Journal of Manufacturing Processes 58 (2020) 1257–1269

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Journal of Manufacturing Processes

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Eco-friendly NaCl-based electrolyte for electropolishing 316L stainless steel

Wei Han a, Fengzhou Fang a, b, *
a
Centre of Micro/Nano Manufacturing Technology (MNMT-Dublin), University College Dublin, Dublin 4, Ireland
b
State Key Laboratory of Precision Measuring Technology and Instruments, Centre of Micro/Nano Manufacturing Technology (MNMT), Tianjin University, Tianjin
300072, China

A R T I C L E I N F O A B S T R A C T

Keywords: Since the environmental and safety issues closely related to the widely used mixture electrolytes of H2SO4 and
Electropolishing H3PO4 in electropolishing 316 L stainless steel, the development of new electrolytes, which do not contain any
316L stainless steel acid is of a great demand. This study is to electropolish 316 L stainless steel in a NaCl-based electrolyte, not
NaCl-based electrolyte
containing any acid as the conventionally used electrolytes. The electropolishing effect with the NaCl-based
Surface roughness
electrolyte is compared with the conventional H2SO4-based electrolyte. The experimental results show that
the proposed electrolyte can be used for the electropolishing of 316 L stainless steel to obtain a comparable
electropolishing effect with the conventional H2SO4-based electrolyte. Moreover, the NaCl-based electrolyte
shows a higher material removal rate than the H2SO4-based electrolyte. It is also found that a brown product
generated and covered on the anode electrode surface during the electropolishing with the NaCl-based elec­
trolyte. According to the EDS analysis, it mainly contains dissolved metal elements, Cl and Na element from the
used electrolyte. Furthermore, the electropolishing effect can be improved by the ethanol addition in the NaCl-
based electrolyte due to the reduced influence of the brown product.

1. Introduction the applications of biomedical materials [7,8]. Corrosion resistance

strongly depends on the metal surface, and the electropolishing removes
316L stainless steel has an excellent corrosion resistance in severely the outermost damaged surface layer caused by previous machining
corrosive environments, such as sea water, acidic and alkaline media, processes and creates a new thicker oxide film layer, resulting in
hence, it is widely used in marine, biomedical equipment, chemical and improved corrosion resistance. Electropolishing is usually carried out in
petrochemical plants [1]. In the processing of 316 L stainless steel, the concentrated acid electrolytes, such as phosphoric acid, sulfuric acid,
metal surface comes with much contamination and quite coarse by the perchloric acid and their mixtures, according to the workpiece materials
rough machining. This could lead to greater friction, substantial toler­ [8]. Methanol [9], glycerol [10], and glacial acetic acid [11] are often
ances and even a source of fatigue crack [2,3]. Therefore, a used as the solvents instead of water in an electropolishing electrolyte.
post-polishing procedure works as a critical process in industrial pro­ However, considering the environmental and safety issues related to the
duction to avoid these problems. widely used acid-based electrolytes for electropolishing, developing new
Mechanical polishing is widely used in industry for various types of eco-friendly and safety polishing electrolytes with a high surface quality
metal materials. However, a damaged surface layer is usually generated is of a high demand. For the electropolishing of 316 L stainless steel, the
on the metal surface after the mechanical polishing due to the contact mixture solutions of sulfuric acid and orthophosphoric acid are normally
force between the workpiece and tool. Such a damaged surface layer has used as the electrolytes [12,13], and perchloric acid can also be used
a deformed structure and contains a lot of structural defects and other [14,15]. On the other hand, for the electropolishing of titanium, Degu­
imperfections, which increase the electrochemical activity and decrease chi et al. [16] proposed an electropolishing procedure using an elec­
the corrosion resistance of metals [4–6]. Comparing with the conven­ trolyte solution with the composition of ethylene glycol solution and
tional mechanical polishing technology, electropolishing is a NaCl. Fushimi et al. [17,18] investigated the anodic dissolution behav­
damage-free process, moreover, the corrosion resistance of metals can iour of titanium in the NaCl-based electrolyte with a rotating disk
be improved by the electropolishing, which is especially important for electrode. However, there was not any reported research on the

* Corresponding author at: Centre of Micro/Nano manufacturing Technology (MNMT-Dublin), University College Dublin, Dublin 4, Ireland.
E-mail address: [email protected] (F. Fang).

https://doi.org/10.1016/j.jmapro.2020.09.036
Received 19 December 2019; Received in revised form 8 September 2020; Accepted 14 September 2020
Available online 23 September 2020
1526-6125/© 2020 The Authors. Published by Elsevier Ltd on behalf of The Society of Manufacturing Engineers. This is an open access article under the CC BY
license (http://creativecommons.org/licenses/by/4.0/).
W. Han and F. Fang Journal of Manufacturing Processes 58 (2020) 1257–1269

Table 1
Conventional electrolyte composition for the electropolishing of 316 L stainless
steel.
NO. Electrolyte Ref. NO. Electrolyte composition Ref.
composition

