Electro Polishing of Surfaces Theory and Applications

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Electropolishing of surfaces: theory and applications
Article in Surface Engineering · July 2016

DOI: 10.1080/02670844.2016.1198452
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Electropolishing of surfaces: theory and

applications
G. Yang, B. Wang, K. Tawfiq, H. Wei, S. Zhou & G. Chen
To cite this article: G. Yang, B. Wang, K. Tawfiq, H. Wei, S. Zhou & G. Chen (2016):
Electropolishing of surfaces: theory and applications, Surface Engineering, DOI:
10.1080/02670844.2016.1198452
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Download by: [Florida State University], [Gang Chen] Date: 13 July 2016, At: 11:43
Electropolishing of surfaces: theory and
applications
G. Yang1, B. Wang2, K. Tawfiq2, H. Wei3, S. Zhou1 and G. Chen∗ 2
Electropolishing is the electrochemical process to remove the metallic material from the workpiece,
in order to obtain a smoother metal surface. It has found vast engineering applications in many
fields, such as food, medical, pharmaceutical and semiconductor industries. This review is
aimed to provide the readership with insightful understanding of the electropolishing process,
from the fundamental aspects as well as from the application aspects. The general aspects of
electropolishing, including its definition, the classic setup, the fundamentals behind it and
Downloaded by [Florida State University], [Gang Chen] at 11:43 13 July 2016
methods used to evaluate the electropolishing finishes are reviewed here. Various
electropolishing theories, be them quantitative or qualitative are briefly discussed. Based on
those theories, important parameters evolved in the electropolishing process are enumerated.
Many microscopic technologies are used to evaluate the electropolishing surface finishes. This
includes optical microscope, electron microscope and atomic force microscope. Some key
features of electropolishing are briefly outlined in the end.
Keywords: Electropolishing, Surface phenomena, Theory, Evaluation methods, Features
Fundamentals of electropolishing current (DC) power supply with the negative terminal
Electropolishing refers to the electrochemical process that being attached to the cathode.2 The piece is then
removes material from a metallic workpiece to polish, immersed into a bath comprised of a specially formulated,
passivate and deburr the metal parts.1–4 As the reverse temperature-controlled electrolytic solution. The acti-
of electroplating, electropolishing is also known as elec- vation of the power supply produces an electrical current
trochemical polishing or electrolytic polishing.5 Readers that passes from the anode to the cathode, resulting in the
can find useful information on the insightful fundamental oxidation of the metal surface and the removal of surface
mechanisms of electropolishing in D. Landolt’s early impurities and irregularities, which are dissolved in the
review (see Landolt1). To the best of our knowledge, how- electrolyte and diffuses through the film to the cathode
ever, a comprehensive review on electropolishing is still at a controlled rate.7,8 At the cathode, a reduction reac-
lacking. This review seeks to fill in this blank, and provide tion occurs, which normally produces hydrogen.1 The
the readers a more comprehensive understanding on the amount of metal removed depends on the specific bath,
electrochemical polishing fundamental mechanisms, the- temperature, current density and the particular metallic
ory development, surface finishes evaluation methods workpiece being electropolished.9 Usually, current and
and applications in various fields. Some most recent pro- time are the two variables that can be controlled to
gress in electropolishing will also be briefly reviewed here. reach the reproducible surface finish.10 Electropolishing
can be described by the Faraday’s laws of electrolysis.
Faraday’s first law of electrolysis and Faraday’s second
Chemistry basis of electropolishing law of electrolysis state that the amount of a material
Chemically speaking, electropolishing is a specific type of deposited on an electrode is proportional to the amount
electrolysis that involves a direct electric current passing of electricity used and the amount of different substances
through an electrolyte in an electrolytic cell (Fig. 1).6 liberated by a given quantity of electricity is proportional
The metal piece to be electropolished serves as the to their electrochemical equivalent (or chemical equival-
anode and is connected to a positive terminal of a direct ent weight).11,12
Electrolytes used for electropolishing are most often
1
Department of Chemical and Biomedical Engineering, FAMU-FSU College concentrated acid solutions having a high viscosity, such
of Engineering, Florida State University, 2525 Pottsdamer Street, Tallahas- as mixtures of sulphuric acid and phosphoric acid.13,14
see, FL 32310, USA Other electropolishing electrolytes reported in the litera-
2
Department of Civil and Environmental Engineering, FAMU-FSU College
of Engineering, Florida State University, 2525 Pottsdamer Street, Tallahas- ture include mixtures of perchlorates with acetic anhy-
see, FL 32310, USA
3
dride and methanolic solutions of sulphuric acid.
State Key Laboratory Geomechanics and Geotechnical Engineering, Insti-
tute of Rock and Soil Mechanics, Chinese Academy of Sciences, Wuhan
Electropolishing has many applications in the metal fin-
430071, People’s Republic of China ishing industry because of its simplicity and that it can
∗
Corresponding author, email [email protected]
be applied to objects of complex shape.15 Typical
© 2016 Institute of Materials, Minerals and Mining

Received 14 March 2016; accepted 1 June 2016
DOI 10.1080/02670844.2016.1198452 Surface Engineering 2016 1
Yang et al. Electropolishing of surfaces
1 Schematic illustration of a typical setup of the electrolytic

cell for electropolishing. The setup is composed of two
electrodes (cathode and anode), which are electrically 2 Schematic illustration of adsorbate acceptor model in
connected and immersed in a certain type of electrolyte. electropolishing. In this system, the anodic dissolution
The external power supply provides current through the of a metal alloy, M occurs in an electrolyte containing a
electrodes, and accordingly, the metal of the positive elec- small quantity of acceptor species, A. The limiting current
trode (anode or workpiece) is removed from the surface is reached if the concentration of the acceptor species, the
and becomes cations, which moved towards the cathodic accepter, A drops to near zero at the electrode/electrolyte
side. Often, the anodic surface becomes smoother after
interphase. At the electrode surface, the dissolution

