Proceedings of the ASME 2013 International Mechanical Engineering Congress and Exposition

IMECE2013
November 15-21, 2013, San Diego, California, USA

IMECE2013-65498

THE RELATIONSHIP BETWEEN SURFACE ROUGHNESS AND CORROSION

Alisina Toloei Vesselin Stoilov

University of Windsor, Dept. of Mechanical,
Automotive and Materials Engineering
Windsor, Ontario, N9B 3P4, Canada
Tel: +1 (519) 253 -3000 Ext.(5980)
Email: toloei@uwindsor.ca
University of Windsor, Dept. of Mechanical,
Automotive and Materials Engineering
Windsor, Ontario, N9B 3P4, Canada
Tel: +1 (519) 253-3000 Ext.(4149)
Email: vstoilov@uwindsor.ca

Derek Northwood
University of Windsor, Dept. of Mechanical,
Automotive and Materials Engineering
Windsor, Ontario, N9B 3P4, Canada
Tel: +1 (519) 253-3000 Ext.(4785)
Email: dnorthwo@uwindsor.ca

ABSTRACT samples and a trend in the effect of roughness on

There are different parameters which can
affect electrochemical reactions such as type of
electrolyte, velocity, temperature, oxidizing
agents, impurities, anode material type and
surface treatment. It has been shown that pre-
treatment of working electrode (anode) through
abrasion techniques is one of the most important
parameters affecting on Tafel slopes and
consequently corrosion rate. Surface roughness of
the metal surface is a major influence on general
corrosion, nucleation of metastable pitting and
pitting potential as well.
In this study different surface roughnesses
were created on nickel surface by SiC papers and
corrosion properties were compared.
Electrochemical impedance spectroscopy (EIS)
and profilometry tests were carried out on all the
samples and the results were compared with
another sample prepared through laser ablation
method. Corrosion rate values were calculated and
were compared with EIS results for all the
corrosion protection of nickel was introduced. SEM
and 3D roughness images were taken and
compared for all of the samples before and after
corrosion tests. Different mechanisms were
distinguished for samples created through
different methods. The lower the roughness
values, the more the corrosion resistance. Sample
with patterns created through laser ablation
method showed the best protection properties
compared to other samples.
INTRODUCTION
Nickel is an important metal and it is used in a
large number of industrial applications such as
rechargeable batteries, coinage, filters and is
widely used as an alloying element in ferrous and
nonferrous alloys due to its strength, toughness
and corrosion resistance [1-3]. The corrosion
resistance of nickel is due to the formation of a
passive film on its surface upon exposure to the
corrosive media. Nevertheless, nickel could be
attacked by acidic media at a considerable rate.