1 a) 85 % H3PO4:93% Ref 2 Mixture of H2SO4 and Ref

H2SO4 = 7:3 (v:v) [19] H3PO4 [20,
b) 100 mL methanol, 21]
300 mL 93% H2SO4
3 45% H3PO4, 35% Ref 4 H3PO4 + H2SO4 + DI Ref
H2SO4 and 20% H2O [22] water [23,
24]
5 80 vol% HClO4 Ref 6 60 vol% H3PO4 (85 wt Ref
Fig. 1. Experimental setup for the electropolishing and electro­ (70 wt%), 20 vol% [14] %), 20 vol% H2SO4 [12]
chemical analysis. glacial acetic acid (95–97 wt%), 10 vol%
(98 wt%) glycerol (99.5 wt%) and
10 vol% DI water
electropolishing of 316 L stainless steel in the NaCl-based electrolyte. 7 Mixture of H2SO4 Ref 8 Mixture of H3PO4 + Ref
In this study, the electropolishing effects with the NaCl-based elec­ and H3PO4 [25, H2SO4 with volume [27]
trolyte, which consists of the ethylene glycol solution containing NaCl in 26] ratios of 1:1, 2:1 and 3:1
the concentration of 1 M, and the H2SO4-based electrolyte, which con­ 9 H3PO4:H2SO4 = 1:4 Ref 10 H2SO4 solution Ref
and 4:1 [28] [29]
sists of the sulfuric acid (98 %), phosphoric acid (81 %) and glycerol 11 H3PO4, H2SO4, Ref 12 H3PO4 (60% v/v) and Ref
with the volume ratio of 5:4:1, were compared with different electrolyte glycerol and DI [30] H2SO4 (40% v/v) [13]
temperatures. The electropolished surfaces and material removal rates water
were compared with different types of electrolyte. Then, the electro­ 13 10 % H2O and Ref 14 45% H3PO4, 35% H2SO4, Ref
H3PO4:H2SO4 = 3:2 [31] and 20% water [32]
polishing effect with the NaCl-containing electrolyte was further stud­
ied, and a brown product was found to be generated in the vicinity of the
anode surface. The brown product deteriorated the electropolishing ef­ used to heat the electrolyte and cooperated with a thermal sensor to
fect by interrupting the diffusion of the dissolved metal ions into the control the electrolyte temperature. A magnetic stir bar was used to stir
bulk electrolyte and the fresh electrolyte towards to the anode surface, the electrolyte with the stirrer speed range of 100–2000 rpm. The po­
therefore, the composition of the brown product was analysed. larization curves were measured by sweeping the potential from 0 V to
Furthermore, the ethanol solution was added into the NaCl-based elec­ 3 V or 9.5 V (vs Ag/AgCl) for different electrolytes at a scan rate of
trolyte to reduce the influences of the brown product, and the experi­ 20 mV/s. To get reliable repeatability, all the tests were repeated three
mental results showed that the electropolishing effect was improved times under the same conditions.
efficiently by the ethanol addition.
2.3. Surface analyses
2. Experimental approaches
The surface morphology was characterized using KEYENCE VHX-
2.1. Material and solution 5000 digital microscope. The surface topography was measured by a
non-contact optical profile (NPFLEX), and all the surface roughness in
The 316 L stainless steel samples with a size of this study was measured in a surface area of 439 μm × 332 μm after the
10 mm × 20 mm × 0.5 mm were used throughout the experiments. The processes of the tilt removal and gaussian regression filter with the short
polishing side was uniformly ground with 600 grit abrasive sandpaper to wavelength cutoff of 0.025 mm. Each electropolished surface was
remove the original oxide film and improve the reactivity. Most surfaces measured at five different positions to get high reliability of surface
of the sample were covered by a nonconductive adhesive tape only evaluation, and the presented surface topographies were selected due to
exposing the electropolishing surface area of 5 mm × 5 mm. After elec­ the high representative. The element components were characterized by
tropolishing, the samples were cleaned using distilled water and ethanol a field-emission scanning electron microscope (FE-SEM).
in sequence in an ultrasonic agitation bath for 3 min. and dried by air
blowing. The NaCl-based electrolyte used was the pure ethylene glycol 3. Comparison of electropolishing effects with different types of
solution containing NaCl in the concentration of 1 M. The ethanol so­ electrolyte
lution of 90 % in volume concentration was used as an additive in the
electrolyte. The H2SO4-based electrolyte was composed of sulfuric acid For the electropolishing of 316 L stainless steel, the mixture elec­
(98 %), phosphoric acid (81 %) and pure glycerol with the volume ratio trolytes of H2SO4 and H3PO4 were normally used, as shown in Table 1. A
of 5:4:1. typical H2SO4-based electrolyte composed of the sulfuric acid (98 %),
phosphoric acid (81 %) and glycerol with the volume ratio of 5:4:1 was
2.2. Electropolishing and electrochemical analysis used to be compared with the NaCl-based electrolyte, and the purpose is
to find an alternative electrolyte of the conventionally used mixture
The electropolishing was performed in a traditional three-electrode electrolytes of H2SO4 and H3PO4 considering the environmental and
cell consisting of a reference electrode of Ag/AgCl reference element safety issues.
surrounded by an electrolyte of 4 M KCl solution saturated with AgCl, a
counter electrode of titanium mesh with the size of 200 mm × 400 mm 3.1. Electropolishing effect at ambient temperature
and an anode electrode (316 L stainless steel workpiece). The inter-
electrode gap width between the anode and counter electrode was set Fig. 2 shows the polarization curves measured in the different elec­
as 10 mm which is maintained by drilling two holes on an acrylic plate trolytes with different stirrer speeds. With the H2SO4-based electrolyte,
with the distance of 10 mm. Fig. 1 shows the experimental setup. A the polarization curves show a passivation region in the applied po­
potentiostat/galvanostat CS310 was used to supply the applied potential tential range from 0 V to 1.32 V, as shown in Fig. 2(a), because an air-
between electrodes and also used for the electrochemical analysis, formed oxide film was covered on the anode surface even if the sam­
which was controlled by commercial software. The hotplate stirrer was ples were ground with a sandpaper before the electropolishing. An