the proper electropolishing process mechanism includes the oxidation of the metal to
adsorbed cations followed by solvation of the adsorbed
ions by the acceptor species, A31
examples are electropolished stainless steel drums of
washing machines and stainless steel surgical devices.16
Electropolishing is also commonly applied to the prep- order of several microns also contribute to the high resist-
aration of thin metal samples for transmission electron ance. The current density is controlled by the diffusion
microscopy because electropolishing does not cause limited acceptor ion approach to the surface, i.e. the con-
mechanical deformation of surface layers usually centration gradient of the metal ions across the diffusion
observed when mechanical polishing is used.9,17 Ultra layer.26 The film formed on a surface undergoing dissol-
high vacuum (UHV) components are typically electropol- ution is not a simple oxide but rather a contaminated
ished in order to have a smoother surface for improved oxide that has incorporated anions from the electrolytic
vacuum pressures, outgassing rates and pumping speed.18 solution.27
Electropolishing proceed by the dissolution or oxi-
dation of the metal, during which cations are released
Surface phenomena occurring during and adsorbed onto the surface (Fig. 2). The blocking of
electropolishing the surface by these adsorbed ions may lead to overpoten-
Understanding the surface processes occurring on the tial for metal dissolution.28 The cations are removed from
metal surface during electropolishing is the key to derive the surface by the acceptor ions that diffuse to the surface
its mechanism. It can also help optimise the parameters to solvate the metal ions. The process of electropolishing
of practical operations.19 Electropolishing may be limited results in the density near the electrode different from the
by mass transport, more specifically, diffusion of the dis- bulk of the solution resulting in a hydrodynamic flow. At
solving metal ion, acceptor species from the electrolyte steady state, the concentration of the acceptor ions at the
and water molecules. Commonly the diffusion limitation surface is fixed at zero if they are consumed as soon as
is the metal ion. Subsequently, a salt film precipitates on they reach the surface. A recent study of copper electro-
the surface, either, porous or both compact and porous. polishing in phosphoric acid and niobium electropolish-
It is believed that salt layer formation takes place at the ing in sulphuric acid-hydrofluoric acid mixture verified
bottom of pits and there is an ionic transport through that the acceptor species was the rate limiting species
this layer because of the presence of a high electric field that diffuses to the surface.29,30 The potential transients
across the layer.20 A compact film on the surface will be measured for copper electropolishing displayed a sharp
formed during electropolishing and gas bubble evolution rise in potential with applied current, followed by a poten-
does not occur on the surface even though the potentials tial increase owing to the activation overpotential and
are high enough to thermodynamically allow bubble for- mass transport overpotential.30 The huge jump in poten-
mation due to the non-electron-conducting nature of the tial after the transient time indicated a very high
film.21 The mechanism of conduction is thought to be resistance.
solid state conduction in the compact layer and the high
resistance of the compact film is attributed to low mobi-
lity of ions for solid state transport.22 The thickness of Cathode, electrolyte and viscous layers
the compact film is considered to be in the order of For electropolishing, the anode is connected to a positive
10 nm due to the low mobility of ions by solid state trans- terminal of a DC power supply with the negative terminal
port process.23 The conduction in the porous region is by being attached to the cathode. Current flows in from the
migration in the electric field. There is no diffusion in the power supply and the cathode is the terminal where cur-
porous region since the pores are filled with the electrolyte rent flows back to the power supply. Cathode polarity
saturated with the dissolved metal ions.24,25 The low por- with respect to the anode can be positive or negative
osity of the porous film and its large thickness on the depending on the device and the way it operates.32
2 Surface Engineering 2016

Positively charged cations always move towards the cath- Therefore, the value of the limiting current would be lar-
ode and negatively charged anions move away from it. In ger over the protrusion compared to that over the valley,
the Electropolishing setup, the anode is positive and the resulting in the metal surface being levelled out as electro-
cathode is negative.33 polishing proceeds.31 Mass transport control has been
The electrolyte is the substance that produces an electri- established as the reason behind electropolishing, which
cally conducting solution when dissolved in a polar sol- is associated with the voltage range and is characterised
vent, such as water.4 The dissolved electrolyte separates by a constant current density, independent of the voltage
into cations and anions, which disperse uniformly through applied.1,40
the solvent. During electropolishing, the cations of the
solution would be drawn to the electrode that has an
abundance of electrons, while the anions would be Relation between anode potential and anode
drawn to the electrode that has a deficit of electrons.8 current density
The movement of anions and cations in opposite direc- Faraday’s laws provide the theoretical basis of electrode
tions within the solution amounts to a current. Different potential and current density.11,41 However, in a real
metals may need different types of electrolyte. The com- application, many factors influence the eletropolishing
position and properties of the electrolyte is very important quantity and quality. Faraday’s laws state that the amount
for the electropolishing quality.1 In addition to metal of chemical charge at an electrode is exactly proportional
salts, Electropolishing electrolytes usually contain a num- to the total quantity of the electricity. However, side reac-
ber of additives for various purposes. Some agents are tions may consume the product if taking place simul-
used to increase electrolyte conductivity (supporting elec- taneously at the electrode.42 Therefore, inefficiencies
trolytes). Others may be used for increasing bath stability may arise from the side reactions other than the intended
(stabilisers), activating the surface (surfactants or wetting reaction takes place at the electrodes. In electropolishing,
agents), improving levelling or metal distribution (level- sufficient voltage should be provided by the power source.
ling agents), or optimising the chemical, physical or tech- The voltage–current relationship follows the Ohm’s law,
nology properties of the surface.34,35 These properties i.e. the current is driven by a potential difference, or vol-
include corrosion resistance, brightness or reflectivity, tage through the conducting medium, either electrolytic
hardness, mechanical strength, ductility, internal stress, or metallic. The local current density is a very important
wear resistance or solderability.36,37 The properties of variable in electroplating operations and affects the char-
electrolyte are usually characterised by electrolytic con- acter of the electropolishing. The local current density on
ductance, which is different from electrical conductance an electrode, defined as the current in amperes per unit
in metal. Both inorganic and organic salts, acids and area of the electrode, is a function of the position on the
alkalis can be used to increase the electrolytic conduc- electrode surface and the current passing through the elec-
tance. The conductivity of an electrolyte is a function of trode that accomplishes the desired electropolishing is
the degree of dissociation, the mobility of the individual expressed in terms of current efficiency.40,43 The current
ions, the temperature and viscosity, and the electrolyte distribution over an electrode surface is complicated and
composition.31 tends to concentrate at edges and points, and unless the
During Electropolishing, a viscous layer on the work- resistance of the solution is very low, the current will
piece is formed.5,38 The non-uniform thickness of the vis- flow to the workpieces near the opposite electrode more
cous layer over the material surface results in a different readily than to the more distant workpieces. It is desired
ohmic resistance from the cathode to the anode, which to operate processes with uniform current distribution,
causes greater dissolution of the protruded parts com- i.e. the current density is the same at all points on the elec-
pared to the depressed part, thus creating a uniform sur- trode surface.44
face profile.39 A varying concentration gradient of the When the workpieces are immersed into a solution,
dissolved metal ions over the protrusions and valleys equilibrium is reached between the tendency of the
occurs (Fig. 3). The thickness of the diffusion layer over metal to enter solution as ions and the opposing tendency
the protrusion is smaller than the value over the valley. of the ions to lose their charge and deposit on the cathode.
The equilibrium is dynamic with metal being ionised and
discharged as well as being deposited and reduced. These
two effects cancel each other and there is no net change in
the system. For the realisation of metal deposition at the
cathode and metal dissolution at the anode, the equili-
brium is broken by an external potential, which makes
the electrode reactions take place at a practical rate. The
extra energy needed to force the electrode reaction to pro-
ceed at a required rate (or its equivalent current density) is
quantified in terms of overpotential or electrode polaris-
ation, the difference in the electrode potential of an elec-
trode between its equilibrium potential and its operating
potential when a current is flowing.45 The operating
potential of an anode is always more positive than its
equilibrium potential, while the operating potential of a
cathode is always more negative than its equilibrium
potential.46 The value of the overpotential depends on
3 Schematic cartoon indicating the concentration gradient the inherent speed of the electrode reaction, which
difference over protrusions and valleys on the anode increases with increasing current density. A slow reaction
surface
Surface Engineering 2016 3

