Surface & Coatings Technology 205 (2010) 26052610

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Surface & Coatings Technology

j o u r n a l h o m e p a g e : w w w. e l s ev i e r. c o m / l o c a t e / s u r f c o a t

A comparative research on corrosion behavior of a standard, crack-free and duplex

hard chromium coatings
M.R. Saghi Beyragh a,b,, Sh. Khameneh Asl a, S. Norouzi c
a
b
c

Department of Materials Engineering, Faculty of Mechanical Engineering, University of Tabriz, 51666-16471 Tabriz, Iran
Faculty of Materials Engineering, Sahand University of Technology, Tabriz, Iran
Electrochemistry Lab, Material and Energy Research Center, 14155-4777 Tehran, Iran

a r t i c l e

i n f o

Article history:
Received 16 February 2010
Accepted in revised form 4 October 2010
Available online 29 October 2010
Keywords:
Metal coatings
Polarization
Corrosion
Hard coatings
Passivity

a b s t r a c t
In this study, the single and duplex layers of standard and crack-free hard chromium coatings were prepared
by using direct current (DC) and pulse current (PC) electroplating processes on mild steel substrates. The
coatings are studied from microstructure, microhardness and corrosion resistance viewpoints. The coating's
corrosion resistances have been compared through electrochemical polarization in a 3.5% NaCl solution and
standard salt spray test. Before and after corrosion tests microstructural characterization tests were done by
optical microscopy (OM) and scanning electron microscopy (SEM). The micro-crack density, in the hard
chromium microstructure, could be limited by using the pulse current electrodeposition. Crack-free hard
chromium coatings, which are deposited by PC-electroplating, were excellent in terms of corrosion resistance.
The thickness ratios in duplex coatings with crack-free sub-layer and hard chromium top coat, were also
prepared by PC- and DC-electroplating processes respectively in the standard chromium plating bath.
Standard hard chromium coating deposited by DC-electroplating had rust stains on the surfaces and edges.
The coatings with crack-free sub-layer coatings exhibited excellent results in corrosion resistance, with no
corrosion product on the surfaces and edges of the samples. Their icorr in the 3.5% NaCl solution are lower than
the standard Cr-deposited by DC-electroplating. All of the coatings are passivated in both 3.5% NaCl solution
and salt spray test environments. In addition, between the duplex layer coatings, the coating with a ratio of a
75% crack-free sub-layer (25% cracked hard top layer) showed the best corrosion resistance.
2010 Elsevier B.V. All rights reserved.

1. Introduction
Hard chromium plating is the most used electrodeposited coating
which results in high level of hardness, wear and corrosion resistance
and a low coefcient of friction in the eld of aerospace, automotive
and petrochemistry [1,2]. Hard chromium coating properties, such as
hardness and micro-crack density, change with some parameters like,
the bath composition, current density, bath ageing, temperature, etc.
[3,4]. A signicant property of the chromium coating deposited with
DC-electroplating is the high tensile residual internal stresses
originating from the decomposition of chromium hydrides during
the electrodeposition process. The high tensile stresses in hard
chromium coatings increase as the thickness increases and are
relieved by local micro-cracks produced and developed, during DCelectroplating. Therefore, micro-crack densities are related to the
tensile residual internal stresses, hardness, corrosion, and wear
resistance. On the other hand, the DC-electroplating process yields
deeper micro-cracks on the surface of the coating, which act as a canal
Corresponding author. Department of Materials Engineering, Faculty of Mechanical
Engineering, University of Tabriz, 51666-16471 Tabriz, Iran. Tel.: + 98 411 3313676.
E-mail addresses: mr.saghi@gmail.com (M.R. Saghi Beyragh),
0257-8972/$ see front matter 2010 Elsevier B.V. All rights reserved.
doi:10.1016/j.surfcoat.2010.10.009

