The effect of water content on the electropolishing behavior of Inconel 718 alloy

in perchloricacetic acid mixtures

Ching An Huang
*
, Yu Chen Chen
Department of Mechanical Engineering, Chang Gung University, Taoyuan 333, Taiwan
a r t i c l e i n f o
Article history:
Received 6 August 2008
Accepted 26 March 2009
Available online 28 May 2009
Keywords:
A. Inconel 718 alloy
B. Electropolishing
C. Electron beam welding
Perchloric and acetic acid mixture
a b s t r a c t
The electropolishing behavior of Inconel 718 alloy was studied in perchloricacetic acid mixtures using a
rotating disc electrode. The electropolishing behavior of an Inconel 718 weld, which was prepared with
electron beam welding, was also investigated. A leveled but not brightened surface can be achieved when
Inconel 718 alloy is potentiostatically polished in the acid mixture with 20 vol.% perchloric acid. Interest-
ingly, a brightening effect could be obtained in this acid mixture by adding 1050 ml l
1
water or by
being at rest at room temperature for several days. When electropolishing in acid mixture with
40 vol.% perchloric acid, leveling and brightening of the Inconel 718 surface can be detected. When elec-
tropolished in this acid mixture, the fusion zone of the Inconel 718 weld cannot be leveled together with
its nearby base metal. Nevertheless, a good polished surface of the Inconel 718 weld can be achieved with
the acid mixture with 20 vol.% perchloric acid by adding 40 ml l
1
of water. Electropolishing was per-
formed in the limiting diffusion current region where the transport of water to the anode seemed to
be the rate-determining process.
2009 Elsevier Ltd. All rights reserved.
1. Introduction
Inconel 718 alloy is one of the most widely used Ni-based
superalloys due to its superior mechanical properties and corro-
sion resistance at high temperatures. Therefore, Inconel 718 alloy
is often used in the fabrication of components that require a high
thermal resistance, such as gas turbine engines and blades, and
combustion chambers [15]. It is well known that the fatigue
strength or even the corrosion resistance of an alloy can be im-
proved through electropolishing (EP) [6,7]. It is generally believed
that welding with a relatively low heat input, such as electron
beam welding (EBW), is suitable to join Inconel 718 parts without
a great loss in mechanical properties [8]. In an electron beam (EB)
weld, the fusion zone and heat-affected zone (FZ and HAZ) have
different phases or grain structures from those in the base metal
(BM). Therefore, the leveling and brightening effect on the FZ,
HAZ and BM in a weld is dissimilar. In this study, the EP behavior
of an EB-welded Inconel 718 specimen in perchloricacetic acid
mixtures is also investigated.
Normally, EP on a metallic component could be performed by
anodic dissolution under a mass-transfer-controlled mechanism
in a suitable electrolyte [915]. That is, EP on a metallic component
is carried out by polarizing it at a potential located in the limiting-
current plateau of its anodic polarization curve. Regardless of the
different phases, grain types, and crystalline imperfections in a
metallic component, leveling and brightening of the surface can
be obtained by EP. It is generally accepted that the chemical spe-
cies governing the mass-transfer-controlled mechanism depends
signicantly on both the metallic electrode and electrolyte
[13,16,17].
The commonly used solutions for EP are composed of one or
more concentrated acids, such as perchloric, sulfuric, phosphoric
and acetic acids [13,16]. The EP behavior of a metallic component
can be markedly affected by adding a small amount of H
2
O to the
EP solution. Water added would combine with dissolving cations
or act as an oxidant during EP [13,18]. Electropolishing is generally