(with small exchange current density) will require a larger odour, limited cathode time and the electrolyte being dif-
overpotential for a given current density than a fast reac- ficult to maintain and expensive to replace, even under
tion (with large exchange current density). Since an elec- active chilling conditions during the production tails for
trode reaction commonly occurs in more than one deburring automotive parts in an ethylene glycol electro-
elementary step, there is an overpotential associated lyte with ammonium salt.59,60
with each step. Even for the simplest case, the overpoten- The second contribution to the increasing electrolyte
tial is the sum of the concentration overpotential and the resistance comes from the limited diffusion process on
activation overpotential. The terms overpotential is some- the cathodic surface. As has been mentioned before, the
times called overvoltage, the difference between the cell diffusion layer thickness increases with the electrolyte vis-
voltage (with a current flowing) and the open-circuit vol- cosity.31 Jacquet reported that the optimum region for
tage.47 Consequently, the cell voltage of the electrolytic electropolishing is the current limited plateau in the polar-
cell is always more than its open-circuit voltage. The over- isation curve.61 Later, Wagner studied the ‘microprofile’
voltage is the sum of the over potentials of the two electro- levelling under mass transport limited conditions for the
des of the cell and the ohmic loss of the cell.48,49 case of large diffusion layers.26 The reasons for the
For electropolishing, the current source is a power build-up of the diffusion limitations are due to the limited
source in the form of a battery or rectifier that converts diffusion of the dissolved metal ions away from the
alternating current electricity to regulated low-voltage polished workpiece surface62 and/or the limited diffusion
DC current. The geometric shape and contour of a work- of an ‘acceptor ion’ from the bulk electrolyte to the
piece to be polished affect the quality of the eletropolish- polished surface.39 These diffusion limitations further
ing. The DC current flows more densely to sharp edges increased the electrolyte resistance, thus hindering the
than to the less accessible recessed areas, making electro- electropolishing process.1
polishing possible. In other words, the current distribution Another issue brought by continuous DC electropolish-
is not uniform. Therefore, a judicial placement of the ing is the uneven striping of the anodic metal from the sur-
anode(s) as well as modifications of the current density face. This will lead to a rougher surface.59 The reason is
is required to obtain quality eletropolishing results.50,51 stated as follows. A passive oxide film usually grows on
the anode surface during electropolishing process, as
Effect of pulsed current can be described by
The conventional electropolishing is normally performed M + xH2 O M(Ox ) + 2xH+ + 2xe− (1)
in media with high viscosity and/or low conductivity such
as concentrated acid (phosphoric acid, sulphuric acid and The continuous DC current supply preferably creates
their mixtures or in perchloric acid-acetic acid solutions) high current density areas and low current density areas
and non-aqueous solutions (ethylene glycol, methanol- on anodic surface. As time goes on, some anodic surface
sulphuric acid).1 Sometimes methanol, instead of water would be blocked by thus generated oxidative film (on
is used as a solvent.13,14,52 In the last century late fifties high current density areas) whereas the striping is still
and early sixties, the development of electrochemical occurring on areas that has not been blocked, thus gener-
machining showed that fast dissolution of metals in natu- ating uneven anode surfaces.59
ral electrolytes under vigorous convection conditions may
lead to electropolished surfaces,53 with the controlling Pulse/pulse reverse current in electropolishing process
factors being convective mass transfer.54,55 Soon after, it The pulse/pulse reverse current has been vastly used in
was found that the electropolishing in neutral salt sol- electrodeposition process,63–65 in which the potential or
utions could be reached at relatively low average current current is alternated fast between two different levels.
densities and flow rates if pulse current with high density This leads to a series voltage or current pulses of nearly
was utilised.56 More tables and electropolishing electro- equal amplitude, duration and polarity (Pulse-se),66 segre-
lytes for various metals can be obtained in the books by gated by reference current (usually zero). Each pulse is
W. J. McTegart5 and P. V. Shigolev.57 composed of an ON-time (ton) at which the potential or
current is applied and an OFF-time (toff) during which
Motivation of using pulse current in electropolishing the potential or current is kept zero (shown in Fig. 4).
As has been mentioned in earlier sections, the asperities The pulse reverse technique67 plating current is inter-
on the metal surface are preferentially removed during rupted by a striping time, instead of the zero-current
an electropolishing process. In order to focus the electric time in pulse electrodeposition process (i.e. the OFF-
field on surface asperities, low conductivity electrolytes time in Fig. 4 is replaced by a negative current on time)
of high viscosity, such as ethylene glycol may be resorted
to.1,5 In this way, the voltage gradient between the asperi-
ties and the recesses becomes bigger along with the
increase of the electrolyte resistance, so that the asperities
are preferentially removed. Despite the merits of applying
low conductivity electrolytes in electropolishing process,
excessive heating of the electrolyte was often observed
during the process, due to the greatly increased electrolyte
resistance.58 Thus, a chilling process should be performed
during electropolishing. However, even with a chilling
process, the excessive heat issue could still not be fully
avoided. For instance, Ford Motor Co. reported that the
excessive heating resulted in an unacceptable ammonia 4 Schematic illustration of a typical pulse current waveform

Two potential issues are involved in the DC electrode-

position. First, a negatively charged layer around the
cathode/electrolyte interface is generated as the electro-
plating process continues. This layer obstructs the metal
ions from arriving at the cathode surface. Second, the
high current density areas in the electrolyte bath becomes
more depleted of ions than low current density areas. To
solve these issues, pulse/pulse reverse technique is resorted
to. For instance, in pulse electrodeposition process, the
output is periodically turned off to cause the discharge
of ion diffusion layer close to cathode surface. In addition,
during the OFF-time, the ions migrates to the depleted
area, thus counterbalancing the non-evenly distributed
cations during continuous DC electrodeposition process.
The same scenario applies to electropolishing process.
In previous section, it has been stated that a diffusion
layer of anions could be established on the anode surface
during continuous DC electropolishing. The uneven dis-
tribution of the anion on the anode surface on high cur-
rent density areas versus low current density areas could
also result in pitting issues. Taylor68 has developed a sur-

face finishing process based on the electrolysis in aqueous
electrolytes. As shown in Fig. 5, a generalised pulse–pulse
reverse wave form can be described as follows.59 The
anodic forward pulse is tuned on (pulse-time and peak 5 Generalised Pulse/pulse reverse waveform for electropol-
voltage) to enhance the anion transport to anode. During ishing. The anodic pulse can be utilised to enhance anions
the reverse pulse phase, the cathodic pulse is tuned on. It transport, and the cathodic pulse facilitates to depassivate
is capable of depassivating the surface and thereby elimi- the anodic surface. During OFF-time, the reacting agents
nating the need of using chemical additions such as hydro- are replenished and the anodic surface byproduct is
fluoric acid or other oxide. This process might be followed removed59
by an OFF-time to facilitate replenishment of reacting
species and removal of byproducts and heat.
Because of the much higher instantaneous anodic pulse Basic control parameters governing the
current density than the DC steady state current, pulse/ performance
pulse reverse electropolishing generally has a higher The key parameters related to voltage–current curve
material removal rate than/equal to that of a DC electro- include applied voltage range, the current density range.
polishing process.59 The factors related to electrolytes include the component
In the conventional DC electropolishing, only one par- ratio of the species, temperature, the electrolyte bath age,
ameter is of concern and can be tuned, which is the cur- the convection of the electrolyte bath and duration of the
rent density. As shown in Fig. 5, many parameters in whole electropolishing time.29,32,73
pulse/pulse reverse waveform could be adjusted in order As many factors are involved and have to be optimised
to optimise the electropolishing results, such as the pulse in an electropolishing process, there is no one-fit-all par-
time, ta, the pulse reverse time, tc, the OFF-time, toff ameter set for all electropolishing setups. First, the elec-
and the current density amplitudes, ia and ic. To fully trode-electrolyte system should be specified. The choice
understand the guiding principles of optimising the of electropolishing electrolyte is highly dependent on the
pulse/pulse reverse waveform, the concentration profile anodic metal type. Second, the parameters related the
of the anions from the anodic surface to the bulk electro- electropolishing process are normally optimised against
lyte should be considered.69–71 It has been proposed that available current–voltage relationship, which has nor-
from the anode surface to the bulk electrolyte, two diffu- mally been documented in literature for specific elec-
sion layers, namely a stationary layer (δs) and an inner trode-electrolyte systems. Many electropolishing systems
pulsating layer could be used to describe the concen- exhibit general current–voltage curves akin to the one
tration profile. With the assumption of the linear concen- given in Fig. 6.61,74–76 As aforementioned, in Regime I,
tration gradient, the thickness of the inner pulsating layer what primarily occurs is the direct dissolution of the
was considered to be proportional to the pulse time, t70 p : metal (i.e. etching occurs). In Regime II, the slight
decrease current density with increase applied voltage
normally indicates the generation of the passive layer on
Dtp the anodic surface. In Regime III, the passivation layer
dp = 2 (2)
p is stabilised and anions dissolved from the metal surface
diffuse through the passivated layer. In Regime IV, with
With D the diffusion coefficient. the further increment of the voltage, the passivated later
As emphasised by M. Inman et al., although more breaks down on anodic surface. Also in this area, the
accurate estimates of the pulsating layer thickness anodic metal surface will begin pitting. It should be men-
exist,59,72 Equation 2 should be sufficient to describe the tioned that, despite the well-established current–voltage
tunability of the pulsating layer thickness by the pulse relationship, the refinement to the current–voltage curve
time due to their proportionality. is necessary for a given electropolishing cell.