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Fig. 2. Polarization curves measured in the (a) H2SO4-based electrolyte and (b) NaCl-based electrolyte at ambient temperature with different stirrer speeds. The scan
rate was 20 mV/s, and the potential ranges were 0 V to 3 V and 0 V to 9.5 V for (a) and (b), respectively.

active anodic dissolution was initiated from the potential of 1.32 V, and the increase of the current density.
the current density increased dramatically by increasing the applied With the NaCl-based electrolyte, the current density was also
potential in the potential range of 1.32 V to 1.6 V. This region is also increased with increasing the stirrer speed, as shown in Fig. 2(b), due to
defined as the etching region in the electropolishing [8], and pitting the same reason as Fig. 2(a). It is noted that small current density peaks
corrosion generates on the anode surface normally. Then, a peak was appeared at the applied potential range of 1.2 V to 1.5 V with the stirrer
observed at the applied potential of 1.6 ± 0.5 V, and the current density speed lower than 667 rpm, and they disappeared with increasing the
decreased with increasing the potential in the potential range of stirrer speed. It is considered that this is mainly caused by a brown re­
1.6 ± 0.5 V to 1.8 V. This is because a new passivate oxide film was action product generated in the vicinity of the anode surface, and it
generated on the anode surface, resulting in a decrease in the current could be observed clearly by naked eyes during electropolishing. Fush­
density. A narrow limiting current density plateau region, in which the imi et al. [17,18] measured the polarization curve of titanium in the
best electropolishing effect can be obtained [33,34], was observed after NaCl-based solution and reported that the current density decreased
the passivation region. The current density was constant with increasing gradually when the electrolyte colour in the vicinity of the anode surface
the applied potential in this region because a compact salt film layer [35, changed to brown. They thought that the brown product was due to the
36] or an adsorbate acceptor layer [35,37] was formed on the anode dissolution of the air-formed oxide film on the anode surface and the
surface. The thickness of the salt film layer or adsorbate acceptor layer following anodic dissolution of the titanium. It is considered that the
changes with increasing the applied potential, resulting in the constant first current density peaks at the applied potential range of 1.2 V to 1.5 V
current density. The mass transport in the limiting current density with the stirrer speeds lower than 667 rpm, as shown in Fig. 2(b), was
plateau region was limited, and the mechanism could be the salt film mainly caused by the brown product because the inter-electrode gap
model or adsorbate acceptor model, which was not investigated in this resistance was increased when the brown product was generated and
study. Then, the current density increased dramatically with increasing covered on the anode surface, and the composition of it was studied in
the applied potential to the higher magnitude than 1.8 V, and this region the following section. Besides, the current density peak disappeared
was nominated as the gas evolution region [8]. Oxygen gas bubbles were with increasing the stirrer speed because the brown product covered on
generated on the anode surface due to the electrochemical reaction (1), the anode surface was detached with a high stirrer speed, which could
and the gas bubbles could be seen on the anode surface in this region. also be observed directly from the surface colour of the anode electrode.
Moreover, it is noted that the current density peak due to the
4OH − − 4e− →2H2 O + O2 (1)
passivation process with a higher applied potential was shifted from a
A viscous film layer was formed on the anode surface because the lower potential of 3 V to a higher potential of 6 V with increasing the
dissolved metal ions could not diffuse away from the anode surface in stirrer speed, as shown in Fig. 2(b), which indicated that the tendency of
time [38]. The viscous film layer has a gradient in the concentration of the 316 L stainless steel towards passivity was decreased with increasing
the dissolved metal ions, and the concentration was higher on the anode the stirrer speed. This is probably because the anode surface was less
surface and decreased with increasing the distance to the anode surface. protected due to the formation of a porous oxide film, and the critical
Fig. 2 shows that the current density was increased with increasing the dissolving power of the NaCl-based electrolyte on the formed oxide film
stirrer speed mainly due to the influence of the stirring process on the was increased with increasing the stirrer speed [39]. Besides, the current
viscous film layer. The stirred electrolyte increased the diffusion process density oscillation was observed with the stirrer speeds higher than
of the dissolved metal ions into the bulk electrolyte resulted in a thinner 889 rpm because the electrolyte became unstable, and many bubbles
thickness of the viscous film layer, and a smaller inter-electrode gap generated due to the high stirrer speed.
resistance was formed with increasing the stirrer speed, resulting in an To compare the polarization curves with different types of electrolyte
increase in the current density. Moreover, the current density was shown in Fig. 2, a wide passivation region from 0 V to 1.32 V before the
slightly changed with the stirrer speeds of 1111 rpm and 1333 rpm, as active dissolution was observed with the H2SO4-based electrolyte, as
shown in Fig. 2(a), therefore, the stirrer speed has a limited influence on shown in Fig. 2(a). However, the corresponding passivation region was
much narrower with the NaCl-based electrolyte, as shown in Fig. 2(b). It
is known the initial passivation region was due to the air-formed oxide
Table 2 film; hence, the air-formed oxide film has a less stability in the NaCl-
Optimized electropolishing conditions used for different types of electrolyte at based electrolyte, and it would be removed easily with the NaCl-based
ambient temperature. electrolyte. The potential range of the limiting current density plateau
Electropolishing conditions H2SO4-based NaCl-based region with the NaCl-based electrolyte was much wider than the H2SO4-
electrolyte electrolyte based electrolyte. The wider limiting current density plateau region
Applied potential [V vs Ag/ 1.9 6 means a bigger electropolishing potential window to obtain the best
AgCl] electropolishing effect. Besides, the limiting current density was slightly
Stirrer speed [rpm] 889 444 higher with the NaCl-based than the H2SO4-based electrolyte. Therefore,
Electropolishing duration [s] 1200 1200
a higher material removal rate and electropolishing efficiency can be

