The First National Conference for Engineering Sciences FNCES'12 / November 7-8, 2012
Photoelectrochemical Hydrogen Evolution on the
Copper Surface
Hassan A. Alsaadi, Chemical Eng. Dept., College of Eng., University of Baghdad,
Baghdad, Iraq
alwan_hassan@yahoo.com
Abstract- This electronic document is a part of the MSc.
degree in the Corrosion Control Eng./UK. The aim of this
project is to investigate whether or not the oxygen-free
water oxidises copper due to the photoelectrochemical
decomposition of water at prior either copper oxides or
copper sulfide that covered copper surface. This study
involved study the effect of the visible light irradiation on
the current density of either Cu2O or Cu2S that covered
copper surface immersed in either aerated or deaerated 0.1
M NaCl solution, calculation concentration of dissolved
hydrogen in the water, and detection hydrogen gas.
This study showed that the current density of either Cu2O or
Cu2S increased toward cathodic region at light condition. It
also showed that hydrogen evolution on the Cu2O surface,
which was formed on the clean copper surface by anodic
polarisation method, was detected and the oxygen that was
produced could react with copper.
Introduction
According to Pourbaix diagram, copper shows
excellent corrosion resistance in natural water.
This is due to formation a passive film of copper
oxides after exposure to the water for long time
[1]. However, Studying behaviour of copper in
deaerated pure water has been a major interest to
the scientists since Hultquist stated in 1986 that
hydrogen evolution on the copper surface, which
immersed in deoxygenated pure water, was
observed. This means that copper is corroded by
pure water [2]. The main reason why research on
copper corrosion in pure water is vital to do
efforts in experimental and theoretical work is
related to the danger of the
nuclear waste radiation which causes severe
damage to the human and the environment.
In the recent years pure copper is used as a high
level nuclear waste canister in order to separate
the dangerous of the radioactive waste from
human and the environment. Copper canister in
which the spent fuel is stored is designed by SKB
(Swedish Nuclear Fuel and Waste Management
Company). The high level nuclear waste canister
consists of an outer corrosion resistant metal that
1
make of copper and a pressure-bearing insert of
cast nodular iron. Then, the copper canisters are
shield with a thick layer of bentonite clay before
they buried in deep ground water (repository)
about 500 m down in the Swedish bedrock [3, 4].
Since concentration of dissolved oxygen is reverse
proportion to the depth of the water, therefore,
concentration of dissolved oxygen in the deep
ground water is lower than that at the surface of
the water. However, copper can form two types of
oxides (i.e. Cu2O, CuO) since copper is oxidised
by water not by oxygen which supports formation
of the passive films on the copper surface [1].
Copper also forms copper sulphate from its
reaction with sulphate that is present in the
groundwater. If the anaerobic sulphate-reducing
bacteria (SBR) exist beneath copper sulphate, it
leads to reduce sulphate into copper sulphide.
Copper (I) oxide (Cu2O) and copper sulphide
(Cu2S) are well known to accelerate
decomposition of water into H2 and O2 on their
surface under visible light irradiation [5,6,7,8,9].
Hydrogen evolution from decomposition of water
on a semiconductor with energy band gap range
1.5 3.1 eV under visible light irradiation is
thermodynamic feasible [5,6]. (Cu2O) and Cu2S
are a p-type semiconductors with energy band gap
2 eV and 2.3 eV respectively. It is sufficient to
split water into H2 and O2 under visible light
irradiation [7,8,9].
The first paper about studying corrosion of copper
in pure water was published by Hultquist in 1986.
He stated that copper is susceptible to the uniform
corrosion in pure water. As a result, cuprous oxide
is formed on the copper surface as a corrosion
product that accompanied with hydrogen
evolution [2]. In contrast, Simpson et al and
Eriksen et al stated that the copper showed
excellent corrosion resistance in either dilute de-
aerated sodium chloride solution or pure
deoxygenated water when they studied behaviour
of copper in de-aerated water in 1987 and 1989
respectively. A gas chromatograph was used by
both of them in order to detect hydrogen gas that
evolved from corrosion of copper by oxygen-free
water [10,11]. In spite of the work of Simpson et
 The First National Conference for Engineering Sciences FNCES'12 / November 7-8, 2012
al. and Eriksen et al., Hultquist et al. reported
further experiments in 1989 that confirmed his
observations obtained in 1986. The new
experimental tests based on visual monitoring the
appearance of two samples of clean copper
surfaces that were placed in two different vessels
containing 1.7 dm-3 of distilled water which
contained 0.032 mg of oxygen at 50 C. Oxygen
was prevented to enter to the systems. This
obtained by using palladium enclosure to close
one vessel while the other was closed with Pt.
enclosure. Hultquist observed that the specimens
oxidised and all the dissolved oxygen was
consumed [12].