the stainless steel would have a microscopically smoother

surface, leading to a decreasing bacterial attachment.89
The selection of the electropolishing electrolyte of the
stainless steel has some prerequisites:
a. Being capable of dissolving metallic surface layer on
some preferential parts on an atomic level;
b. Being capable of providing the control over the
oxide film thickness- electropolishing rate would
be extremely slow if the passive layer is too thick,
whereas preferential etching occurs at a too thin
passive layer;
c. Should favour the formation of a viscous diffusion
layer which promotes the macroscopic levelling.
The major processing parameters significantly affect
6 The general polarisation curve showing the current/vol- the properties of the stainless steel, such as the surface
tage relationship in the metal electropolishing process smoothness and anticorrosion performance.43,90 Table 2
is a brief summary on many work done on electropolish-
ing stainless steel previously.
Normally, the electrolytes suitable for electropolishing
are acids (e.g. perchloric, sulphuric, phosphoric, etc.) or The influence of temperature
their mixtures in a certain solvent, such as water, alcohol
and acetic acid. In order to increase the solution viscosity, The temperature was important for electropolishing. For
glycerol, butyl glycol or urea, etc. are usually added.43,73 example, in Ashwini Chandra’s work on electropolishing
Copper is one of the most intensively studied workpieces of Niobium, the plateau current density in the current–
for electropolishing system. Many types of electrolytes32,75 voltage curve was found increasing with temperature.29
or electrolytes mixtures61,76–80 meet the requirement in pol- The second example of the temperature effect comes
ishing copper. Some of the previous work, under which from the stainless steel electropolishing in an electrolyte
conditions the electropolishing process was performed composed of 65%H3PO4+20%H2SO4+15%H2O per-
has been summarised in Table 1. formed at 25, 50 and 70°C by D. Landolt, et al. 92 It
Another type of metal that is a good raw model to illus- was found that the limiting current density, as reflected
trate the importance of the electropolishing condition by the current plateau in the polarisation curves increased
optimising is the stainless steel. Stainless steel has found as the temperature went up.
vast applications in nowadays society. However, their The temperature effect is explained as that the diffusion
standard colour-light grey does not always fit in the sur- coefficient of the rate limiting species in the electropolish-
roundings where they are applied. Surface treatments, in ing bath is affected by95

this sense, are crucial to their versatility. Before the surface Qa
treatments executed, a surface polishing step is a must.83 D = D0 exp − (3)
RT
Among many surface polishing methods, such as mechan-
ical polishing or grind, chemical polishing and electropol- in which Do is the exponential pre-factor, Qa is the acti-
ishing, the latter method has many advantages versus its vation energy for diffusion, R is the gas constant and T
counterparts.84,85 For example, the dissolution rate of is the absolute temperature.
the metallic surface can be removed at a significantly The limiting current density of a specie in electropolish-
increased rate compared with chemical polishing, with ing bath can be described as96
an enhanced-quality of the metal surface finish.
nFDC
The stainless steel surface smoothness also plays a key iL = (4)
role for some biomedical applications. For example, it is d
known that the substrate roughness affects the adhesion where n is the molar of the total charge of ion involved, F
of the bacteria.86–88 With a careful electropolishing process, is the Faraday constant, C is the saturation concentration
Table 1 Summary of major parameters of electropolishing process on copper workpiece
Current density Voltage Literature

Electrolyte Temperature range range reference
Anhydrous orthophosphoric acid 25°C Not specified Not P.A. Jacquet81

specified
Orthophosphoric acid solution (Non-agitated Solution) −5.6°C to 53°C 0.2 to 1.5 A/dm2 0.7 to 0.9 V P.A. Jacquet61
Orthophosphoric acid/water solution (Agitated solution) −5.6°C to 53°C 0.2 to 1.5 A/dm2 Not P.A. Jacquet61
specified
Orthophosphoric acid/water solution 25°C 0.0625 A/cm2 0.8 to 1.2 V J. A. Allen77
Phosphoric acid/water solution with/without glycerol, 17 to 25°C 2 to 4.2 mA/cm2 0.25 to 1.5 V H.F Walton78
ethylene glycol
Phosphoric acid/copper phosphate/water solution 25°C 50 to 1000 mA/cm2 0.2 to 0.8 V S.H. Glarum
J.H. Marshall79,82
Orthophosphoric acid/sulphuric acid/water solution 25°C 0.1 A/cm2 1.8 to 2.2 V E.C.W Perryman80

Table 2 Summary of major parameters of electropolishing process on stainless steel workpiece
Stainless Current Literature

Electrolyte steel type Temperature density range Voltage range reference
Phosphoric acid, sulphuric acid and 304 30 to 70°C 0.5 to 1 A/cm2 Not specified Tai-Chou Lee
glycerol mixture et al. 43
Phosphoric acid, sulphuric acid and 304 5 to 80°C 0.5 to 1 A/cm2 Not specified Chi-chang Hu
glycerol mixture et al. 91
Phosphoric acid, sulphuric acid and water Fe13Cr 25 to 70°C 0.01 to −0.81 to 1.45 V D. Landolt,
solution 0.225 A/cm2 et al. 92
Four electrolytes (Mixtures of sulphuric 316L 50 to 80°C Not specified Voltage scanning Herzog, Grégoire
acid, phosphoric acid and glycerol) rate 5 mV/s et al. 93
Mixtures of Sulphuric acid, phosphoric 316L 50 ± 95°C 0.5 to 2.5 A/ Not specified Y. F. Chen, et al. 90
acid and water with/without glycerine cm2
Mixtures of sulphuric acid, phosphoric 316L 65 to 70°C Not specified 2.5 to 10 V Sasha Omanovic
acid, water and glycerol et at.94
of metal ions in the solution and δ is the thickness of the forced stirring of the electrolyte during electropolishing
anodic diffusion layer. of niobium led to an increase in the limiting current den-
Substituting Equation 3 to 4 yields sity at 22°C.
The effect of convection on the limiting current can be