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Fig. 3. Surface topographies of the electropolished surfaces with (a) the H2SO4-based electrolyte and (b) NaCl-based electrolyte. The electrolyte temperature was
ambient temperature. The stirrer speed and applied potential were 889 rpm and 1.9 V with the H2SO4-based electrolyte and 444 rpm and 6 V with the NaCl-based
electrolyte.

expected with the NaCl-based electrolyte. the original anode surface was covered by many scratches due to the
The optimized electropolishing conditions with different types of previous grinding process and there was no scratch after the electro­
electrolytes could be determined according to the polarization curves polishing, a sufficient electropolishing effect was realized with the
shown in Fig. 2. Since the stability of the limiting current density plateau duration of 1200s for the two types of electrolytes. With the H2SO4-
region and the current density which is of critical importance for the based electrolyte, the electropolished surface was deteriorated by
material removal rate and electropolished surface quality, the optimized pitting corrosion, as shown in Fig. 3(a). With the NaCl-based electrolyte,
electropolishing conditions for the H2SO4-based electrolyte and the there was no pitting corrosion observed on the polished surface, as
NaCl-based electrolyte are shown in Table 2. The electropolishing shown in Fig. 3(b). However, the surface was not smooth enough. It is
duration of 1200s was mainly determined by the H2SO4-based electro­ considered that the electropolished effect was influenced by the gener­
lyte to get a sufficient electropolishing effect because the NaCl-based ated brown product on the anode surface because the stirrer speed of
electrolyte could obtain a sufficient electropolishing effect with a 444 rpm was not high enough to remove the generated brown product
shorter duration than 1200s due to the higher current density shown in from the anode surface. This could be verified by observing the anode
Fig. 2. surface during the electropolishing, and the brown colour in the vicinity
Fig. 3 shows the optical microscope images and surface topographies of the anode surface was distinct. The surface area, which was covered
of the electropolished surfaces with different types of electrolyte. Since by a thick brown product, would have a lower material removal rate due

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Fig. 4. Current density transitions with the applied potentials of 1.3 V and 6 V.
The electrolyte was the NaCl-based electrolyte, and the stirrer speed
was 444 rpm.

Fig. 5. Electropolished surfaces with different applied potentials. The stirrer

speed was 444 rpm, the electropolishing duration was 1200s, and the electro­
lyte was the NaCl-based electrolyte.

to the protective effect, resulting in a rough surface shown in Fig. 3(b).

The surface roughness Sa = 108 nm was lower with the NaCl-based Fig. 6. Contour image of the corrosion pits generated on the electropolished
electrolyte than the Sa = 139 nm with the H2SO4-based electrolyte. surface with the applied potential of 1.3 V and stirrer speed of 444 rpm. The
In addition, Fig. 2(b) shows that current density peaks were observed electrolyte was the NaCl-based electrolyte, and the electrolyte temperature was
ambient temperature.
in the applied potential range of 1.2 V to 1.5 V with the NaCl-based
electrolyte, following a similar limiting current density plateau region.
The electropolishing effect in this region was studied and compared with 1.3 V failed to get an effective electropolishing effect even through the
the limiting current density plateau region in the potential range of 4.5 V polarization curves, as shown in Fig. 2(a), show the similar limiting
to 7 V. Fig. 4 shows the current density transitions with the applied current density plateau regions in the applied potential range of 1.2 V to
potentials of 1.3 V and 6 V, and the electropolishing duration was 1200s. 1.5 V with the lower stirrer speeds than 667 rpm. The result coincides
The current density with the applied potential of 6 V shows a typical with the characteristics of the current density transients shown in Fig. 4
current density transit in electropolishing [34,40]. Upon applying the with the applied potential of 1.3 V, which was different from a typical
constant potential, the current density decreased due to the generation current density transient in an electropolishing. Besides, the results also
of a passive oxide film on the anode surface. Then, the current density confirmed that the initial decrease in the current density with the
reached a stable state, and the generation rate of the passive oxide film applied potential of 1.3 V, as shown in Fig. 4, was more probably caused
was balanced by the dissolution rate. With the applied potential of 1.3 V, by the generated brown product on the anode surface than the passiv­
the current density shows different characteristics. It decreased in the ation of the anode electrode. Moreover, Fig. 6 shows the contour image
initial 30 s upon applying the potential, and the reasons might be the of the corrosion pits generated on the electropolished surface with the
generation of a passive oxide film and/or the generated brown product applied potential of 1.3 V, which shows that the passive oxide layer was
on the anode surface. The decrease duration in the current density was broken at the corrosion pit.
significantly shorter compared with the applied potential of 6 V. Thus,
the current density was in a high possibility that influenced by the 3.2. Electropolishing effect with heated electrolyte
generated brown product. Since the stirrer speed of 444 rpm was not
high enough to remove the brown product covered on the anode surface, With the different types of electrolyte, the electropolished surfaces at
the current density would be decreased at the beginning of the elec­ the ambient temperature, as shown in Fig. 3, was not smooth enough
tropolishing due to the increased inter-electrode resistance. Then, the considering the surface roughness Sa of 139 nm and 108 nm. This might
current density increased dramatically to a higher current density, as be influenced by the low electrolyte temperature because the electro­
shown in Fig. 4, indicating an active dissolution of the anode. polishing effect is closely related to the electrolyte temperature. The
Fig. 5 shows the electropolished surfaces with different applied po­ dependence of the limiting current density on the electrolyte tempera­
tentials of 1.3 V and 6 V, corresponding to the current density transients ture in the electropolishing cell with a rotating-disk electrode can be
shown in Fig. 4. A smooth surface was obtained with the potential of 6 V, calculated as following equation [33].
as shown in Fig. 5(b), indicating that an electropolishing effect was
achieved. The electropolishing effect confirmed the typical current Ea
ilim = k0 exp(－ )Ω1/2 (2)
density transient in electropolishing with the applied potential of 6 V RT
shown in Fig. 4. However, the obtained surface with the applied po­ where, k0 is a constant independent of electrolyte temperature, Ea is the
tential of 1.3 V, as shown in Fig. 5(a), shows that the grain boundaries activation energy, R is the universal gas constant 8.314 J*mol－1 K－1, T
and pitting corrosion were observed clearly. The applied potential of is the electrolyte temperature, Ω is the disk rotation rate. Hence, the