Further more; in 2007 Szakallos et al observed
that hydrogen gas evolved from the corrosion
system in the absence of the oxygen. He also
stated that rate of the hydrogen evolution
determines the amount of corrosion product in
form hydride. This obtained during studying
corrosion of clean copper in deionised water under
vacuum pressure [13].
The Experimental Work
The experimental work for studying
photoelectrochemical hydrogen evolution on the
copper surface comprised of three stages. The first
stage involved preparation of either a gray porous
structure of copper (I) sulfide (Cu2S) thin film or a
reddish thin film of Cu2O on a clean surface of
pure copper with 62.84 cm2.
Formation a thin film of copper (I) sulfide (Cu2S)
on the copper surface was achieved by the
reaction of a solid clean copper with hydrogen
sulfide gas (H2S) at room temperature and
atmospheric pressure according to the following
equilibrium reaction [14]:
2Cu + H2S + 1/2O2 Cu2S + H2O
In this experiment, hydrogen sulfide was produced
from the dissolution of iron sulfide (FeS) in dilute
sulphuric acid according to the following reaction
[15]:
+ 2+
FeS + 2H Fe + H2S(g)
Whereas, Formation of a reddish thin film of
cuprous oxide (Cu2O) on copper surface was
obtained by anodic polarisation of the copper
sample in neutral or alkaline solution at constant
applied potential at which a solid Cu2O is
2
thermodynamically stable surface according to the
following reaction [1].
2Cu + H2O = Cu2O + H2
Both layers (Cu2S and Cu2O) are applied on the
copper surfaces after removing a prior oxide,
grease, and dirt from the surface of the copper
samples by using a chemical pickling process.
The second stage included measure of the current
of the pure copper containing either cuprous oxide
or copper sulfide at dark and light conditions in
order to monitor the effect of visible light
irradiation on current of a p-type semiconductor
(Cu2O, Cu2S) under aerated and deaerated
conditions. A nitrogen gas stream was used to
deaerate the system. This was achieved by
bubbling a solution with oxygen-free nitrogen gas
which caused removal of a high proportion of the
dissolved oxygen gas from the system.
In this stage a calomel electrode was used as a
reference electrode which was placed close to the
WE (working electrode) during polarisation of the
latter in either 0.1 M Na2SO4 solution (pH 7) or
0.05 M Na2SO4 solution at pH 10. This led to
decrease of the resistance of the electrolyte to the
flow of ionic current [16].
In additional to the reference electrode the
electrochemical cell consisted of AE (auxiliary
electrode) that was Platinum wire with a diameter
of 0.2 mm and a pure copper sheet, which
contains either a reddish thin film of (Cu2O) or
gray porous structure of (Cu2S) on its surface, acts
as working electrode (WE).
Then, the current densities of the WE were
measured when switching light off and switching
light on after the applied potential had been fixed
at Erest of the WE, i.e at corrosion-free potential.
The period of light condition was between 5
seconds and 10 seconds while the period of dark
condition was between 10 seconds and 15
seconds. Figure1 shows the setting up of the
electrochemical cell. Table1 explains the
conditions for three experimental tests that were
performed in this stage under various conditions.
 The First National Conference for Engineering Sciences FNCES'12 / November 7-8, 2012
should be differ from that at switch light off, if the
hydrogen was evolved from splitting of water.

In this experiment, the system consisted of a ref.

Figure1: Experimental arrangement for studying effect of
the visible light irradiation on clean copper surface
containing Cu2O/Cu2S
E. (calomel electrode) and A.E. (Pt. rod), while
the W.E. was a 3.14x10-2 mm2 of a Pt. wire. The
W.E. was placed at a distance of 0.2 mm of the
oxidised copper sample in order to avoid
dispersion of the hydrogen gas away from the Pt.
wire surface. The values of the applied potentials
that were used in this test were 0 V under
deaerated condition.