performed in the potential region where the limiting diffusion cur-
rent is observed. If the diffusion of H
2
O to the anode is the rate-
determining process, the limiting diffusion current should increase
with increasing H
2
O content in the electropolishing solution. In
this work, the EP behavior of as-rolled and EB-welded Inconel
718 specimens in the perchloricacetic acid mixtures is investi-
gated by using a rotating disc electrode (RDE). Meanwhile, the ef-
fect of adding H
2
O to the acid mixture with 20 vol.% HClO
4
on the
EP behavior of Inconel 718 alloy is also studied.
2. Experimental procedure
An as-rolled Inconel 718 sheet with dimensions 120
40 3 mm
3
was used in this study, and its chemical composition
is given in Table 1. Disc-type specimens with a diameter of 6 mm
were cut from the as-rolled Inconel 718 sheet by wire electrical
discharge machining to a make rotating disc electrode (RDE) with
0010-938X/$ - see front matter 2009 Elsevier Ltd. All rights reserved.
doi:10.1016/j.corsci.2009.03.039
* Corresponding author. Tel.: +886 3 2118800x5346; fax: +886 3 2118050.
E-mail address: gfehu@mail.cgu.edu.tw (C.A. Huang).
Corrosion Science 51 (2009) 19011906
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an exposed area of 0.28 cm
2
. The disc specimen cut from the Inco-
nel 718 sheet was tightly embedded with M-bond epoxy (M-bond
610 ADHESIVE KID, Measurement Group Inc., USA) in a polypropyl-
ene sleeve and connected to the spindle of the RDE-cell kid (EG&G
Model 616) with a exible spring and a stainless steel bar. The RDE
was used for electropolishing and electrochemical tests. The rotat-
ing speed of RDE was kept constant to be 1000 rpm during electro-
polishing and electrochemical test. The RDE surface was
mechanically ground with 600 grit emery paper, cleaned with dis-
tilled water, dried with a cold air blow dryer, and then prepared for
electropolishing and electrochemical tests.
In this work, the EP behavior of Inconel 718 alloy after EBW was
also studied. The EB-welded Inconel 718 specimen was joined by
two welding processes, as given in Table 2, in which penetration
welding was used to join two Inconel 718 plates in the rst process
and then cosmetic welding was performed to trim surface under-
cut in the second process. As shown in Fig. 1, an EB-welded speci-
men with a disc shape was mounted in a polypropylene sleeve and
shaped to be a RDE. The welded portions, including FZ, HAZ, and
BM, were electropolished at the same time. Therefore, the EP
behavior of the EB-welded Inconel 718 specimen can be evaluated
by investigating its surface morphology after electropolishing in
the acid mixtures.
Electropolishing and electrochemical tests were conducted at
27 + 1 C in an electrochemical three-electrode cell with potentio-
stat/galvanostat (EG&G Model 2263A). As mentioned above, the
RDE made of Inconel 718 was used as the working electrode. A
platinum plate with an exposed area of 1 cm
2
was used as the
counter electrode and set parallel to the working electrode with
a distance of 1 cm. The Ag/AgCl electrode in the saturated KCl solu-
tion was used as the reference electrode. The anodic polarization
curve of the RDE specimens was measured potentiodynamically
with a scan rate of 5 mV/s, from 250 mV (vs. open circuit poten-
tial) to 9 V (vs. Ag/AgCl
sat.
). Concentrated perchloric acid (70 wt.%)
and acetic acid (99.7 wt.%) in analytical grade were mixed in vari-
ous volume ratios for electrochemical polishing and testing.
According to the anodic polarization behavior, the potential range
corresponding to the limiting-current plateau was determined, and
EP was conducted in this range.
After EP, the RDE was cleaned with distilled water, ultrasoni-
cally cleaned in ethanol for 5 min, dried with a cold air blaster,
and then examined with an optical microscope (OM, Olympus