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Fig. 7. Polarization curves measured in the (a) H2SO4-based electrolyte and (b) NaCl-based electrolyte at the electrolyte temperature of 66 ◦ C with different stirrer
speeds. The scan rate was 20 mV/s, and the potential ranges were 0 V to 3 V and 0 V to 9.5 V for (a) and (b), respectively.

Fig. 8. Polarization curve measured with the NaCl-based electrolyte and the
stirrer speed of 889 rpm at the electrolyte temperature of 66 ◦ C. The scan rate
was 20 mV/s, and the potential range was 0 V to 9.5 V.

limiting current density increases with increasing the electrolyte tem­

perature. It is known that a better electropolishing effect can be obtained
normally with a higher current density. Besides, when the H2SO4-based
electrolytes were used in previous researches, Rokosz et al. [28] elec­
tropolished austenitic AISI 304 L and AISI 316 L stainless steel at a high
electrolyte temperature of 65 ◦ C, Kim et al. [24] electropolished L-sha­
ped tube 316 L stainless steel at a electrolyte temperature of 60 ◦ C and ur
Rahman et al. [19] also used a high electrolyte temperature of 60 ◦ C.
Fig. 9. The influences of the electrolyte temperature on the passivation region
Therefore, the electropolishing effects with different types of electrolyte width and the limiting current density plateau region width: (a) Potential
at a high electrolyte temperature of 66 ◦ C were studied and compared widths of the passivation region with the H2SO4-based electrolyte, and (b)
with the ambient electrolyte temperature. Potential width of the limiting current density plateau region with the NaCl-
Fig. 7 shows the polarization curves measured in the H2SO4-based based electrolyte.
electrolyte and NaCl-based electrolyte with different stirrer speeds at the
electrolyte temperature of 66 ◦ C. It is noted the current density was the high temperature limit, and T0 is the Vogel temperature at which all
increased significantly compared with the results measured at the movements of the constituent elements of a liquid are considered to be
ambient temperature shown in Fig. 2. The current density with the totally frozen. Therefore, the appropriately maximum stirrer speed was
H2SO4-based electrolyte was increased by ten times with increasing the decreased with increasing the electrolyte temperature due to a decrease
electrolyte temperature to 66 ◦ C, and it was increased by about five in the electrolyte viscosity. As shown in Fig. 7(a), the current density
times with the NaCl-based electrolyte. The Eq. (2) shows that the obtained with the H2SO4-based electrolyte oscillated with the stirrer
limiting current density is increased with increasing the electrolyte speed of 889 rpm, and the current density was also unstable with the
temperature. The diffusion rates of ions in the electrolyte are mainly NaCl-based electrolyte with the stirrer speed of 889 rpm, as shown in
determined by the electrolyte temperature, diffusing ions, bulk elec­ Fig. 8. Therefore, the available stirrer speeds with different types of
trolyte and concentration differences, and the temperature has the electrolytes were decreased with increasing the electrolyte temperature
greatest effect on the diffusion rates. The ions energy was increased with according to the polarization curves shown in Fig. 2, Figs. 7 and 8.
increasing the electrolyte temperature, and the ions bounced against However, it is noted that the current density was increased with
each other more frequently with higher energy, resulting in a higher increasing the electrolyte temperature by comparing Figs. 2 and 7
diffusion rate. Besides, the electrolyte viscosity was decreased with although the maximum stirrer speed was decreased, this is because the
increasing the electrolyte temperature according to the Vogel-Fulcher- electrolyte temperature has a more dominant effect on the current
Tammann (VFT) equation [41,42]. density than the stirrer speed.
BVFT Moreover, when increasing the electrolyte temperature, the poten­
ln η = AVFT + (3) tial width of the passivation region was narrowed with the H2SO4-based
T − T0
electrolyte, as shown in Fig. 9(a). It indicates that the passivity ability of
where, η is the viscosity, AVFT = ln(η∞) and η∞ is the viscosity value at the anode electrode was reduced with increasing the electrolyte

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Fig. 10. Optical microscope images and surface topographies of the electropolished surfaces with (a) H2SO4-based electrolyte and (b) NaCl-based electrolyte. The
electrolyte temperature was 66 ◦ C. The stirrer speed and applied potential were 444 rpm and 2 V with the H2SO4-based electrolyte and they were 444 rpm and 4.5 V
with the NaCl-based electrolyte.