nFD0 C Qa
iL = exp − (5) explained by the Equation 4. The diffusion layer thick-
d RT ness, δ is decreased with the convection flow, thus increas-
Equation 5 relates the bath temperature to the plateau ing the limiting current density, iL.
current density (i.e. stable current density). Following this However, as shown in Tian et al.’s study,105 the temp-
equation, it is obvious that the increase of the temperature erature of the electrolyte near the Nb electrode surface
would result in an exponential increase of the current den- was a bit higher than that of the bulk electrolyte. Stirring
sity. However, it should be noticed that, as the tempera- could remove the excess heat on the anodic surface, thus
ture rises, the viscosity of the diffusion layer on anode bringing down the temperature. This should result in a
surface is decreased, making it more difficult to maintain decrease of the current density indicated by Equation 4.
a viscous anode layer. This would inevitably affect the The synergetic effect of the two, however, still contributed
metal surface finish quality. In this sense, the temperature to an increase limiting current density.29
range to reach an optimum electropolishing result for a
specific system should be carefully selected. Other effects
Other factors that affect the electropolishing process
includes pretreatment of the metal surface, orientation
The influence of convection of the workpiece in electropolishing bath, choice of the
Many studies on the electropolishing mechanism have cathode material, electrode spacing, bath age, electropol-
revealed that the electropolishing is a diffusion-dominated ishing time, etc.73
process,1,62 which occurs at a certain limiting current. The pretreatment is curtail to the electropolishing pro-
Hence, the electropolishing can be treated similar to the cess. For instance, if the sample surface roughness is too
mass transfer in a cathodic deposition process, in which large, a high voltage and long electropolishing time
mass transfer theory has been well established.97 Many should be chosen in order to improve the surface finish
works have been performed in studying the forced convec- quality. The electropolishing bath age is also a big concern
tion mass transfer during electropolishing78,98–101 For during the process. This is because that it is a standard
example, H. F. Walton78 studied an electropolishing sys- practice in industry to reuse the electrolyte to keep a
tem composed of a rotating copper electrode and a low profile of cost and minimise the detrimental effect
CuHPO4 in aqueous phosphoric acid and phosphoric to the environment.106 However, as time goes on, it is
acid-glycerol-ethylene glycol mixtures. The limiting cur- commonly seen that the limiting current density decreases
rent density was found to be dependent on the anode after a certain course of time due to the consumption of
rotating speed, which was correlated to the agitation of the cations.107 Thus, it is critical to guaranty a preferable
the electrolyte. chemistry for electropolishing and the bath age should be
Natural convection electropolishing conditions have tuned to an optimistic value.
also been studied. For example, Fouad et al. 102 used a ver-
tically placed copper electrode in phosphoric acid bath to
study the mass transfer under free convention in electro-
Electropolishing theory
polishing. Triggered by Fenech and Tobias103 electrode- In an electropolishing system, the interface between the
position work with a horizontal electrodes under natural metal and the electrolyte has an active surface, regulating
convection mass transfer conditions, A. M. Ahmed the dissolution of the metallic material. Generally speak-
et al. 104 illustrated the role of the mass transfer in the kin- ing, three components are included in the electrolytic sol-
etics of electropolishing of horizontal flat copper plate ution: an acid or a base to ensure the oxidation of the
facing downwards under natural convection conditions. material, a reagent to regulate the dissolution speed (i.e.
The convection flow was driven by the electrolyte density passivator) and an element to promote the viscous state
difference between the bulk and anodic surface. In a study in the solution/metal interface. This viscous layer is
performed by Ashwini Chandra,29 it was found that the formed due to the continuous dissolution of the metal

depression. In their study, an inverse relationship of cur-

rent density and viscosity was also observed with an
increased current density with stirring. The earliest
descripting on the resistance of the viscous film formed
between anode and the electropolishing liquid described
by Jacquet is somewhat obscure.
Diffusion phenomena (Elmore theory)

7 Schematic illustration of the ionic concentration gradient The Jacquet’s resistance theory on electropolishing was
on a rough anode surface later challenged by Elmore.62 It has been observed that
the factors which might facilitate to destroy the electro-
lytic layer between the anode and electrolyte led to uneven
into metal ion, which moves from the metal surface to the polishing of the metal surface.78,111 This case, however,
bulk electrolytic solution. Thus, on a rough metal surface, could be altered by modifying the electropolishing con-
an ionic concentration gradient forms between the cre- ditions (e.g. temperature, agitation, electrolyte viscosity
vices and the projections (Fig. 7). A higher current density and anode position from being horizontal to vertical).75
exits on the projections than on the crevices, resulting a Based on these observations, Elmore62,112 postulated the
faster dissolution of the metal on these regions. In this
importance of diffusion in the electropolishing process.

way, the rough surface gradually levels out, becoming He used the copper-in-orthophosphoric as a model sys-
smoother. tem and studied the current–voltage relationship, and
Many theories explain this effect, including Jacquet eventually attributed the polishing effect to a varying con-
Theory, Elmore Theory, Edwards Theory, Hoar and centration gradient of the dissolved metal ions over the
Farthing Theory and Darmois Theory etc.108 It should projections and crevices.
be noted that, because the electropolishing process is gov- The basic assumptions of Elmore theory of electropol-
erned by many different mechanisms and depends on ishing are: (a) metal ions are dispersed from the anode by
many parameters, despite the simplicity of the scenario diffusion and convection instead of electrolytic migration;
described above, no single theory is capable of covering (b) the interface of anode and electrolyte is saturated with
all the complexities. However, these theories are con- the products of solution. On this basis, Elmore believes
sidered of key importance in helping the readership better that in the case of copper polished in orthophosphoric
understand the electropolishing process. Therefore, in this acid, the concentration of anodic copper ions in the elec-
section, a brief introduction to these theories will be trolyte increases with current density, until it reaches a
sketched. maximum value. Dissolution of the metal continues
beyond this point only to the extent that copper ions are
Effect of resistance (Jacquet theory) allowed to diffuse into the bulk electrolyte from the
boundary layer. The value of the Nernst diffusion layer
Jacquet was the first researcher who investigated the
thickness, δ over the projection is smaller than the value
importance of the ohmic resistance of the viscous liquid
over the crevices,97,113 which results in a larger limiting
layer between the anode and the electrolyte during elec-
current, as defined by Equation 6,114 over the projection
tropolishing.74 The non-uniform thickness of the viscous
part than the crevices.
layer on the material surface leads to different resistance
between the cathode and the anode, which causes larger
dissolution of the protruded parts versus the depressed nFD(Cs − Cb )
part. On this basis, a uniform surface profile can be cre- iL = (6)
d
ated. In a later experiment led by Jacquet and others,61
they showed that in a plot of current density, J as a func-
tion of cell potential (or anode potential), E, a horizontal n is the total number of ions involved; F the Faraday con-
plateau existed for many solutions used in electropolish- stant; D the diffusion coefficient of the rate limiting
ing processes. The J-E plot was found that whenever the species; Cs the surface concentration, i.e. saturation con-
diffusion of one reactant consumed by an electrode pro- centration of metal ions in the solution and Cb the bulk
cess was the controlling factor. The concentration of the concentration of the ions.
electrode surface reactant is much less than its bulk The larger limiting current density around projection
counterpart, and the effective thickness of hydrodynamic part results in the metal surface being levelled out as elec-
boundary layer has a definite value determined by either tropolishing proceeds. In the Nernst diffusion layer model
forced or natural convection. Particularly, a limiting cur- (Equation 6), a concentration gradient is assumed to be at
rent density is observed for the electrodeposition of metals the interface, which varies linearly at the immediate vicin-
at the cathodic side. In a parallel study, Kolthoff and ity of the metal surface and then has a curvature until it
Miller109 also observed a limiting current density for the merges with the final constant electrolyte bulk concen-
anodic dissolution of mercury if the diffusion of the com- tration of the species.96 It is a mathematical construct
plexing ions such as S2O− − − −
3 . SO3 CN and SCN was set as that artificially separates the electrolyte region near the
the limiting factor. anode surface from rest of the electrolyte. This has
In a later study,110 Hickling and Higgins showed that, become the generally accepted mechanism for electropol-
in the anodic dissolving rate determining step, the current ishing and the mass transport control has been established
density of a 0.15 mm asperity could be 2.5 times that of a as the reason behind electropolishing.