leading the corrosive environment to the substrate/coating interface

[5].
One of the ways used to reduce the tensile stress was passing the
pulse current during the electroplating. This pulsed current has been
produced by special rectiers by means of onoff or forwardreverse
current. With this method the crack density level has been reduced to
almost zero. It is necessary to maintain that the pulse current
electroplating reduces the internal stress of the chromium which
leads to less hardness [6]. Leisner et al. [7], indicate that the current
efciency of the PC-electroplating process was strongly affected by
the anodic and cathodic charge ratio (Qa/Qc). The optimal Qa/Qc
value lies between 0.0020 and 0.0085. The current efciency in DCand PC-electroplating processes is usually lower than 25% in the
sulphate-catalyzed acid bath [8]. However, the chromium electroplating by pulse current results in lower wear resistance compared to
DC current chromium electroplating. The wear and corrosion
resistance of hard chromium deposits have been studied by several
researchers [917]. High wear resistance and low coefcient of
friction for Cr-deposits with DC-electroplating have been studied and
reported that they are caused by the high hardness and low surface
energy of these deposits. The wear mechanism in Cr-deposits
with DC-electroplating is mainly fatigue and abrasive wears and in

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M.R. Saghi Beyragh et al. / Surface & Coatings Technology 205 (2010) 26052610

Cr-deposits with PC-electroplating is mainly adhesive wear. The

coefcient of friction of DC-hard chromium coatings is lower than
PC-crack-free chromium [13,14]. Previous studies show that the best
wear resistance in the duplex coatings can be obtained by a thin
crack-free sub-layer (approximately 20 m) under the main hard
chromium layer [15].
In the case of Cr-deposits with DC-electroplating, it is found that
the corrosion resistance of these coatings in HNO3 is higher than
WCCo HVOF-sprayed coatings, because in a strong oxidizing
environment of HNO3 hard chromium becomes passivated, while in
the WCCo HVOF coat this effect did not happen. The previously
mentioned effects were completely reversed with HCl environment
[16]. The passivation of the chromium in HNO3 happened because of
the formation of a thin protective lm on the chromium by the NO 3
ion oxidizing action. The Cl ions instead, can chemically alter and
locally remove the passivating oxide lm, promoting pitting corrosion;
furthermore, their higher mobility (caused by their smaller dimension
than NO 3 ions), enables them to penetrate easily into the coating
micro-cracks, which often become preferential corrosion initiation
sites.
According to Natishan et al. [17], the hard chromium coating had the
best corrosion resistance on the 7075 aluminum substrate with no pits
or blisters on its surfaces or edges. However, it shows a lower resistance
protection of the 4340 steel substrate. Overall, it is concluded that the
performance of the hard chromium coatings on the 4340 steel and the
13-8 stainless steel was equivalent to that of WC/Co coatings.
Nascimento et al. [5] investigated the salt fog resistance of hard
chromium coatings on the AISI 4340 steel. It was observed that hard
chromium coatings were completely corroded after 72 h exposure.
Very few studies have been done about the characterization of the
corrosion resistance of Cr-deposits with PC-electroplating. With the
rapid advancement in technology, the need for components with high
wear and corrosion resistance is arising. The present work was an
attempt to meet this emerging technological need. This paper is a
presentation of comparing the corrosion and mechanical properties of
single and duplex (i.e. a hard layer on top of a crack-free sub-layer
with ratios 25/75, 50/50, and 75/25) chromium coatings electrodeposited on a mild steel substrate obtained by direct current and
pulse current. The corrosion resistances have been tested through
electrochemical polarization in the 3.5% NaCl solution and salt spray.

