray phase analysis of the as-received sinters and the
sinters after remelting was carried out using a diffractometer
Seifert XRD-3003 T-T with a cobalt lamp (lCoKa = 0.17902 nm).
Using a Hommel T1000 contact profilometer, the authors
determined parameters that characterized surface topography
(Ra, Rz, Rmax) for each of the samples. The measurements were
repeated for three times in contact with the surface examined
through coupling of the stylus with a differential measure-
ment system.
Microhardness measurements by means of the Vicker's
method were conducted for the cross-sections using a
microhardness tester (Future-Tech FM-7) with the load of
980.7 mN.

3. Results and discussion

Selection of adequate parameters of remelting of the surface


layer is particularly difficult for sintered steels. Remelting
largely depends on the shrinkage effect, which might lead to
the deformation of the material surface and material
cracking. Therefore, it is recommended to use the remelting
parameters which will cause thickening of the material in a
small volume.
Based on the macroscopic observations of the remelted
surfaces, further part of the study was carried out using the
sinters remelted with the current intensity of 35 A. The current
intensity of 30 A was too low for the adopted scanning rate to
cause considerable changes in the surface layer. An insignifi-
cant and irregular arc remelted track was observed only for the
sinter A, whereas the surface of the other two sinters exhibited
only a colourful oxide layer. The opposite effects were
produced by remelting with the current intensity of 40 A,
which negatively affected the surface quality in sinters A and
B, forming deep holes and material displacement. Conse-
quently, a loss of material and even deformation of the
specimen was observed in the sinter A. The bands remelted
with the current intensity of 35 A in all the three sinters were
characterized by even width throughout the arc effect zone
and improved surface smoothness. These observations were
reflected by the results of roughness tests (Table 4). Lower or
similar values of the Ra parameter were observed in all the
remelted zones compared to the surface of the initial material.
Fig. 2 is a graphical representation of the geometrical
characteristics of the remelted layers. It is obvious that the
shape, width and depth of the remelted layer largely depend
Fig. 1 – Microstructure of sinters in the initial state: (a) 80%
on the welding current intensity and scanning rate. Similarly
304L:20% 434L (sinter A), b) 50% 304L:50% 434L (sinter B), (c)
important role is also played by the material microstructure,
20% 304L:80% 434L (sinter C), metallographic cross-
its thermal conductivity and, in sinters, porosity. The bigger
sections, magnification 200T.
width and depth of the remelted layer was obtained for the
sinter A, where contribution of the austenitic phase was the
highest. In other sinters, both parameters had lower values.
The microscopic examinations of polished and etched The obtained results should be related to thermal conductivity
materials were carried out using an optical microscope and a of austenitic and ferritic steels (15 J/m K and 25 J/m K,
scanning electron microscope. The width and depth of the respectively). Regarding the sinter B, an additional limiting
remelted zone were estimated from the cross-sections of the factor in arc effect was high porosity (14.71%), which lowered
specimens. thermal conductivity.
428 archives of civil and mechanical engineering 14 (2014) 425–432

Table 2 – EDS analysis of sintered duplex steels in the initial state.


Element Weight concentration (%)
Sintered steel designation

A B C
0 0
g a g a g a0
Cr 18.41 19.79 17.86 18.38 17.53 17.95
Ni 7.81 2.08 10.17 4.28 8.95 0.59
Si 0.30 0.65 0.71 0.67 Below error level
Fe 72.54 77.30 71.10 76.66 73.52 79.50
0
Chemical analysis were carried out on two adjacent areas of g (austenite) and a (martensite).
In this table each percentage content is the mean value of five measurements.

Table 3 – Summary of technological parameters.


Sinter Current Arc voltage, Total arc Arc linear Scanning Gas type and
intensity, I (A) U (V) power, qc (W) energy, E (kJ/m) rate, V (mm/min) feed rate
A 30 10.5 315 55.65 340 Argon 10 l/min
35 10.5 367.5 64.92
40 10.7 428 75.62
B 30 9.5 285 50.35
35 10.2 357 63.07
40 10 400 70.67
C 30 10 300 53.06
35 10.2 357 63.07
40 10.5 420 74.2