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 This is why nickel has been the subject of
significant number of studies related to dissolution
and passivation mechanisms in acid medium [4-
6].
a has been observed e.g. mild steel [14] and AE44
b corrosion process He also suggests that the
Figure 1: 3D topography image for samples G180 (a) before and (b)
after corrosion tests
Material composition, manufacturing geometry
and roughness have been considered as important
parameters in determining corrosion properties of
the materials [7, 8]. Surface roughness plays a
significant role on the corrosion behaviour of
metals. It has been reported that an increase in
the surface roughness of magnesium alloy AZ91
[9], stainless steels [10, 11], copper [12],
aluminum and titanium-based alloys
increases the pitting susceptibility and general
corrosion rate. Typically, the general and localized
corrosion behaviour of alloys would depend on
their passivation properties. Hence, it is important
to know the passivation behavior of alloys with
different surface finish to correlate the surface
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roughness to their general corrosion and pitting
tendency [7, 9]. For metals with the ability to
form a passive layer, a decrease in surface
roughness increases the corrosion resistance but
for the ones with no passive film a reverse trend
magnesium alloy [7].
Surfaces with different roughness finishes showed
that increase in the roughness lowers the pitting
potential in 304L stainless steel in chloride
solution [15]. Burstein et.al [16] showed that the
smoother surface in stainless steel is less capable
of propagating metastable pits than the rougher
one, mainly because the sites of pitting on the
smoother surface are on average more open.
Sharland [17] suggested that the local
concentration of a solution was influenced by the
geometry of surface’s peaks and valleys. This in
turn, affected the diffusion of active ions during
corrosion resistance is closely related to the
distribution of the valleys on the surface. The
significant influence of the valleys on corrosion
resistance is related to the depth of the valleys
which affects the diffusion of active ions during
corrosion [17-20].
There are different methods to evaluate the effect
of surface roughness on corrosion behavior of
metals such as potantiodynamic polarization
method [21] and electrochemical impedance
spectroscopy (EIS). EIS is the most suitable
method for a detailed analysis of electrochemical
reactions mechanisms and kinetics. Impedance
diagrams provide data on the elementary steps
occurring in an electrochemical reaction and on
their kinetics. They also allow a thorough study of
the role of intermediate species adsorbed on the
surface and of reaction mechanisms, as well as a
study of the properties of passive films [22]. The
impedance characteristics of an electrode in acid
solutions depend largely on the type of the surface
pretreatment and surface roughness of the
electrode [10, 23]. In this study the corrosion
behavior of aligned roughness and patterned
[13]
surfaces of nickel created through laser ablation
were investigated in dilute sulphuric acid and EIS
was used to study the effect of the formation of
passive layer in both cases.
MATERIALS AND METHODS
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 Sample Preparation
15 × 15 × 1 mm high purity (99.7%) nickel
sheets were used as the test material. For
obtaining different surface roughness, the samples
were unidirectionally grinded with different grits of
silicon carbide (SiC) (i.e., 60, 180, 320 and 800)
and the samples were named with letter “G”.
Before use, they were embedded in mounting
materials and mechanically polished. Their active
test area is 1 cm2. An additional sample with
predetermined surface pattern was created by
laser ablation method. Patterns were labeled using
DxLy format where D is the hole diameter and L is
the inter-hole spacing (D10L20). To create the
holes, a copper bromide laser was used and single
pulse was applied. Nitrogen gas was blown in
order to protect the surface from oxidation.
All electrochemical experiments were conducted at
Figure 2: SEM of the sample G320 (a) before and (b) after corrosion and patterned sample (c) before and (d) after corrosion.
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room temperature. A classical three-electrode cell
was used with a saturated calomel electrode as
reference and platinum wire as counter electrode.
Prior to testing, the samples were allowed for 30
minutes to reach a stable open circuit potential.
Electrochemical measurements (open circuit
potential, potentiodynamic polarization, and
electrochemical impedance spectroscopy) were
carried out in a 0.5 M H2SO4 solution using a
CHI660D, Electrochemical Workstation Beta,
(version 11.17). A potentiodynamic polarization
technique was used to evaluate the parameters
related to corrosion and EIS measurements were
made in order to investigate the effect of surface
modification on the general corrosion resistance of
the surface. EIS diagrams were then recorded at
the open circuit potential for nickel samples. To
ensure a complete characterization of the
electrode/electrolyte interface and corresponding
processes, EIS measurements were made over six
3 Copyright © 2013 by ASME
 frequency decades from 10 mHz to 10 kHz at
open circuit (i.e., corrosion) potential and the best
equivalent circuit model was selected. The main