Table 2
Electroplating current information of single layer specimens.
Specimen

Type of
current

Cathodic
current
density
(A/dm2)

Anodic
current
density
(A/dm2)

On time
(s)

Off time
(s)

Current
density ratio
of on/reverse

DC
PC

Direct
Pulse

40
40

0
10

30

0.03

25%

reverse square pulse currents were used in the process. The detailed
explanation of the PC-crack-free hard chromium coating procedure has
been given by Khameneh Asl et al. (Table 2) [15]. The distance between
anode and cathode was 10 cm, while the area ratio was 1:1. The total
thickness of the coatings was approximately 100 m.
2.2. Experiment details

2. Experiment

Cross-sectional microhardness measurements were tested using

the micro Vickers hardness tester (HMW-20000), by means of Vickers,
indentation at a load of 50 g. Selected measure was an average of 5
indentations for each site.
The corrosion resistance of samples was evaluated by means of
electrochemical measurements in 80 mL aerated and unstirred 3.5%
NaCl solution. An Ag/AgCl, KCl-saturated electrode was used as a
reference electrode and a Pt rod as a counter electrode. A working
electrode of each coated sample was horizontally xed at the bottom of
the electrochemical cell with an exposure of 1 cm2 to the solution.
Open-circuit (OCP versus time) and voltammeter curve (CP) measurements were taken using an EG&G Parc-273 (Princeton, NJ) device. Linear
sweep voltammeter carried out in a potential range from 0.7 to
+2.5 V and OCP at 0.32 mV/s. All of the electrochemical measurements
were carried out in a limited temperature.
The salt fog spray tests were carried out according to the ASTM
B117-90 standard, using 5 wt.% NaCl, pH of 6.57.2, at 35 C. The
samples were placed in the salt spray chamber, at 15 tilted from the
vertical position. The samples were observed after 72 h for corrosion
products on their surfaces. Then, for each sample a protection rating
based on the standard ASTM B537-70 was assigned, which is
summarized in Table 3. The protection rates are an indication of
how well the coating was effective in protection of the substrate.
The microstructures of all the coatings were investigated using an
optical microscope (OM) and a scanning electron microscope (SEM).

2.1. Material specication

3. Results and discussion

In this experiment, two types of hard chromium coatings were

studied. In the rst stage, a sample was coated by standard hard
chromium with direct current. The second specimen was plated by
crack-free chromium with the pulse electroplating process. In the
second stage, duplex hard chromium coatings (i.e. a standard cracked
hard chromium layer on top of a crack-free chromium sub-layer) with
ratios of 25(standard)/75(crack free), 50/50, and 75/25 were prepared.
The selected substrate material was a St 37 mild steel (a plain carbon
steel, ~0.17% C). Specimens were polished with 1000 grit sand papers.
Hard chromium bath has been used with industrial deposition
parameters, the detail of which is shown in Table 1. Direct and periodic

The Cr-deposit with DC-electroplating has a smooth and bright

surface, while the Cr-deposit with a PC-electroplating surface is dull
and grey (Fig. 1). Figs. 2 and 3 represent the microhardness prole of
single and duplex hard chromium coatings. The microhardness of
the DC-coating was 875 Vickers, whereas the microhardness of the

Table 1
Hard chrome deposition parameters.
Bath composition
Bath temperature (C)
Approximate current density (A/dm 2)
Thickness (m)

CrO3 250 g L 1; H2SO4 2.5 g L 1;

no additives
50
40
100

Table 3
Protection rating vs. area of defect from ASTM B 537-70.
Area of defect (%)

Rating

0
to 0.1
0.10.25
0.250.5
0.51.0
1.02.5
2.55.0
510
1025
2550
N 50

10
9
8
7
6
5
4
3
2
1
0

M.R. Saghi Beyragh et al. / Surface & Coatings Technology 205 (2010) 26052610

2607

1000

Hardness (HVN)

900

PC

75%PC

50%PC

25%PC

800
700
600
500
400
300
0

20

40

60

80

100

120

Distance from Surface (m)

Fig. 3. Through thickness HV microhardness for duplex electrodeposits.

Fig. 1. Images of (A) PC-coating, (B) 75%, (C) 50%, and (D) 25% PC duplex deposit surface
appearance.