temperature. Escrivà-Cerdán et al. [43] reported that the passivity of incorporate with the passive oxide film to form a high non-adherent
Alloy 31 was lost as increasing the temperature from 20 ◦ C to 80 ◦ C in porous oxide film [44]. The passive oxide film can be easily removed;
the polluted 40 wt.% H2SO4 (5.5 M) solution. The high electrolyte then, the surface is attacked by the Cl－ ions which may cause pitting
temperature favours the anodic dissolution because the anodic current corrosion. It has been reported that the presence of Cl－ions were closely
density was higher with the high electrolyte temperature, and the related to the generation of pitting corrosion [45–47]. The higher
dissolution of the species in the passive oxide film was increased by electrolyte temperature makes the passive oxide film more porous and
increasing the electrolyte temperature. On the other hand, the potential less protective [48]; therefore, the stability of the limiting current
width of the limiting current density plateau region with the NaCl-based density plateau region was decreased with increasing the electrolyte
electrolyte was narrowed with increasing the electrolyte temperature, as temperature in the NaCl-based electrolyte, resulting in a decrease in the
shown in Fig. 9(b). The generation rate of the passive oxide film on the potential width of the limiting current density plateau region.
anode surface is balanced by the dissolution rate of the passive oxide Fig. 10 shows the optical microscope images and surface topogra­
film in the limiting current density plateau region. When the dissolution phies of the electropolished surfaces with different types of electrolyte at
rate becomes dominant, the balance of the limiting current density the electrolyte temperature of 66 ◦ C. The surface roughness Sa was
plateau region is broken, and the electrochemical process enters the gas 100 nm and 20.4 nm with the H2SO4-based electrolyte and NaCl-based
evolution region. With the NaCl-based electrolyte, the Cl− ions can electrolyte, respectively. It is found that the electropolished surface

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Fig. 11. (a) Current density transients and (b) Material removal rates and
average current densities with different types of electrolyte. The electrolyte
temperature was 66 ◦ C, and the stirrer speed was 444 rpm. The applied po­
tentials were 2 V and 4.5 V for the NaCl-based and H2SO4-based electrolyte, Fig. 12. Images of the brown product generated on the anode surface: (a)
respectively. During electropolishing, (b) After electropolishing and (c) Dried after two
weeks. The applied potential was 3.6 V, the stirrer speed was 0 rpm, and the
was influenced by local flow with the H2SO4-based electrolyte. The electrolyte temperature was 66 ◦ C.
NaCl-based electrolyte also shows a better electropolishing effect at the
ambient electrolyte temperature than the H2SO4-based electrolyte, as sample mass before and after electropolishing with a laboratory elec­
shown in Fig. 3. It can be concluded that a higher electrolyte tempera­ tronic weighing scale, and the weight scale has a high accuracy of
ture is needed for the H2SO4-based electrolyte to get a comparable 0.1 mg. A long electropolishing duration of 2000s was used to get more
electropolishing effect with the NaCl-based electrolyte. It is noted that material removal mass and accurate calculation of material removal
the electropolished surface roughness Sa was decreased from 139 nm rate.
and 108 nm to the 100 nm and 20.4 nm with the H2SO4-based electro­ Fig. 11 shows the current density transients, material removal rates
lyte and NaCl-based electrolyte, respectively, when the electrolyte and average current densities with different types of electrolyte. The
temperature was increased from an ambient temperature to 66 ◦ C. The current density was slightly higher with the NaCl-based electrolyte than
mass transport limitation mechanism in the limiting current density the H2SO4-based electrolyte, which coincides with the polarization
plateau region is closely related to the electrolyte temperature [33]. curves shown in Fig. 7. However, the material removal rate of the NaCl-
When increasing the electrolyte temperature, the diffusion rates of the based electrolyte was twice of the H2SO4-based electrolyte, as shown in
dissolved metal ions on the anode surface was increased, and the solu­ Fig. 11(b). It is known that the material removal rate is higher with a
bilities of the metal ions in the bulk electrolyte were also increased. The higher current density in electropolishing [8]. However, the current
thickness of the viscous film layer was decreased due to the increased density of the NaCl-based electrolyte was just slightly higher than the
diffusion rates of the metal ions and the increased solubilities of the H2SO4-based electrolyte, as shown in Fig. 11. It is considered the much
metal ions in the bulk electrolyte, which results in an improved elec­ higher material removal rate of the NaCl-based electrolyte was mainly
tropolishing effect. Moreover, it is noted that some corrosion pits were due to the higher current efficiency than the H2SO4-based electrolyte. It
generated on the electropolished surface with the NaCl-based electro­ has been reported that the NaCl aqueous solution usually has a signifi­
lyte, as shown in Fig. 10(b). It is thought that the Cl－ ions incorporated cantly high current efficiency near 100 % even with a small current
with the passive oxide film to form a porous oxide film which could be density [49,50]. Its current efficiency possibly exceeds 100 % in some
easily removed. Then, the anode surface was attacked by the pitting case because of an erosion of inert particles from the workpiece [49].
corrosion due to the Cl－ ions. A less influence of pitting corrosion was However, an H2SO4 solution typically has a lower current efficiency
observed with the H2SO4-based electrolyte due to the absence of the Cl－ than 100 % [51,52], especially with a low current density. It was found
ions, as shown in Fig. 10(a). that the current efficiencies of H2SO4 solution with the low current
densities of 0.1 A/cm2, 0.2 A/cm2, 0.25 A/cm2 and 0.3 A/cm2, which are
close to the current density shown in Fig. 11, were lower than 50 % [52].
3.3. Material removal rates with different types of electrolyte
Therefore, it is thought that the higher material removal rate of the
NaCl-based electrolyte shown in Fig. 11 was mainly determined by the
The material removal rates with different types of electrolyte were
higher current efficiency instead of the slightly higher current density.
compared under the electrolyte temperature of 66 ◦ C due to the better
electropolishing effect, as mentioned by the previous sections. The
4. Electropolishing characteristics with the NaCl-based
applied potential and stirrer speed were 2 V and 444 rpm with the
electrolyte
H2SO4-based electrolyte, and they were 4.5 V and 444 rpm with the
NaCl-based electrolyte, which were determined by Fig. 7. The material
The experimental results show that the NaCl-based electrolyte is
removal mass due to the electropolishing was obtained by measuring the