BH2-UMA) and a surface proler (Hommel Werk Model T2000).
3. Results and discussion
3.1. Potentiostatic etching in the limiting-current plateau
Fig. 2 shows the anodic polarization curves of the Inconel 718
RDE in acid mixtures with 20 and 40 vol.% HClO
4
. It can be seen
that a limiting-current plateau was detected when the anodic po-
tential was higher than 4.2 V in the acid mixture with 20 vol.%
HClO
4
. The limiting-current plateau in the acid mixture with
40 vol.% HClO
4
was found in a potential range between 3.5 and
4.5 V. According to the anodic polarization curves shown in
Fig. 2, potentiostatic etching was conducted at 7 V in the acid mix-
ture with 20 vol.% HClO
4
, and at 4 V with 40 vol.% HClO
4
. After
potentiostatic etching, the surface morphologies of Inconel 718
were studied and are presented in Figs. 3(a) and (b). Leveling with-
out brightening of the Inconel 718 surface was observed for the
specimen that was potentiostatically etched in the acid mixture
with 20 vol.% HClO
4
; on the other hand, a well electropolished sur-
face, that is, a leveled and brightened surface, can be obtained in
the acid mixture with 40 vol.% HClO
4
.
As shown in Fig. 4, leveling and brightening of the surface can be
achieved when the Inconel 718 RDE is potentiostatically etched in
acidmixturewith20 vol.%HClO
4
after beingat rest for about 10 days
at roomtemperature. That is, thereis anagingeffect for theacidmix-
turewith20 vol.%HClO
4
ontheEPbehavior of theInconel 718RDE. It
implies that the acid mixture with 20 vol.% HClO
4
gradually changes
its chemical reactivity. Fromtheanodic polarizationcurves shownin
Fig. 5, the limiting-current density measured in the aged acid mix-
ture with 20 vol.% HClO
4
is obviously higher than that in the as-pre-
pared one. The aging effect of the acid mixture with 20 vol.% HClO
4
on the EP behavior could be resulted from the decomposition of
HClO
4
with a high oxidation capacity in the acid mixture.
3.2. The EP behavior in the acid mixture with 20 vol.% HClO
4
with
different amounts of H
2
O added
Fig. 6 shows the anodic polarization curves of the Inconel 718
RDE in the acid mixture with 20 vol.% HClO
4
with the H
2
O added,
from 2 to 80 ml l
1
. The anodic polarization curve obtained from
the aged acid mixture is also presented. Obviously, the limiting-
current density increases, and the threshold potential for the lim-
iting-current plateau shifts toward more active potential with
increasing H
2
O concentration in the acid mixture with 20 vol.%
HClO
4
. As expected, a similar anodic polarization effect for the acid
mixture with 20 vol.% HClO
4
being at rest for ca. 10 days on the
anodic polarization behavior was observed.
Table 1
The chemical composition of the as-rolled Inconel 718 sheet used in this study.
Element Ni Fe Cr Nb Mo Ti Al Mn Co Si
wt.% bal. 19.5 17.65 5.14 2.94 0.99 0.60 0.1 0.14 0.15
Table 2
The welding schedule for EBW used in this study.
Welding
schedule
Voltage
(kV)
Current
(mA)
Focus depth
(mm)
Feed rate
(mm/min)
Heat input
(J/mm)
Penetration 50 55 3.45 1016 162
Cosmetic 50 100 3.46 2173 138
Fig. 1. Schematic of the RDE specimen of an Inconel 718 weld.
1902 C.A. Huang, Y.C. Chen/ Corrosion Science 51 (2009) 19011906
By electropolishing in the acid mixture with 20 vol.% HClO
4
, lev-
eling without brightening of the Inconel 718 surface was achieved,
with a granular surface morphology [see Fig. 3(a)]. Fig. 7(a)(e)
shows optical micrographs of the surface morphologies of Inconel
Fig. 3. Surface morphologies of Inconel 718 alloy potentiostatically polished in acid mixtures with (a) 20 and (b) 40 vol.% HClO
4
.
Fig. 4. Surface morphology of Inconel 718 alloy potentiostatically etched in the acid
mixture with 20 vol.% HClO
4
being at rest for ca. 10 days.
0 2 4 6 8
-0.01
0.00
0.01
0.02
0.03
0.04
0.05
0.06
C
u
r
r
e
n
t