Elmore further concluded that the ratio could be with the anodic metal. In this framework, the basic elec-
defined as tropolishing mechanism is one of the migration of ‘accep-
tors’ to the anode instead of the diffusion of metallic ions
t0
r= (7) in the opposite direction. Accordingly, the limiting factor
i0 t1/2
0 Cm AF (pD)
1/2
of the current density is related to a maximum concen-
where io is the applied current, to is the transition time to tration gradient when almost all the acceptors approach
build the polishing conditions, Cm is the solubility of the anode and react with the surface metallic ions on
metal in the electrolyte, A is the surface area of the the anode. Due to the continuous consumption of the
anode, F is the Faraday constant and D is the diffusion acceptors on the anode surface, the acceptor concen-
coefficient of dissolved metal (constant). It is worth noting tration is much lower around the electrode than that in
that, the ratio in Equation (7) was developed based upon the bulk solution.
Smuluchowski’s equation115correlating the motion of Later, Carl Wagner26 used the acceptor theory to math-
charged species to the surrounding media viscosity. And ematically analyse an ideal electropolishing process. He
it does not consider the diffusion rate decrease resulted assumed that the electrode surface could be best described
from the viscosity increase. Thus, Elmore’s theory has by a sing wave profile, as described below
its own limitation, considering the viscosity is capable of y = b sin (2px/a) (8)
answering: (a) why many polishing baths are viscous
liquids; (b) why the character of polishing increases with where a is the wavelength, b is the amplitude, y is the dis-
viscosity78; and (c) why dilution or increase in tempera- tance from the ‘average surface plane’ of the anode and x
ture hinder the polishing of copper in orthophosphoric
is the coordinate parallel to the average surface plane. The

acid.32 ionic concentration profile versus y is schematically illus-
Later, Williams and Barrett20 offered the experimental trated in Fig. 8. This profile, based upon Fick’s second
details to confirm Elmore’s theory. law, was eventually derived as26
Focused on the film formed on copper during electro-
polishing, they showed that the film is composed of a ∂C ∂C 2p b
1+ sin(2px/a) if
phosphate of copper characterised using electron diffrac- ∂y y=bsin(2px/a) ∂y ave a
tion techniques. This facilitated to confirm the basic
assumption in Elmore’s theory that a solubility limit of b ,, a and a ,, d
copper existed in the boundary layer of the electrolyte. (9)
A further study led by Hoar and Farthing116 showed
that, since the copper phosphate film is soluble in phos-
phoric acid even in the absence of applied potential, the Here the (∂c/∂y)ave is the average value of the concen-
solubility limit could be attributed to the a decrease in tration gradient at the anode. A linear dependence of
hydrogen ion concentration at the anodic surface during the concentration on the distance, y could only be found
polishing process. at the inner most part of the discussion layer.
Taking into consideration of the change in the shape of
the surface profile as a function of time, the sine wave
Acceptor theory – distribution of anions amplitude at time t could be derived as
While Elmore and others proposed that the diffusion of
metal ions determined the dissolution of the metallic b = b0 e−2pm/a if b ,, a and a ,, d (10)
anode to the liquid electropolishing agent, Halfway
suggested that, instead of ionic diffusion, the distribution where bo is the amplitude of the sine wave surface profile
of the anions along the anodic surface controlled the dis- at time zero, and b is the surface profile at time, t; u is the
solution of the metal in electropolishing.117 This point of corresponding displacement of the average surface plane,
view was considerably developed by Edwards39 both and could be further derived as
experimentally and theoretically. Using a composite cop-
m = a[Ln(b0 /b)]/2p (11)
per anode, which had projections and recesses on the sur-
face, in phosphoric acid solutions, Edwards found that the
current distribution on the projections and recesses
endured very little change when the total current fell
and polishing conditions were established. Thus, a quan-
titative investigation of the smoothing efficiency under
various conditions on the surface of standard roughness
were performed. The resulted efficiencies in Edward’s
experiment was compared with those calculated from a
wholly diffusion-controlled electropolishing process. The
conclusion drawn in that study was that the smoothing
mode in electrolytic polishing was not specific to pro-
cesses, but caused only by the variations in concentration
gradient through the diffusion layer on anode surface.39
More specifically, the basic assumption in Edward’s
theory is that the polishing effect was determined by the
depletion of the anolyte layer of ‘acceptors’. The term
‘acceptor’ means the anions and molecules (e.g. water 8 Schematic illustration of acceptor concentration profile as
molecules) which has the potential to combine or complex a function of distance from the electrode

Thus, the loss of metal per unit area, Δm/A could be interval of time when a slow rise of anodic single potential
calculated as showed up, followed by a large rapid one at its end right
before polishing happened. They compared the phenom-
Dm/A = ar[Ln(b0 /b)]/2p (12) ena with those established by Muller for the onset of the
where ρ is the density of the metal. passivity of nickel, iron and other metals in less concen-
Using a 2-dimmensional Laplace equation inside the trated sulphuric acid,122 and postulated that the rapid
electrolyte, the local potential gradient could be written as rise of potential at the onset of electropolishing was due
to the similar formation of a compact oxide film on the
∂f ∂f 2pb metal surface to the anodic passivation. However, this
1+ sin(2px/a) if
∂y y=b sin (2px/a) ∂y ave a film dissolved as fast as it was formed anodically from
the metal.99
b ,, a and a ,, d Direct experimental observations on the existence of
(13) the oxide film at the onset of electropolishing was given
by Hoar and Farthing.116 An electropolishing system
The local potential gradient, (∂w/∂y)is linearly related
composed of copper and α-brass anodes, the orthophoric
to the local current density by Ohm’s law. Through the
acid/water bath (50/50 by volume) and a cathode with
set of formulae (from Equation 9 to 13), Carl Wagner
holes was used in their study. Mercury was dropped
mathematically solved the profiles for the decrease of sur-
onto the copper or α-brass anodes through the holes on
face roughness as a function of the recess of the average
cathode, and wetted the anodic surface immediately,
surface, amount of metal dissolved per unit surface
and then spread over it, if the passive film had not formed
area, and product of current density and time. It should