PC-coating was 730 Vickers. The hardness of the substrate/coating

interface decreases due to microstructural changes in this section. As a
matter of fact, the coating surface microstructure is dendritic but the
interface structure due to substrate and coating bonding, and ne
grained and equi-axed structure is far from dendritic structure nature
and its hardness has lower values.
The reason of this difference could be the effect of pulse current on
hydrogen evolution reaction in the PC-electroplating process. The
hydrogen reacts with chromium and produces chromium hydrides.
The hydrogen atoms enter the chromium crystals and make a
distortion in the crystal structure. The crystal structure of the coatings
together with oxide, hydroxide and hydride inclusions with high
levels of internal stress, gives a high hardness and a crack network
throughout the coating (Fig. 4). Oxide, hydroxide and hydride in
standard chromium plating increase the hardness with mechanisms
like limiting the simple slip, preventing the dislocation movements,
and decreasing the slip systems in the structure. Internal stresses in
the structure are due to production of hydrides and parametric crystal
system changes. The PC-electroplating process results in easier
movements of dislocations and increase in slip systems and therefore
reduces hardness by decreasing oxides. Also, using pulse reverse
current pushes the structural hydrogen out of each cycle. During
reverse period in pulse current, stress relief and/or anodic reaction
occurs on the sample surface, resulting in less hydrogen adsorption

and hence less chromium hydride formation [6]. The presence of

chromium hydride is thought to be a main factor for internal stress
and resultant increased hardness.
In addition, the hard chromium coating contains numerous small
vertical micro-cracks. The reason for this cracked morphology in the
Cr-deposit with DC-electroplating has not been completely understood yet. It is believed that they are caused by relaxation of residual
tensile stresses formed during the coat deposition [16]. All of the
coatings showed an excellent interface with the substrate, completely
free from defects.
Using pulse reverse current repels atomic hydrogen which is
produced and absorbed around the cathode. This phenomena cause
the reduction of hardness at the Cr-deposited with PC-electroplating.
On the other hand, using pulse current increases suitable sites of
nucleation during every cycle. This cyclic nucleation produces the ne
grained and equi-axed structure that decreases the internal stress,
because of a lot of grain boundary in equi-axed ne grains. During the
rst stage of coating, deposition is initiated locally on the surface
where the nuclei start to form at the points with high stress and/or
defects [6]. During the deposition period, growth would be into a
dendritic structure, resulting in high internal stresses. But in the case of
interruption, by reverse current, growth is prevented and during
subsequent on periods or forward current, further nucleation occurs,
which results in equi-axed small grains with low internal stress and
lower hardness [18]. In general, equi-axed ne grains have lower
stress, which prevents cracking. In addition, problems like chromium
hydrides and atomic hydrogen causing stress and distortion in
chromium structure, will be removed using pulse current [19]. Fig. 5
shows the SEM micrograph of the PC-coating surface. PC-coated
surfaces contain a series of dome shaped grains. In the PC-coatings,
there is no evidence of any micro-cracking as found in DC-coatings
[20,21]. This point seems to have been caused by the re-oxidation of
hydrogen, which was dissolved in the deposit, during the reversal step.

1000
900

PC

Hardness (VHN)

800

DC

700
600
500
400
300
200
100
0
0

20

40

60

80

100

120

Distance from Surface (m)

Fig. 2. Through thickness HV microhardness for samples of DC- and PC-chromium
electrodeposits.

Fig. 4. SEM micrographs of DC chromium electrodeposits.

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M.R. Saghi Beyragh et al. / Surface & Coatings Technology 205 (2010) 26052610
Tables 4
Polarization test results for hard chromium coatings in a 3.5% NaCl solution.
Coating

DC-coating

Duplex
coating25%
crack-free
sub-layer

Duplex
coating50%
crack-free
sub-layer

PC-coating
Duplex
coating75%
crack-free
sub-layer

Ecorr [mV]
548.3
599.9
677.0
611.8
587.3
icorr [A/cm2] 2.039 10 6 18.61 10 6 1.535 10 6 0.764 10 6 0.108 10 6

Fig. 5. SEM micrograph of the Cr-deposit surface with PC-electroplating.