d
e
n
s
i
t
y

(
A
c
m
-
2
)
Potential (V vs. Ag/AgCl sat.)
as-prepared
being at resr for ca. ten days
Fig. 5. The anodic polarization curves of Inconel 718 in the as-prepared acid
mixture with 20 vol.% HClO
4
and in the acid mixture being at rest for ca. 10 days.
0 2 4 6 8 10
0.00
0.01
0.02
0.03
0.04
0.05
0.06
C
u
r
r
e
n
t

d
e
n
s
i
t
y

(
A

c
m
-
2
)
Potential (V vs. Ag/AgCl
sat.
)
20 vol.% HClO
4
40 vol.% HClO
4
Fig. 2. The anodic polarization curves of Inconel 718 alloy in the acid mixtures with 20 and 40 vol.% HClO
4
.
C.A. Huang, Y.C. Chen/ Corrosion Science 51 (2009) 19011906 1903
0 2 4 6 8 10
0.00
0.02
0.04
0.06
0.08
0.10
0.12
C
u
r
r
e
n
t

d
e
n
s
i
t
y

(
A

c
m
-
2
)
Potential (V vs.Ag/AgCl
sat.
)
20 vol% HClO
4
+
6 ml l
-1
H
2
O
10 ml l
-1
H
2
O
20 ml l
-1
H
2
O
40 ml l
-1
H
2
O
80 ml l
-1
H
2
O
being at rest for ca. ten days
Fig. 6. The anodic polarization curves of Inconel 718 alloy in the acid mixture with 20 vol.% HClO
4
containing different amounts of H
2
O added.
Fig. 7. The surface morphologies of Inconel 718 alloy potentiostatically etched in the acid mixture with 20 vol.% HClO
4
containing (a) 4, (b) 6, (c) 10, (d) 40 and (e) 80 ml l
1
H
2
O added.
1904 C.A. Huang, Y.C. Chen/ Corrosion Science 51 (2009) 19011906
718 potentiostatically etched in the acid mixture with 20 vol.%
HClO
4
containing different H
2
O concentrations. Obviously, the EP
behavior of Inconel 718 alloy is signicantly affected by the amount
of H
2
Oadded to the acid mixture with 20 vol.% HClO
4
. By increasing
the H
2
Oconcentrationfrom4 to 10 ml l
1
, the granular surface mor-
phology was gradually diminished and replaced by a leveled and
brightenedsurface, as shownin Fig. 7(a)(c). Very small precipitates
ina needle formwere not leveledtogether withthe nearby substrate
when electropolished in the acid mixture with a H
2
O concentration
lower than 6 ml l
1
. Addition of 410 ml l
1
H
2
Oto the acid mixture
with 20 vol.% HClO
4
enhances the EP effect on the Inconel 718 alloy.
As presentedinFig. 7(c) and(d), brighteningandlevelingthesurface,
that is, producing a well polished surface of Inconel 718 RDE can be
achievedby electropolishing inthe acidmixture with20 vol.%HClO
4
containing H
2
O added from 10 to 50 ml l
1
. In Table 3, the surface
roughness values, R
a
, of electropolished surfaces are lower than
0.03 lm, which is a reasonable value for the metallic surface rough-
ness after EP as reported by many researchers [17,18]. However,
increasing the H
2
O concentration higher than 60 ml l
1
in the acid
mixture with 20 vol.% HClO
4
leads to small precipitates in a needle
form that were clearly observed on the surface after EP [see
Fig. 7(e)]; that is, these precipitates can not be leveled together with
the Inconel 718 substrate. Thus, electropolishing in these acid mix-
tures, the surfaceroughness values, R
a
, increase slightlyor are higher
than0.03 lm. Some tiny white stains couldbe seenvisually onthese
polished surfaces after EP.
As shown in Fig. 6, increasing water content in 20 vol.% HClO
4
acid mixture increases the limiting diffusion current. This suggests
that the transport of water to the anode surface is the rate-deter-
mining process. Thus, for leveling and brightening of the surface,
the optimal rate of water transport, that is, the optimal concentra-
tion of water such as 1050 ml l
1
in 20 vol.% HClO
4
CH
3
COOH
mixture is required.
3.3. The EP effect on an Inconel 718 alloy after EBW
According to our experimental results, a well polished surface of