on the anodic surface. By telling the different wettability
be noted that, the development of the larger surface
of the mercury droplet on the anodic surface, they showed
roughness profile (i.e. macroprofile) from Wagner’s for-
whether or not that anodic surface was covered by the
mula agrees well with Edward’s theory. Also in his analy-
passivation film.
sis, Wagner rejected Elmore’s theory regarding the
Hoar’s theory could also quantitatively explain the
inconsistence of the metal ion concentration at the con-
‘smoothing’ effect on preferable dissolution of asperities
stant current density at wide variation of anodic potential.
on anode during the electropolishing process.116 The tran-
sient mobile layer of saturated solution and solid formed
Passivation theory (Hoar and Farthing theory) on the anodic surface before the ‘passive’ film had been
Hoar and others98,99 suggested that the thin layer formed produced, and dissipated afterwards. This layer would
between the electrode and the electrolyte during electro- be both thicker and less disturbed in the depression than
polishing was featured as a passivation film. the asperities. Thus, one may expect conditions for passiv-
A metal is considered to be in a passive state when the ity to be reached sooner in the depression part than on the
metal ions cease to dissolve to the surrounding electrolyte asperities, and the resulted great increase in anodic polar-
from the metal surface, even if a more positive potential isation in the depression would divert most current to the
than its oxidation potential is applied to the electrode. asperities. This statement, as drawn by Hoar and Father-
Usually, a fast increase in anodic potential with a sharp ing, was also in agreement with Evan’s theory.118
drop in current density at the onset of the electrochemical Interestingly, a later study led by Rowland123 indicated
passivity can be observed.32 that the observations in Hoar’s experiment could not be
The electrochemical passivation has been known since confirmed. In fact, a copper phosphate film was detected
the Faraday age. Early interpretations of this phenomena by electron diffraction afterwards.20 Therefore, the exact
suggested that the metal surface was oxidised to stop the nature of the film formed on the copper still remained
metal from continuous dissolving from the anodic side. In open to question then.
the case of the oxide films on some metals,118,119 it has The periodic oscillation of the current–voltage curve
been shown that the thickness was the order of a few Ang- before electropolishing conditions were established, as
stroms, and their growth was enhanced by oxidising observed by Hoar and Mowat99 was attributed to an
agents while diminished or prevented by halides or other alternate activation–passivation phenomena. Using silver
reducing agents. anode in cyanide plating bath,124,125 Francis and colner
On the basis of the similarity between the current–vol- recorded the periodic oscillations and observed the for-
tage curves of the electropolishing and those in many pas- mation and dissolution of the film on silver surface. It
sivation reactions, researchers postulated the formation of should be noted that the theory of alternate activation–
the transient passivation film, either salt or oxide, to par- passivation is actually inconsistent with Edward’s accep-
tially explain the phenomena in electropolishing.32 The tor theory. The viscous anodic layer, serving to screen
analogy between the oxidation of an easily oxidised the acceptors, was still basic and may determine the
metal, such as aluminium or zinc, and the electropolish- nature of the film observed in Hoar’s study.
ing has been illustrated by Napier and others.120 They
showed that the aluminium could be polished by placing
it in an anodic oxidation bath, or a bath which dissolved Ionic adsorption (Darmois theory)
the alumina film. A similar study on the formation of the Rowland found that, the noble metals (e.g. gold, platinum
passive layer on iron was performed by Tegart and and palladium) could be anodically polished in the mol-
others.121 They showed that the anodic processes involved ten salt, such potassium chloride or sodium chloride as
alternate passivation for the polishing of iron in sulphuric electrolyte under certain circumstance.123 He considered
acid at around 60–70°C and 4.5 volts. this phenomenon not explainable by postulating the
Hoar and Mowat99 made nickel anodic in a 50/50 sul- anodic layer of oxide, hydroxide, etc. on the anode,99
phuric acid/water bath. They found that there was a short because the substances corresponding to oxides would

be chlorides of the metals. In this case, the possibility of Improperly or inadequately cleaned parts are a frequent
oxide films due to dissolved oxygen was ruled out by the source of rejects. Chemical rinsing can remove any oil,
experiments in hydrogen and by the experiments in grease, shop dirt, fingerprints or similar films left on the
which polishing could occur at temperatures well above parts after manufacture. Surface contaminants present
those at which oxide could survive. He also made the on the parts during electropolishing can lower the quality
comment on Hoar and Farthing study,116 that the non- of the resulting finish, particularly for critical applications
adhesive of mercury droplet to the copper anode was such as medical, pharmaceutical and semiconductor pro-
not due to the formation of the anodic oxide film, but ducts. Once the parts are removed from the cleaner, care
to the failure to establish a contact-adsorbed film of mer- should be taken to avoid unnecessary contact with the
cury at higher current density than required by hands or process equipment. Alkaline cleaning proceeds
electropolishing. by a combination of chemical and physical reactions
Later, Darmois and others126 presented a theory of pol- involving displacement, flotation, penetration, wetting,
ishing which involves the adsorption on the anode of the emulsification and saponification of the contaminants.
anions from the electrolyte. As a specific example,127 in All of these reactions are sensitive to both time and temp-
the case of aceto-perchloric baths, the anode was pro- erature; therefore, care should be taken to make sure the
posed to become covered with a thin layer of ClO− 4 ions cleaning conditions fit the properties of the oil to be
that were capable of establishing an electrostatic field removed. Some soils may require little or no alkaline
intense enough to screen the metal ions. The authors soaking; others may require substantially higher tempera-
also eliminated any mechanism which involved the for- tures, soaking times and chemical concentrations to
mation of an oxide film. achieve cleanliness.
A rinse serves two primary functions in a metal finish-

ing system: (1) to remove by dilution the chemical residue
Pre-treatment and post-treatment from the previous operation, and, (2) to act as a barrier to
Prior to electropolishing, parts are mechanically prepared prevent drag-in to the following operation.23 Surface oxi-
to ensure optimal results. All welds are ground, deburred dation present on the parts during electropolishing can
and inspected to ensure that all seams are free of pockets affect the quality of the resulting finish, particularly for
or gaps.128 Workpieces to be polished may need necessary critical applications such as semiconductor, medical and
pretreating processes, including surface cleaning, surface pharmaceutical products. Alkaline drag-in from the clea-
modification and rinsing. The purpose of surface pretreat- ner tank will gradually destroy the total acid content of
ment is to remove contaminants, such as dust and films the electropolishing bath, causing quality problems.
from the substrate surface. The surface contamination Scale conditions and removal methods vary widely; how-
can be extrinsic, composed of organic debris and mineral ever, some care must be exercised to ensure that the
dust from the environment or preceding processes. It can method chosen is compatible with the electropolishing
also be intrinsic, such as a native oxide layer. Contami- bath and the overall design of the electropolishing line.
nants and films interfere with metal dissolution, which
can cause poor eletropolishing quality. Therefore, surface
pretreatment is important to ensure electropolishing qual- Electropolishing evaluation with
ity. Most (metal) surface treatment operations have three
basic steps: surface cleaning, surface treatment and
microscope
rinsing.128 The electropolishing in a general sense is to smoothen the
Cleaning methods should be able to minimise substrate metal surface finish of a metal by making it anodic in an
damage while removing the contaminants, dust, film and appropriate solution.1 It is commonly distinguished in lit-
or debris.129 Cleaning processes are based on two erature the anodic levelling or smoothing based on the
approaches: chemical approach and mechanical surface brightening. The more ‘shining’ metal surface
approach. Chemical approaches usually include solvent usually means a surface roughness of height < 1 µm,
degreasing, alkaline cleaning, soak cleaning and acid whereas the blunt surface finish indicates a surface rough-
cleaning, etc. For instance, if the metal surface contains ness >1 µm.132 This idea comes from the fact that, the
contaminants of oils, grease, waxes and miscellaneous wavelength of the visible light ranges between 400 and
organic materials, these contaminants can be removed 700 nm. Thus, if the elimination of the surface roughness
by appropriate organic solvents, either by dipping the results in morphology in sub-micron range, which is com-
workpieces in the solvent or by vapour decreasing. Some- parable with the light wavelength, a shining surface would
times, electrocleaning is also used. In electrocleaning, the appear. Edwards further introduced the terms micro-
surface of the workpiece is cleaned by chemical clean smoothing and macrosmoothing.39 These two processes
action by plentiful gas evolution.130 Mechanical are different from each other. The former results from
approaches include polishing, buffing and some vari- the suppression of the influence of surface defects and
ations. Polishing is to remove small amounts of metal of crystallographic orientation on the anodic metal dissol-
by means of abrasives. It produces a surface that is free ution process, while the latter, as aforementioned, is
of the larger imperfections left by grinding, and is a pre- caused by the concentration of current lines on peaks of
liminary to buffing. Buffing is similar to polishing, but a surface profile, which leads to a higher local dissolution
uses finer abrasives to remove very little metal. Buffing rate. These electropolishing surface finishes at different
can produce an extremely smooth surface. size scales require different techniques to evaluate.
Surface modification includes change in surface attri- Although not explicitly mentioned, most literature has
butes, such as application of (metal) layer(s) and/or hard- the microscopic evaluation on the electropolishing
ening.131 Cleanliness should be considered one of the finishes. For example, in Jacquet’s early works published
cardinal principles of all metal finishing operations. in Nature series on the electropolishing of copper, optical