In the case of duplex coatings, microhardness is very close to that of

DC-coating microhardness (Fig. 3). The hardness of the duplex
coatings is higher than the single ones, since the DC-coating is as the
sub-layer. The duplex coating surfaces have some micro-crack that is
extending to the crack-free sub-layer. The crack density of duplex
coatings increases with increases of top hard layer thickness. The dome
dimensions slightly increase in duplex coatings with the increase of
top hard layer thickness (Fig. 6). According to the previously
mentioned experiments, the increase of thickness is the main factor
in the creation of cracks. The microstructures of duplex coatings
surfaces are close to the structure of the crack-free sub-layer, while,
the top hard layer was produced by DC-electroplating.
Table 4 describes the results of the polarization tests for hard
chromium coatings. PC-coating samples show the best corrosion
resistance; in fact, icorr is about 10 7 A/cm2. Polarization diagrams
(Fig. 7) indicate the electrochemical behavior of PC- and DC-coatings.
OM micrographs (Fig. 8) indicate the appearance of some supercial
cracks for DC-coatings, with a clear sign of corrosion products such as
stains of rust on the surface after polarization test. However, in the case
of PC-coatings no clearly visible corrosion products were observed.
These cracks could be the reason why the polarization diagram of the
DC-coating indicates a current density (2.039 10 6 A/cm2) higher
than PC-coatings. The corrosion current density (icorr) in NaCl lies
between 10 5 A/cm2 and 10 9 A/cm2 for PC-coating, conrming that
the coating is substantially passive. Thus, pulse current electroplating is
able to conform the coating a good corrosion resistance over long
periods. The anodic polarization curve of the DC-coating is related to its
cathodic polarization curve, which indicated that the anodic reaction is
overcoming corrosion mechanism. It is conclusive that the polarization
behavior of the hard chromium coating is due to metal dissolution
(Cr atoms). Accordingly, more severe corrosion in the DC-coating layer
is attributed to the accelerated corrosion of the substrate. This corrosion
associated with the inltration of the solution between the coating layer
and substrate interface through the cracks.
Fig. 9 shows the polarization diagrams of the duplex coatings in the
aerated 3.5 wt.% NaCl solution. The duplex coatings with a 75% crack-

800
PC

DC

600
400

E (mV)

200
0
-200
-400
-600
-800
-1000
-10

-8

-6

-4

-2

Logi (A/cm2)
Fig. 6. SEM micrograph of (A) 75%, (B) 50%, and (C) 25% PC duplex deposit surfaces.

Fig. 7. E [V]log (I) [A/cm2] polarization diagrams for PC- and DC-coatings in a 3.5% NaCl
solution.

M.R. Saghi Beyragh et al. / Surface & Coatings Technology 205 (2010) 26052610

2609

Fig. 10. OM micrograph of the DC-coating surface after the salt spray test in a 5% NaCl
solution after 72 h.

Fig. 8. OM micrograph of (A) PC- and (B) DC-coating surfaces after the polarization test
in a 3.5% NaCl solution.

free sub-layer presented a lower current density (0.764 10 6 A/cm2)

than the other duplex coatings, indicating that the duplex coating with a
75% crack-free sub-layer has a higher corrosion resistance in 3.5% NaCl
environment. Previous studies [15] show the formation of few microcracks along the coating cross-section for duplex coatings; these microcracks have not reached the coating interface between the hard layer
and the crack-free sub-layer. The electrochemical behavior of duplex
coatings was very similar to PC-coatings, however its surface has few
micro-cracks but the crack-free sub-layer prevents diffusion of the
corrosive solution to the substrate. The corrosive solution has not
reached the substratecoating interface in any of the duplex coatings,