Inconel 718 alloy can be achieved by potentiostatic polishing in
three kinds of acid mixtures; that is, the acid mixture with
40 vol.% HClO
4
, the acid mixture with 20 vol.% HClO
4
aged for ca.
10 days, and the acid mixture with 20 vol.% HClO
4
with 10
50 ml l
1
H
2
O added. As shown in Fig. 1, an EB-welded RDE speci-
men was prepared to evaluate its EP behavior in the three kinds of
acid mixtures mentioned above.
Fig. 8(a) and (b) shows the surface morphologies of EB-welded
Inconel 718 specimens after EP in the acid mixtures with 20 and
40 vol.% HClO
4
, respectively. As expected, the BM region in the
EB-welded specimen was leveled and brightened in the acid mix-
ture with 40 vol.% HClO
4
, but not leveled and brightened in the acid
mixture with 20 vol.% HClO
4
. Contrary to the EP effect on the BM
region, the FZ in EB-welded specimen was not well electropolished
in either of these acid mixtures. As shown in Fig. 8(b), an obvious
surface step between the FZ and BM can be seen after EP. This indi-
cates that the anodic dissolution rates between the FZ and BMof an
EB-welded Inconel 718 specimen are different. As shown in
Fig. 9(a) and (b), leveling and brightening of the surface of EB-
Table 3
The surface roughness, R
a
, of Inconel 718 alloy polished in the acid mixture with 20 vol.% HClO
4
containing different H
2
O concentrations.
H
2
O content (ml l
1
) 0 2 6 10 20 30 40 50 60 70 80
R
a
(lm) 0.19 0.12 0.04 0.02 0.02 0.01 0.01 0.02 0.05 0.07 0.08
Fig. 8. Surface morphologies of EB-welded Inconel 718 specimens after electropolishing in acid mixtures with (a) 20 vol.% and (b) 40 vol.% HClO
4
.
Fig. 9. Surface morphologies of EB-welded Inconel 718 specimens after electropolishing in acid mixtures with 20 vol.% HClO
4
(a) being at rest for ca. 10 days and (b) with
40 ml l
1
H
2
O added.
C.A. Huang, Y.C. Chen/ Corrosion Science 51 (2009) 19011906 1905
welded Inconel 718 specimen could be achieved when electropo-
lished in the 20 vol.% HClO
4
acid mixture aged for ca. 10 days or
with 40 ml l
1
H
2
O added. These results indicate that the afore-
mentioned acid mixtures are suitable for obtaining a well polished
surface of Inconel 718 alloy after EBW regardless of the different
grain types or phases among the FZ, HAZ and BM in a weld. This
means that EP of an Inconel 718 weld depends strongly on the
electrolyte used.
4. Conclusions
The electropolishing behavior of Inconel 718 alloy and Inconel
718 weld was studied in HClO
4
CH
3
COOH acid mixtures using a
rotating disc electrode. From the experimental results, a leveled
surface without brightening could be achieved when Inconel 718
alloy was potentiostatically polished in the acid mixture with
20 vol.% HClO
4
. But a brightening effect could be observed when
electropolishing in this acid mixture being at rest for ca. 10 days
at roomtemperature or with 1050 ml l
1
H
2
O added. The increase
in the water content of 20 vol.% HClO
4
solutions resulted in the in-
crease in limiting diffusion current. This fact indicates that the
transport of water to the anode is rate-determining process in elec-
tropolishing. By electropolishing in the acid mixture with 40 vol.%
HClO
4
, leveling and brightening of the surface can be detected in
the base metal of the Inconel 718 weld, but the fusion zone cannot
be leveled together with the base metal. Nevertheless, a well pol-
ished surface for the Inconel 718 weld can be achieved in the acid
mixture with 20 vol.% HClO
4
containing 40 ml l
1
H
2
O added.
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