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Fig. 13. SEM image and Energy-dispersive X-ray spectroscopy of the brown product on the anode surface. (b) and (c) are the Energy dispersive X-Ray spectra of
points ‘B’ and ‘C’ marked in (a), and (d) shows the corresponding atomic percentages of the measured elements.

promising to work as an alternative to the H2SO4-based electrolytes for found from the experiment results that there was slight difference in the
the electropolishing of 316 L stainless steel. However, the electro­ surface finish along the vertical direction of workpiece surface even the
polishing process shows that a brown product was generated on the flow velocities are different along the vertical direction due to the
anode surface to deteriorate the electropolishing effect because it in­ changed distances to the stirrer. This is because the electropolishing was
terrupts the diffusion of the dissolved metal ions into the bulk electrolyte conducted at a high electrolyte temperature of 66 ◦ C, and the electro­
and the fresh electrolyte movement towards to the anode surface, polishing temperature played a dominant effect on the surface finish,
especially with a low stirrer speed and low electrolyte temperature. especially compared with the effect of different flow velocities along the
Therefore, the influence of the brown product on the electropolishing vertical direction of the workpiece electrode.
effect was studied, and an ethanol addition was added into the elec­ Fig. 12(b) shows the brown product on the anode surface after the
trolyte to improve the electropolishing effect. electropolishing. The thick brown product can be observed clearly
covering on the anode surface. Fig. 12(c) shows the image of anode
electrode in (b) after placed at the ambient temperature for two weeks
4.1. EDS analysis of the brown product generated on the anode surface
with a cover to prevent contamination, then, the electrolyte on the
workpiece surface has naturally dried, and the solidified brown product
To easily observe the formation of the brown product during the
was left on the anode surface. Fig. 13 shows the SEM image and Energy-
electropolishing and get a thick brown product on the anode surface, the
dispersive X-ray spectroscopy of the brown product on the anode sur­
stirrer speed of 0 rpm was used. The electrolyte temperature was 66 ◦ C,
face. Fig. 13(b) and (c) were the EDS spectra measured from the points
and the applied potential was 3.6 V which was determined according to
‘B’ and ‘C’ marked in Fig. 13(a), respectively, and Fig. 13(d) shows the
the polarization curve shown in Fig. 7(b). Fig. 12 shows the images of
corresponding atomic percentages of the measured elements. The C
the brown product generated on the anode surface under different
element, which was mainly from the contamination, was not considered.
conditions. Fig. 12(a) shows the real electropolishing state, in which a
Fig. 13 shows that the dominant elements were Cl, O, Fe and Na element
brown product generated and covered on the anode surface and
in the brown product. The Cl and Na element were from the NaCl-based
hydrogen gas bubbles generated on the counter electrode surface. Many
electrolyte used in the electropolishing, and the Fe element was from the
bubbles generated from the counter electrode gathers on the top surface
316 L stainless steel. It is considered that the O element was probably
of electrolyte, as shown in Fig. 12(a), and they could cause a low elec­
from the metal oxides, which were generated by the reduction reaction
tropolishing effect on the corresponding workpiece surface due to the
of the Fe, Ni and Cr element during the electropolishing. Moreover, it is
reduced current density. Moreover, the flow velocity of electrolyte due
thought that there were probably some metal chlorides considering that
to stirrer should be different along the vertical direction of workpiece
the atomic percentage of the Cl element was much higher than the Na
surface, and this might cause difference in the surface finish depending
element. In addition, the reaction between ethylene glycol and Fe3+
on the surface is near to or far away from the stirrer. However, it was

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(polarity index = 0.65) is lower than that of ethylene glycol (polarity

index = 0.79). Hence, the solubilities of the Fe3+ and Cl－, which are the
dominant elements in the brown product, as shown in Fig. 13, in the
electrolyte, were increased due to the same mechanism. On the other
hand, the brown product was difficult to be removed from the anode
surface in the ethylene glycol with a low stirring force partly due to the
high viscosity of ethylene glycol. The added ethanol solution, which has
a lower viscosity than the ethylene glycol, decreased the viscosity of the
NaCl-based electrolyte resulted in a less influence of the brown product
on the electropolishing effect.
Fig. 15 shows the electropolished surfaces with the different con­
centrations of ethanol addition and Fig. 16 shows the corresponding
surface roughness Sa. The electropolishing effect was improved with
increasing the concentration of the ethanol addition, and the electro­
polished surfaces with the concentrations of 5.0 % and 10 % show much
smoother surface than the lower concentrations of the ethanol addition.
The surface roughness Sa was decreased from 457 nm to 251 nm by
increasing the concentration of the ethanol addition from 0% to 10 %.
There was less difference in the electropolished surfaces with the con­
centrations of 5.0 % and 10 %, which coincides with the measured po­
larization curves shown in Fig. 14(a). It is considered that the influence
of the brown product was reduced due to the ethanol addition through
increasing the diffusion rate of the contained ions in the brown product
Fig. 14. (a) Polarization curves and (b) Current density transients with into the bulk electrolyte and the fresh electrolyte ions movement toward
different concentrations of ethanol addition in the NaCl-based electrolyte. The to the anode surface.
electrolyte temperature was 66 ◦ C and the stirrer speed was 222 rpm. The scan
rate for the polarization curves was 20 mV/s. 5. Conclusions