focus of this study is to compare samples with
roughnesses prepared by using SiC papers and
the patterned sample from corrosion point of view,
formation of passive layer and evaluate corrosion
properties of different samples using EIS method.
Equivalent circuit is determined, EIS curves are
fitted and corresponding values of the equivalent
elements are calculated.
In order to measure surface roughness
parameters and obtain 3-dimensional images of
the samples a Wyko Surface Profiling System NT-
1100 was used. Average surface roughness (Ra)
has been used as a roughness parameter in order
to describe the unique features of the surfaces.
Finally to compare the surface structure and
composition before and after potentiodynamic
testing, scanning electron microscopy (SEM) was
performed.
All testing procedures were validated by using a
reference system of pure Ni(99.7%) with surface
roughness <50nm. A detailed description of the
validation procedures can be found in [21].
RESULTS AND DISCUSSION
Roughness measurements:
It is seen in Table 1 that by increasing the grit
number, the average roughness value decreased
both before and after corrosion testing but higher
roughness values have seen for all samples after
corrosion testing. The patterned sample however
had higher roughness values and significantly
lower roughness change after corrosion testing
compared to the samples with the unidirectional
grinding roughness.
Table 1: Roughness values for samples before and after corrosion.
Roughness values
Sample Ra (Before Corrosion Ra (After
Testing) Corrosion Testing)
(nm)
G60 704.00
G180 276.00
G320 193.80
G800 41.10
D10L20 526.10
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For sake of brevity a sample 3D topography image
for samples G180 has been shown as an example
before and after corrosion tests in Fig.1(a) and
(b). As a result of corrosion the uniform area has
changed to a surface with deeper grooves with
higher roughness value. Rougher surfaces with
deeper groves have lower openness (ratio of width
to depth at opening of the grooves) which limit
the diffusion of the corrosive ions out of the
formed grooves, hence have a higher possibility to
grow larger [11]. On smooth surfaces however the
formation of stable passive film is more possible
to occur which will result in less corrosion [20]. In
the patterned sample also there was an increase
in surface roughness after corrosion testing and in
the 3D roughness image there was no significant
change in the surface appearance which will be in
agreement with the results of the corrosion rate,
EIS and SEM analysis.
Scanning electron microscopy
Figures 2(a, b). illustrate SEM images of
sample G320 before and after corrosion as one of
the examples of samples with unidirectional
roughness. It is obvious that the corrosion is more
significant along the grooves. Lee, et.al, also
reported that the deep valleys on the ground
surface are favorable sites for pit nucleation [18].
For rougher surfaces more surface degradation
was observed after corrosion testing. The results
are in agreement with the corrosion rate, EIS and
roughness observations. Figures 2(c) and 2(d)
show the microstructure of patterned sample
before and after the corrosion tests. No severe
corrosion on the surface is observed in the SEM
images. This is also in a good agreement with the
measured electrochemical values. The reason for
this phenomenon is due to the formation of
passive oxide layer and existence of air pockets
inside the holes [24]
Electrochemical measurements:
Corrosion rate (CR) values were calculated
(nm) using the Tafel extrapolation method and are
summarized in Table 2. As it is seen, by
1680.00
decreasing the roughness value from sample G60
802.28 to G800 the CR values decreased. It has been
552.10 suggested that this variation in CR were primarily
due to the anodic behavior of the alloy [9, 21].
289.58
778.23
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 Table 2: Corrosion parameters for samples with different prevented the dissolution of this layer. Therefore,
roughness the contact area between the corrosive solution
βa βc Corrosion and the substrate has decreased which
Ecorr
Sample Rate consequently results in decrease in the corrosion
(mV) (mV) (mV)
(mil/year)
rate [24, 25].
G60 -319 104.7 114.6 9.53
G180 -325.5 111.2 113.8 8.35 Nyquist and Bode plots are the two common
G320 -300.8 100.0 112.1 7.96 methods for displaying EIS data. The Nyquist
G800 -272.9 82.3 107.9 5.48 representation has the real part of the complex
impedance plotted on the X-axis and the
D10L20 -327.4 153.4 128.5 2.61
imaginary part on the Y-axis. Figure 4 shows the
The patterned sample created by laser ablation Nyquist impedance plots of nickel with different
method had the lowest value of the corrosion rate surface roughness in 0.5M sulphuric acid. The
compared to the samples with unidirectional plots of nickel shown in this figure consist of
grinding roughness (Blue point in Fig.3). The distorted semicircles. A similar behavior is
authors have shown that in patterned sample observed for all samples. As seen, the size of the
semicircle, increases with decreasing roughness.
The Nyquist plots were analyzed by fitting the
experimental data to the equivalent circuit model
shown in Fig.5. In this circuit Rs represents the
solution resistance; Rct is the charge transfer
resistance and CPE is constant phase element
related to the double-layer capacitance (Cdl).