Tabl1: Explains the conditions for four experimental tests Results and Discussion
that were performed in this stage under various conditions Photoactivity of Cu2O Formed by Anodic
Condition Exp.1 Exp.2 Exp.3
Polarisation
Form of a Cu2O Cu2O Cu2S
semiconductor Figure2 shows the current density at Erest versus
time at switching light off and switching light on
Method of the
formation Anodic Anodic Chemical
for two types of Cu2O that were formed on the
Cu2O/Cu2S Polarisation Polarisation reaction copper surface by anodic polarisation. For the first
Total period of type of Cu2O, the formation of Cu2O on clean
the formation 46 96 2
Cu2O/Cu2S (h) copper surface was performed in 0.1 M Na2SO4 at
Total surface pH 7 for 46 h. For the second type, it was
area of the 63.66 63.75 62.6
sample (cm2) performed in 0.05 M Na2SO4 at pH 10 for 96 h.
Electrolyte 0.1 M 0.05 M 0.8 M Study of the effect of visible light irradiation on
Na2SO4 Na2SO4 NaOH
the surface of each type was performed in two
pH of solution
7 10 7 conditions that were either aerated or deaerated
The exposed conditions. The experimental tests for both types
area of the 44.5 40.6 49 started with switch light on for 10 sec followed by
sample (cm2)
Period of switch light off for 15 sec. The current density of
deaeration 27 96 24 WE (oxidised copper sample) at switch light off
process (h)
Erest under was about zero at Erest.
aerated - 65.3 - 55 - 278.5
condition
(mV SCE)
Erest under
deaerated - 147.7 - 329 - 290.7
Condition
(mV SCE)
Hydrogen gas detection stage, this was third
stage in the experimental work for studying
photoelectrochemical behaviour of either cuprous
oxide or copper (I) sulfide (Cu2S) under visible
light irradiation. This achieved by Monitoring the
current of the Pt. wire (W.E.) at dark and light
conditions to detect hydrogen evolution on a Cu2O
surface. In this stage, a copper sample, which had
Cu2O on its surface, was used only.

The principle of this experimental test involved
that the W.E. (Pt. wire) was subjected to an
applied potential at which the hydrogen, which
was evolved on the surface of the copper sample
under visible light, started to oxides at the Pt. wire
surface. The current on the W.E. at switch light on
3
Figure2: Photoactivity of Cu2O that is formed on the clean
copper surface by polarisation method in Na2SO4 pH 7 and
pH 10. The period of each switch light on was 10 sec
followed by switch light off for 15 sec.
It can be seen from the above Figure that the
current density of the WE under either aerated or
 The First National Conference for Engineering Sciences FNCES'12 / November 7-8, 2012
deaerated conditions for each type of Cu2O
increases suddenly and becomes more negative at
each time when switching light on than when
switching light off, which was about zero. This
means that a cathodic reaction took place on the
surface of a p-type semiconductor (Cu2O) during
light on period. Since hydrogen evolution from
photoelectrochemical decomposition of water
took place at a p-type semiconductor with a band
gap above 1.6 eV, therefore reduction of water
into H2 and OH- occurred at a Cu2O surface and
led to make the current density of copper (I) oxide
to be more negative than that at switching light off
[17] Splitting of water into H2 and O2 at the
excited Cu2O involved two electrochemical
reactions, which were reduction of water and
oxidation of hydroxyl into O2 and H2O according
to the following equations that occurred
simultaneously [17].
- -
2H2O + 4e H2 + 2OH
2OH- H2O + O2 + 2e-
The cathodic reaction happened at the WE
(Cu2O), whereas the anodic reaction took place at
the AE (Pt). The electrons, produced from the
anodic reaction, moved through the connection
wire to the cathode and then transferred across the
majority electrical charge carriers (electron holes)
from the valence band to the conduction band of
the Cu2O at which water reduction occurred [17].
As a result, the current density tended toward
cathodic current.
It also can be seen from the graph that an increase
in the current density of the WE at switching light
on happened for a short time and then began to
decrease gradually with time. This was because
when a semiconductor was subjected to a visible
light energy that was higher than its band gap
energy, electrons and electron holes were
generated in the semiconductor. As a result, their
concentration was grown above the equilibrium
concentration until the production rate was
compensated by recombination reaction of the
holes and electrons. Recombination reaction leads
to reduced amount of the electrical charge carries
that were available to convert the light energy to
chemical energy at the semiconductor-electrolyte
interface [18].