whereas the corrosive solution has reached and attacked the substrate
of the DC-coating. The PC and duplex (with a 75% crack-free sub-layer)
coatings have protected better the substrate from corrosion attributed
to their lower porosity and micro-cracks. Generally, In NaCl solutions, all
of the coatings passivate and show an extremely good resistance.
The visual inspection is found to be a qualitative way to get the
result of the salt spray test. Figs. 10 and 11 clearly show the higher
salt spray resistance of the PC-coating specimen. In relation to the
PC-coating specimen with 100 m thickness which is subjected to
72 h in a salt spray environment, it was observed that its surface has no
corrosion products (Table 5). Under the same condition, the corrosion,
DC-coating specimen was visually 100% corroded. This experimental
behavior is related to the high content of micro-cracks in the surface
and depth of cracks. For duplex coatings, we did not observe any
corrosion products on their surfaces either, which is due to good
protection resistance of the PC-sub-layer in them.
Table 6 represents the protection ratings for the coatings. The
protection ratings for individual samples are assumed to be 0 to 10.

800
75%PC

50%PC

-5

-3

25%PC

600
400

E (mV)

200
0
-200
-400
-600
-800
-1000

-9

-8

-7

-6

-4

-2

-1

Logi (A/cm2)
Fig. 9. E [V]log (I) [A/cm2] polarization diagrams for duplex coatings in a 3.5% NaCl
solution.

Fig. 11. Images of (A) PC- and (B) DC-coating surfaces after the salt spray test in a 5%
NaCl solution after 72 h.

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M.R. Saghi Beyragh et al. / Surface & Coatings Technology 205 (2010) 26052610

4. Conclusions

Table 5
Results of the salt spray test in 36 and 72 h.
Exposed
time

DC-hard
chrome
(%)

Duplex
coating25%
crack-free
sub-layer (%)

Duplex
coating50%
crack-free
sub-layer (%)

Duplex
coating75%
crack-free
sub-layer (%)

PC-hard
chrome
(%)

36 h
72 h

50
100

0
0

0
0

0
0

0
0

Table 6
Average value of the protection rating.
Coatings

DC-hard chrome
Duplex coating25% crack-free sub-layer
Duplex coating50% crack-free sub-layer
Duplex coating75% crack-free sub-layer
PC-hard chrome

Approximate rating
after hours
36

72

1
10
10
10
10

0
10
10
10
10

The average of the corrosion rating for the DC-sample is 1.5, while the
protection ratings for all samples of duplex and PC-coatings were 10.
The performance of the duplex and PC-coating was excellent as
coatings provided signicant protection for the St 37 mild steel.
It is well known that the DC-electroplating process has deeper
micro-cracks, while in the PC-coating surface no cracks exist to lead
corrosive solution in the substrate/coating interface. In addition, PCcoatings have a ne and dense structure in comparison with DCcoatings. As a result, there is no possibility for diffusion of the
corrosive environment to the substrate/coating interface through a
dense structure. The corrosion mechanism of standard chromium
coatings (DC) is deep cracks, which grow through the interface of the
substrate/coating into the base metal (Figs. 10 and 11B). A signicant
characteristic of standard chromium electroplating is the high tensile
residual internal stresses originating from the decomposition of
chromium hydrides during the electrodeposition process. These high
tensile stresses in electroplated chromium coatings increase as
thickness increases and are relieved by local micro-cracking during
electroplating. Therefore, basically, micro-crack density is related to
the high tensile residual internal stresses, hardness, and corrosion
resistance [2225]. It is also clear that the increase in the thickness
enhanced the hard chromium protection to the salt spray corrosion.

The salt fog and electrochemical tests showed better resistance for
the Cr-deposits with PC-electroplating. For the salt fog tests, corrosion
products were not found on the duplex and PC-coatings, even after
72 h test. The sample, with Cr-deposits using the PC-electroplating
process, showed a lower current density than the Cr-deposits with
DC-electroplating, it has been observed that the electrolyte did not
reach the mild steel substrate even in a 3.5% NaCl solution. Cr-deposits
with DC-electroplating had an average rating protection for surfaces
approximately 1.5. In addition, duplex and PC-coatings had rating
protection surfaces approximately 10. With these tests, we reached to
the highest point of corrosion protection in duplex coatings with
saving the level of hardness on the surface up to the standard hard
chromium coating hardness.
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