The sintered steels were characterized by a considerable of austenite which formed a narrow transitional zone in the
microstructural non-homogeneity, which, with open porosity, sinters A and B between the remelted layer and base material.
considerably reduces functional properties of the surface layer Columnar crystals were oriented according to the direction of
and is conducive to corrosion and uneven wear on the surface. heat transfer, perpendicularly to the specimens' surface. A
The content of individual microstructural components more complex microstructure was observed in the remelted
changes depending on the contents of the powders of ferritic surface layer of the sinter C (Fig. 6). Columnar crystals occurred
and austenitic steels used for obtaining the sinters. Remelting only locally in the areas where remelting temperature gradient
caused formation of a cellular structure in the microstructure was the highest. Dendritic grains were also formed, which
of the surface layer in the sinters A and B (Figs. 3–5). The cross- suggests that solidification was the slowest for the sinter C. No
sections revealed columnar crystals, whereas surface exam- transitional zone was found between the base material and
inations exhibited evenly distributed equiaxed crystals (Fig. 3). the remelted layer. Porosity of the surface layer was entirely
Nucleation and formation of the primary structure was of removed. Presence of small empty spaces that were formed
epitaxial character and occurred on partially remelted grains during solidification of the liquid material was only observed.
It was caused by locking gas generated during the remelting
process.
Fig. 7 presents diffractograms of the steels studied in the
Table 4 – Surface roughness of sintered steels in the initial state and after remelting. The curves recorded for the
initial state and after remelting.
sinter A contain peaks from the austenitic phase (g). In the
Sintered steel Roughness parameter (mm) sinter B, peaks from the austenitic phase, which resulted
mainly from the presence of martensite (a0 ) in the microstruc-
Ra Rz Rmax
ture, can be observed only in the diffractogram of the initial
A
material. Remelting caused that the austenitic phase was
Substrate 1.81 17.36 28.04
Remelted layer 1.16 9.35 13.63
formed on the surface layer, which was noticeable in the chart.
B The diffractogram for the sinter C in the initial state contains
Substrate 1.74 13.97 20.46 distinct peaks from the ferritic phase. As results from the
Remelted layer 1.38 8.65 13.25 diffractogram of the remelted layer in the sinter C, the content
C of the ferritic phase was significantly reduced in favour of the
Substrate 2.08 12.49 16.61
austenitic phase. These observations suggest that the remelt-
Remelted layer 2.07 15.97 26.42
ing used in the study promoted formation of the austenitic
Ra, arithmetic mean roughness deviation from mean line; Rz, phase in the remelted layers.
maximum height of the profile; Rmax, maximum distance of profile
The EDS analysis of the chemical composition was carried
peak from the lowest valley
out for the remelted surface. The results are presented in
archives of civil and mechanical engineering 14 (2014) 425–432 429

Fig. 2 – Geometry of the remelted zone.

Fig. 3 – Microstructure of the remelted zone in the sinter B: BM – base material, RM – remelted material, TZ – very thin
transitional zone; surface section, magnification 100T.

Fig. 4 – Microstructure of the remelted layer in the sinter A; Fig. 5 – Microstructure of the remelted layer in the sinter B;
cross-section, magnification 200T. cross-section, magnification 200T.
430 archives of civil and mechanical engineering 14 (2014) 425–432

Table 5. Fig. 8a and b present SEM microstructures for the


sinters B and C with the areas subjected to the analysis. The
differences in the content of the alloy elements (Cr, Ni, Mo and
Si) were observed for all the three sinters between the cell
cores and the intercellular spaces. This points to a specific
process of migration of the alloy elements to cell's boundaries
that occurs during solidification [24]. Hence higher concentra-
tion can be observed in the elements in the intercellular areas
than in the axes. The greatest differences in chemical
composition occurred in the area of the remelted layer in
the sinter A. Lower contents of chromium, nickel and silicon
were found compared to the intercellular spaces (2.67%, 1.44%
and 0.75%) in the centre of the cell.
Fig. 9 presents the results of microhardness examination of
individual phases present in the base material and the
remelted layer in the sinters studied. Remelting led in all of
Fig. 6 – Microstructure of the remelted layer in the sinter C; the cases to homogenization of the microstructure, which,
cross-section, magnification 200T. apart from the microstructural examinations, was confirmed
by the microhardness tests. The hardness of the obtained
surface layer was similar to the sinters A and B, with 292.58

Fig. 7 – Diffractograms of the sintered steels obtained using XRD method for the initial material and the remelted layers.

Table 5 – EDS analysis of chemical composition of the remelted surface layers.


Element Weight concentration (%)
Sintered steel designation

A B (Fig. 8a) C (Fig. 8b)

Cellular Intercellular spaces Cellular Intercellular spaces Cellular Intercellular spaces


Cr 17.87 20.54 17.25 19.32 17.47 20.32
Ni 8.93 10.37 5.11 5.46 2.31 2.64
Mo – – 0.65 1.61 0.13 1.15
Si 0.38 1.13 0.34 0.57 0.28 0.67
Fe 72.82 67.97 76.66 73.04 79.81 75.22
archives of civil and mechanical engineering 14 (2014) 425–432 431

HV0.1 and 299.13 HV0.1. The highest value (363.65 HV0.1) was
reported in the remelted layer of the sinter C, which resulted
from the high concentration of martensite in the microstruc-
ture of the base material.

4. Conclusions

In the present work, the effect of remelting by means of GTAW


method on the microstructure and selected properties of
sintered multi-phase stainless steels obtained from powders
of 304L and 434L were studied. The following conclusions can
be drawn from the study:

 arc remelting reduced surface roughness and contributed to


densification of the surface layer and elimination of the open
porosity, which improved functional properties of the
sinters studied,
 the sinter which is the most susceptible to remelting is sinter
A due to the high concentration of austenite in its
microstructure,
 regarding the sinters A and B, the surface layer exhibits a
uniform cellular structure obtained during directional
crystallization, whereas a cellular-dendritic structure was
formed in the sinter C,
 the diffractograms recorded in the study lead to the
conclusion that the remelting used was conducive to
formation of the austenitic phase in the obtained remelted
layers; the microstructure of the remelted surface layer of
the sinters A and B exhibited presence of the austenitic
phase, while the austenitic and ferritic phases were found in
the sinter C,
Fig. 8 – Analysis of chemical composition of the cell's core
 a migration of alloy elements towards cell's boundaries
(spectrum 1) and intercellular space (spectrum 2) in the
occurred during solidification, which was reflected in the
remelted zone of the sinters: (a) B and (b) C, magnification
results of the analysis of chemical composition of the cells
3500T; b0 – irregular cells in the microstructure of sinter C,
and intercellular spaces,
magnification 700T.

Fig. 9 – Microhardness of the remelted layer and phases present in the initial material.
432 archives of civil and mechanical engineering 14 (2014) 425–432

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