Finally, the cathodic current density that was
produced by indirect photoelectrochemical
4
decomposition of water on the surface of the
second type of Cu2O forming on copper surface
by anodic polarisation of clean copper in 0.05 M
Na2SO4 at pH 10 for 96 h was higher than that
produced on the surface of the first type that was
formed by anodic polarisation of clean copper in
0.1 M Na2SO4 at pH 7 for 46 h. This was because
the period of formation of Cu2O on the copper
surface in the second type was longer than for
formation of oxide on the first type. As the
thickness of the passive film increases with time,
therefore the film thickness of the second type
was thicker than for the first type of a p-type
semiconductor. This led to the increase of the
excited area of the electronic state for the second
type during the light on period. Hence, an increase
in the concentration of the electrons in the
conduction band and concentration of the holes in
the valence band occurred under the visible light
irradiation. Consequently, the rate of
photoelectrochemical decomposition of water at
the surface of the second type of Cu2O increased.
Photoactivity of Cu2S
Figures3 and 4 show the current density at Erest
versus time for copper sulfide in 0.8 M NaCl at
switching light off and switching light on. The
former was obtained under aerated conditions,
while the latter was achieved under deaerated
conditions. The experimental tests was started
with switch light on for 5 sec followed by switch
light off for 10 sec and this was repeated until the
end of the experiment.
Figur3: Photoactivity of Cu2S in aerated solution of 0.8 M
NaCl. The period of each switch light on was 5 sec and then
followed by switch light off for 10 sec.
 The First National Conference for Engineering Sciences FNCES'12 / November 7-8, 2012
Figure 5 shows the current density of Pt in
deaerated solution of 0.1 M Na2SO4 versus time
under dark and light conditions at 0 V. The
experiment started measuring the current density
of WE at switch light on for 10 sec followed by
switch light off for 15 sec. This was repeated until
the end of the experiment. It was performed in the
presence of the oxidised copper sample in the
system. However, the copper sample was not
connected to the electrochemical cell. This means
that WE and AE were Pt wire and Pt electrode
Figure4: Photoactivity of Cu2S in deaerated solution of 0.8 respectively.
M NaCl. The period of each switch light on was 5 sec and
then followed by switch light off for 10 sec.

It can be seen from each Figure that the current

density of a WE at each light on period increased
suddenly and became more negative than that at
each switching off of light. This means that a
cathodic reaction took place on the surface of a p-
type semiconductor (Cu2S) during light period.
This cathodic reaction thought to be hydrogen
evolution from indirect decomposition of water
that took place at the p-type semiconductor
(Cu2S)/electrolyte interface at switching light on.
For a p-type semiconductor splitting of water into
Figure5: Detection of hydrogen evolution on platinum surface in
H2 gas and OH- ions (reduction reaction) occurs deaerated solution of 0.1 Na2SO4 in the presence of Cu2O in the
on the surface of the semiconductor, while system that was formed by anodic polarisation. Each switch light
oxidation reaction occurs on a metal surface [17]. on that was for 10 sec, followed by switch light off for 15 sec.

On the other hand, all metal sulfides are As can be seen from Figure, significant change
susceptible to the photodegradation. This is took place in the current density of the WE (Pt) at
because the S2- anion oxidises instead of water each switching on of light compared with that in
under visible light [5]. This was the reason why Figure 6 which shows the effect of the visible
copper sample, which had copper (I) sulfide on its light irradiation at various applied potentials on
surface, did not used in the last stage of this the current density of the Pt in the absence of the
studying. Cu2O from the system under deaerated condition.
The change in the current density of WE in the
experimental test happened for short time (about
Detection of Hydrogen Gas 1-2 sec). As can be seen from the Figure 5, the
current density of WE under light conditions
According to the experimental results, the became more positive than that at dark conditions.
concentration of H2 that is evolved by
photoelectrochemical decomposition of water at
either Cu2O or Cu2S/electrolyte interface was
higher than its solubility in the water at actual
partial pressure of hydrogen in the atmospheric
( pH 2 ) 4.935x10-7 atm. Therefore, hydrogen gas
can be detected by using any technique such as
gas chromatographic technique, solid electrolyte
probe technique, and polarisation method. In this
study, polarisation method was used.

5
 The First National Conference for Engineering Sciences FNCES'12 / November 7-8, 2012
Figure6: Photoactivity of platinum in deaerated solution of 0.1 M
Na2SO4 in the absence of Cu2O from the system. Each switch light
off that was for 15 sec, followed by switch light on for 10 sec.