nitrate system has been studied by Roşu et al. [53]. A homopolynuclear The NaCl-based electrolyte, which is eco-friendlier than the
compound forms with the formula [Fe(C2O4)(OH)(OH2)]n.0.3nH2O. The conventionally used H2SO4-based electrolytes, is first used to electro­
oxalate anion (C2O2－
4 ) works as ligand and is formed by the following polish 316 L stainless steel successfully. The electropolishing effect of
reaction. the NaCl-based electrolyte was studied and compared with the con­
ventional H2SO4-based electrolyte. The following conclusions can be
3HOCH2CH2OH + 8NO−3 + 2H+ → 3C2O2-
4 +8NO + 10H2O (4) drawn.
It is speculated that the homopolynuclear compound possibly formed
(1) The NaCl-based electrolyte shows a better electropolishing effect
in the electropolishing of 316 L stain steel in the NaCl-based electrolyte
than the H2SO4-based electrolyte at ambient electrolyte temper­
with the Cl－ anion instead of NO－ 3 anion. The [Fe(C2O4)(OH)
ature. It has a wider potential range of the limiting current den­
(OH2)]n.0.3nH2O compound also shows brown colour, and it has
sity plateau region, and a lower surface roughness Sa was
remarkable stability due to the very strong hydrogen bonds between
obtained with the NaCl-based electrolyte than the H2SO4-based
adjacent layers. However, the speculation of the compound formation in
electrolyte.
this study needs more investigation in synthesis.
(2) The NaCl-based electrolyte and H2SO4-based electrolyte show
comparable electropolishing effects at the high electrolyte tem­
4.2. Effect of the ethanol addition on the electropolishing effect perature of 66 ◦ C. The electropolished surface roughness Sa were
20.4 nm and 100 nm for the NaCl-based electrolyte and H2SO4-
The effect of the ethanol addition in the NaCl-based electrolyte on based electrolyte, respectively. However, the electropolished
the electropolishing effect of 316 L stainless steel was studied by surface with the NaCl-based electrolyte was slightly influenced by
changing its volume concentrations at 0%, 2.5 %, 5.0 %, 10 % and 20 %. the pitting corrosion mainly due to the contained Cl－ ions in the
A lower stirrer speed of 222 rpm was used for the easy observation of the electrolyte.
differences in the electropolishing effect due to the influence of the (3) The NaCl-based electrolyte has twice material removal rate of the
brown product because the influences of the brown product were closely H2SO4-based electrolyte, and the reason is considered as the
related to the stirring process. The electrolyte temperature was 66 ◦ C, higher current efficiency of the NaCl-based electrolyte.
and the applied potential was 4 V which was determined according to (4) A brown product is generated in the vicinity of the anode surface
the polarization curve shown in Fig. 7(b). Fig. 14 shows the polarization with the NaCl-based electrolyte, which deteriorates the electro­
curves and current density transients with different concentrations of polishing effect by decreasing the diffusion rates of dissolved
ethanol addition. The limiting current density plateau region was dis­ metal ions and fresh electrolyte towards to the anode surface. The
appeared with the ethanol concentration of 20 %, as shown in Fig. 14(a). EDS analysis shows that the brown product consists of high per­
The electropolishing effect was eliminated with a too high concentration centages of Cl and Na element due to the NaCl contained in the
of ethanol addition. The polarization curves show that the current electrolyte, and high percentages of Fe and O element are also
density was increased with increasing the ethanol concentration, which measured. It is speculated that the brown product mainly con­
is in agreement with the current density transients, and there was a tains dissolved metal oxides and metal chlorides.
slight change when the concentration was higher than 5.0 %. The in­ (5) The influence of the brown product on the electropolishing effect
crease in the current density can be explained from the solubilities of the was reduced by the ethanol addition in the NaCl-based electrolyte
containing ions in the brown product and the electrolyte viscosity. Kim because the solubilities of the ions contained in the brown
et al. [54] reported that the solubility of TiCl3 in the NaCl-based solution product were increased and the adherent ability of the brown
was increased by an ethanol addition because the polarity of ethanol product on the anode surface was decreased. The surface

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W. Han and F. Fang Journal of Manufacturing Processes 58 (2020) 1257–1269

Fig. 15. Optical microscope images and topographies of the electropolished surfaces in the NaCl-based electrolyte with the ethanol concentrations of (a) 0%, (b) 0%,
(c) 2.6 %, (d) 2.6 %, (e) 5.0 %, (f) 5.0 %, (g) 10 % and (h) 10 %. The electrolyte temperature was 66 ◦ C and the stirrer speed was 222 rpm, and the electropolishing
duration was 1200s.

roughness Sa was decreased from 457 nm to 251 nm by Declaration of Competing Interest

increasing the concentration of the ethanol addition with the
electrolyte temperature of 66 ◦ C and stirrer speed of 222 rpm. The authors report no declarations of interest.

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W. Han and F. Fang Journal of Manufacturing Processes 58 (2020) 1257–1269

electropolishing treatment. J Nucl Phys Mater Sci Radiat Appl 2015;467:194–204.

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