Figure 5: Schematic for the equivalent circuit of nickel [26-28].

Figure 3: Change of corrosion rate for samples with different
roughness values
alternating solid/liquid zones, stable air/vapour
pockets and a passive oxide layer has been
formed and the existence of air/vapor pockets
Rs is in a series with a parallel combination of a
constant phase element CPE (Q) and Rct. Q is used
instead of Cdl to account for the depression of the
capacitive loop [29]. The CPE is a generalized
frequency dependent element which impedance is
given by:

Figure 4: Nyquist plots of nickel for different surface roughness

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 ZCPE=1/(Q(iω)n )
Where, i = (-1)1/2, ω is the angular frequency, ω =
2πf and f is the frequency. n=0 corresponds to a
pure resistor, n=1 to a pure capacitor and n=0.5
to a Warburg type impedance [30]. Changes in n
values have been related to diffusion process,
porosity and roughness [31].
Figure 6: Bode plots for nickel for different surface roughness
By plotting the Nyquist diagrams, it is seen that all
diagrams are characterized by depressed
capacitive loop with the theoretical center located
below the real axis. This feature reflects surface
inhomogeneity which results from surface
roughness of structural or interfacial region. These
results are consistent with literature [23, 27]. This
shape of the Nyquist plots suggests that charge
transfer controls the corrosion of Ni in acid
solutions [28]. The capacitance loops in Figure 4
enlarge by the decrease of roughness which
indicates that the corrosion is mainly a charge
transfer process [32]. It means that the resistance
is proportional to the decrease of roughness.
Namely, the lower the roughness, the higher the
resistance. It is worth noting that the decrease of
roughness in H2SO4 solution does not change
substantially the shape of the plots but increases
the impedance. This observation confirms the
suggestion that roughness does not alter the
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(1) mechanism of corrosion reaction but decrease the
corrosion by retarding the charge transfer. [28]
The same can be seen in the Bode plots which
represents a log/log plot of the magnitude of
impedance plotted on the Y-axis and the angular
frequency plotted on the horizontal axis. As it is
seen in Fig.6, the total impedance of smooth
nickel samples in solutions is relatively high
compared with rough samples. The patterned
sample again shows highest impedance value.
Bode plots show only one phase maximum at
intermediate frequencies. This result indicates that
the corrosion process occurs via one step
corresponds to one time constant [28]. The Bode
plot show that by decreasing the roughness value
maximum phase angle shifts to lower frequencies
and the polarization resistance increases resulting
in less corrosion [27]. According to Fig.7, for
lower roughness values the phase angle is around
80° suggesting that the electrochemical process
occurring at high frequency decreases the
corrosion rate [27]. It is also said that the
maximum phase angle θmax is less than 80° as a
result of the roughness of the electrode surface
[28]. Corrosion of Ni in H2SO4 solution also
enhances the roughness of the electrode surface
and therefore reduces the value of θ max.
Therefore, higher corrosion rate is related to
6 Copyright © 2013 by ASME
 higher roughness value. Thus, the lowest value of
θmax is related to more corroded sample which is
the one with the highest roughness [28].
The EIS parameters of Ni in 0.5 M H 2SO4 with
different roughnesses are given in Table 3.
Increasing Rct values with decrease of the
roughness, for nickel, suggests a decrease of the
corrosion rate since the Rct value, is a measure of
electron transfer across the surface, and it is
inversely proportional to the corrosion rate [26].
Similar trend has been reported by Hong et.al. in
their potantiodynamic tests and EIS analysis that
says the total number of the surface sites
available for metastable pits on the electrode at a
given potential decreases with increasing the grit
number of the silicon carbide paper for final
surface grinding and it implies that metastable pit
or pits starting to grow on the smoother surfaces
is more difficult than that on the rougher surfaces
[10]. The smooth surfaces also have fewer places
for pit nucleation and can quickly form a passive
film [7]. Rough surfaces also limiting diffusion out
of the grooves or forming pits and also are able to
Table 3: values of the equivalent elements
Rs Rct
Sample
(Ω) (Ω)
G60 7.99 1664.2
G180 9.21 3514.7
G320 8.56 3764
G800 8.68 4463.1
D10L20 8.98 4733.5
Figure 7: Bode phase plots for nickel for different surface roughness
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trap the corrosive ions and the corrosion products,
allowing for more pitting to occur on the semi-
polished samples [10, 11, 20]. In the fitting
method, a combination of randomize followed by
Levenberg-Marquardt fitting, was used [33].
Based on equivalent circuit model in Figure 5, the
plots are best fitted and the fitting results are
shown in Fig.8. as solid lines passing through the
testing results.
There is a good agreement between experimental
and fitted impedance spectra as well as a good
correlation between the corrosion rate and 𝑅ct
values.
In the case of the patterned sample, according to
the author’s work, the retention of the passive
oxide layer inside the holes doesn’t let the fluid
reach the bottom of the patterned hole. It has
been resulted in less contact area between
solution and the substrate and consequently will
result in smaller corrosion rate of the patterned
sample [24].
CPE
n
(Ω-1cm-2Sn)
5.58E-05 0.898
3.76E-05 0.922
4.51E-05 0.920
4.57E-05 0.920
4.52E-05 0.922
7 Copyright © 2013 by ASME

Figure 8: Fitted curve for the selected equivalent circuit
CONCLUSIONS:
The effect of different roughness created on
nickel surface was investigated through EIS, Tafel
extrapolation method, roughness measurement
and SEM. A smoother surface in the case of the
unidirectional rough surfaces will result in lower
corrosion rate of nickel samples. So, samples with
lower roughness act as better barrier to
penetration of the aggressive electrolyte to the
metal substrate. This is mainly due to the fact that
nickel forms a stable passive layer/film which
significantly reduces further mass loss(corrosion).
The introduction of the unidirectional roughness
effectively increased the area of the contact
surface between the electrolyte and the metal
surface, which in turn led to increase of the
corrosion rate. In contrast, in the patterned
surface has the highest roughness but showed the
smallest corrosion rate compared to the
unidirectional roughness samples. This result was
consistently repeated in the roughness
measurements, EIS analysis, potentiodynamic
polarization tests and SEM images. The clear
conclusion based on these results is that the
corrosion mechanism governing the
electrochemical process in the patterned surface
and the unidirectional surface roughness are
different. The most likely explanation of the
superior performance of the patterned surface is
the formation of heterogeneous wetting interface
(trapped air pockets within the surface holes),
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which significantly reduced the electrolyte/metal
surface area and the corresponding corrosion rate
[25].
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Optimization, Springer, USA.

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