According to the Pourbaix diagram for copper-
water containing SO42- ions, the equilibrium
+
potential of H /H2 can be calculated from the
below equation [19]:
Eoa= 0.00 - 0.0591pH - 0.0295 log pH 2
Where
Eoa = equilibrium potential of H+/H2
pH = 7
pH 2 = partial pressure of H2 (atm)
Partial pressure of H2 can be calculated from
(Henrys law), Henrys constant for H2 is k =
8.5x10-4 M/atm [11]. According to the
experimental results, the concentrations of
dissolved H2 in water were between 4.9x10-9 M
-7
and 2.5x10 M at pH7. Then, the pH 2 is between
5.76x10-6 atm and 3x10-4 atm. Hence, the
equilibrium potential of H+/H2 is between -0.26 V
NHE (-0.5 V SCE) to -0.31 V NHE (-0.55 V
SCE). The applied potential, which was used in
the experimental test, was 0 V SCE. Therefore, if
H2 was evolved by photoelectrochemical
decomposition of water at Cu2O surface that was
not connected to the electrochemical cell, it would
oxidise on the Pt surface.
A semiconductor that is used as a photocatalyst
for photo chemical decomposition of water into
H2 and O2, should have band gap energy between
1.5 eV and 3.1 eV. [7,8] The band gap energy of
Cu2O is 2 eV, which is sufficient for
decomposition of water under visible light
irradiation [8].
The rate of photoelectrochemical decomposition
of water into H2 and O2 is controlled by the
partial pressure of O2 in the system.
Decomposition of water on the surface of Cu2O
under light condition is in reverse proportional to
the pO2 in the system. This means that hydrogen
evolution from splitting of water decreased with
the increase of the pO2 in the system [8]. In order
to avoid this from happening, the system of
experiment was deaerated for 5 days. This was
sufficient to remove most of the O2 from the
system. As a result, H2 evolution could obtain.
As can be seen from the Figure5, the current
density of Pt wire at light condition increased
slightly and became more positive than at dark
condition. This was due to the H2, which was
evolved due to the photodecomposition of water
into H2 and O2 at the Cu2O/electrolyte interface,
oxidised at the WE surface. Indirect
decomposition of water under visible light
irradiation consisted of two reactions. They were
either oxidation of water and H2 evolution or
water reduction and oxidation of hydroxyl [5,17].
Since the Cu2O sample did not connect to the cell,
therefore the H2 evolution (reduction reaction)
could occur on the Cu2O surface and O2 evolution
thought to be occurred on the copper surface.
Then, H2 and O2 gases tend toward the Pt surface
(WE) that was subjected to applied potential at
which oxidation of H2 and reduction of O2
occurred (i.e. O2 reacted with H2 to produce H2O
on Pt surface). In this case the current density of
the Pt should be not changing. This was because
the net current density of the Pt (WE) should be
zero (i.e. current density of O2 reduction = current
density of the oxidation of the H2). However, the
current density of Pt increased towered the anodic
region. This indicated that the reactions that took
place on the copper sample under light condition
were oxidation of copper by water (i.e. corrosion
of copper) and H2 evolution on the Cu2O surface
[2,12,13].
Conclusion
The conclusion of this study can be summarised
in the following points:
1. The current density of either Cu2O or Cu2S
increases suddenly toward the cathodic
region at switching light on. This means
that H2 evolution due to
photoelectrochemical splitting of water at
a p-type semiconductor/electrolyte surface
thought to be occurring.
2. Hydrogen evolution on the Cu2O surface,
which was formed on the clean copper
surface by anodic polarisation method,
was detected and the oxygen that was
produced could react with copper.
3. The lifetime of the effect of visible light
irradiation on the current density of either
Cu2O or Cu2S is about a few seconds.
6
 The First National Conference for Engineering Sciences FNCES'12 / November 7-8, 2012
4. The rate of hydrogen evolution, i.e. current
density, on either Cu2O or Cu2S surface at
switching light on is function of the area of
the excited system, i.e. the thickness of the
Cu2O and Cu2S.
5. Concentration of H2 that is evolved by
photoelectrochemical decomposition of
water at either Cu2O or Cu2S/electrolyte
interface was higher than its solubility in
the water at pH 2 4.935x10-7 atm.
Therefore, hydrogen gas can be detected
by using any technique such as gas
chromatographic technique, solid
electrolyte probe technique, and
polarisation method.
6. Decomposition of water into H2 and O2 at
p-type semiconductor surface of Cu2O
under visible light is influenced by the
band gap energy of copper oxide that was
present on the clean copper sample, and
partial pressure of O2 in the system.
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 The First National Conference for Engineering Sciences FNCES'12 / November 7-8, 2012
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