microscope was used intensively to display the metal sur- further brought down to sub-nanometre range. For
face finishes after electropolishing.61,76 Most recently, instance, an electron microscope equipped with a 5 KeV
most publications related to the stainless steel electropol- electron source is capable to produce the electron
ishing use either scanning electron microscope (SEM) or irradiation of 0.248 nm. Atomic-resolution image could
atomic force microscope (AFM) or both to evaluate the even be generated with a sub-50 pm electro probe.135
surface finishes. Microscope technique is an indispensable Two types of electron microscopes are often used in elec-
diagnostic tool to evaluate the surface finishes of the tropolishing finishes evaluation. The first one is TEM,
specimen after electropolishing. This review will be the using which the high energy electron beam transmits
first of its kind, to provide the readership the overview through a thin specimen that is partially transparent to
of the microscopic evaluation on electropolishing tech- electron beam. The electron beam carrying the specimen
nique. The macroscopic smooth and the microscopic structural information, and the spatial variation of the
smooth of electropolishing, the two very important sample structural information can be viewed by either a
types of smooth that the electropolishing technique can fluorescent viewing screen or recorded by a charge-
provide are discussed. coupled device (CCD) camera.136 The second type of
electron microscope is scanning electron microscopy,
Optical microscope often abbreviated as SEM. It produces the images by
probing the specimen with a focused electron beam
In order to characterise and evaluate the surface mor-
which scans across a rectangular area on top of the
phology before/after the electropolishing process, many
sample surface, and it has been vastly applied to charac-
microscope techniques have been utilised. Optical micro-
terising the nanometre surface morphology.137–140
scopes are the oldest design among its category, and has
TEM has become a key tool to correlate the nature of
been intensively used to observe the electropolishing sur-
the microstructure of metals and the alloys directly with
face finishes. For example, in some of the Jacquet’s pio-
their important physical and chemical properties. The
neer electropolishing work,61,76 optical microscope was
metal specimen for TEM has to be delicately prepared
employed to show the surface brightness and crystal
in order to make it thin enough to let the electron transmit
grains of the copper anode (using polarised light source)
through.133 The thin metal foils are usually of a thickness
after electropolishing process.
of a few hundred nanometres or less.141,142 In addition,
In a study on the mechanism of electropolishing,
the successful TEM analysis highly depends on the qual-
Edwards made a copper composite anode with projec-
ity of the thin metal foils prepared. Although pure mech-
tions and recesses on the surface which were isolated
anical polishing technique exists to make the TEM thin
with each other. By using a binocular optical microscope,
specimen, the sample quality usually is hard to be fully
he could observe the smoothing effect preferably on the
controlled.143,144 Intensive studies have demonstrated
projections during electropolishing process, thus being
that an electropolishing step is necessary for TEM sample
able to quantitatively evaluate the electropolishing
preparation.133,143,145,146 Normally, the preparation of the
smooth efficiency.39
thin TEM specimen is composed of three steps, (a)
The optical microscope is also an important tool to esti-
obtaining a sample piece less than 2 mm thick, (b)
mate the sample quality used for more advanced electron
mechanically thinning the sample down to about
microscope. For instance, R. D. Schoone et al. develop an
0.2 mm and (c) further decreasing the sample thickness
electropolishing unit for preparing the thin metal speci-
down to nanometre range so that sufficient electron
mens for transmission electron microscope (TEM). The
beam penetration can occur.147
electropolishing finishes were evaluated using optical
The key factors of electropolishing, including voltage,
microscope. It was determined in their study that, under
current density, temperature, electropolishing duration
certain electropolishing conditions, the dislocations and
and convective flow rate need to be carefully optimised
stacking fault in pure cobalt existed, whereas fine metallic
in order for one to obtain an ideal TEM sample for repro-
grain structure was observed for Fe–Ni alloy.133
ducible observation. Necip148 prepared high quality pure
Despite the intensive employment of optical micro-
aluminium TEM samples through a double-jet electropol-
scope, its resolution is limited by the interference of the
ishing technique. Some useful hints to obtain the least fail-
visible light, which is about one half of the minimum vis-
ures in preparing the TEM specimen with optimum
ible light wavelength (200 nm).134 Thus, microsmoothing
electropolishing parameters were given in his study.
surface finishes after electropolishing process cannot be
Besides pure metal, the alloy microstructures are criti-
effectively evaluated by solely the optical microscope.
cally important for insight understanding of their mech-
Thus, other techniques should be resorted to if one
anical properties. For example, two phase TiAl alloy has
needs to perform characterisation on the microelectropol-
a great potential for aerospace applications due to its
ishing finishes below 200 nm.
excellent specific mechanical properties.149 Considerable
research effort has been dedicated to detailed characteris-
Electron microscope ation of TiAl on the microstructure-related mechanical
Restricted to light diffraction issue, traditional optical properties. A. Couret et al. 150 used a jet electropolishing
microscope could not be used to evaluate the surface fea- technique with a polishing solution composed of perchlo-
ture smaller than the light diffraction limit. However, if ric acid and methanol to prepare the TEM thin specimen.
the light source is changed by something with much A quantitative TEM analysis of the lamellar microstruc-
higher energy, the irradiation wavelength should be ture in the TiAl alloy could be performed due to the deli-
decreased accordingly. Based on this point, electron cate electropolishing specimen preparation process. Using
microscope became to play an important role in detecting a range of advanced methods combined with region
structures much smaller than light diffraction limit.134 specific replication entails and the electropolishing
With improved beam energy, the wavelength can be method, S. Sulaiman et al. 151 prepared TEM replica

specimens of P91 steel and carried out quantitative micro- One of many important applications of AFM in evalu-
analysis on the P91 steel specimen. ating the electropolishing metal surface is to directly offer
Despite its versatility in determining the thin specimen the information of the sample surface roughness, which
microstructure, TEM cannot be used to determine the cannot be fulfilled by electron microscopes. For example,
sample surface morphology. Thus, in order to determine Chi-Chang Hu et al. 91 studied the factors that affect the
the surface morphology after electropolishing, other tech- surface roughness (Ra) of 304 stainless steel (304 SS) elec-
niques should be used. SEM is such a tool, which utilises a tropolished in a mixture of phosphoric acid, sulphuric
high energy electron bean to scan the sample surface. acid and glycerol. The factor Ra was characterised by
After interaction with the sample, the electrons which using AFM height profile on the electropolished 304 SS
carry sample structural information are probed by elec- surface. They found that the bath temperature and polish-
tron detectors. As such, the sample surface structure can ing time were two key factors that affect the 304SS Ra. In
be revealed. a sister study of the same group, they found that the sur-
Didier Pribat et al. 152 used SEM to evaluate the electro- face roughness of 304 SS could be tuned from 7 to 45 nm
polishing effect on copper foil in H3PO4 bath at elevated by controlling electropolishing variables in glycerol-con-
temperature. The surface of the electropolishing finishes taining baths. The surface roughness, again was deter-
was analysed by a JEOL JSM-7600F field emission mined by the AFM height profile.43 T.M. Dahy et al. 153
SEM. The copper grain size on the specimen surface adjusted current density, duration, temperature and vis-
was analysed by the electron backscattering diffraction cosity in electropolishing process on commercialised cop-
(EBSD) images. They found that the copper foil electro- per foil, in order to remove the tarnishing and roughness.
polished at a small window near 65°C in 2.17 M H3PO4 The surface roughness of the electropolished copper foil
bath, exhibited a larger grain size than samples obtained was characterised by using AFM height images. Jerzy
under other conditions. In a similar study, T.M. Dahy Zak et al. 156 studied the electropolishing conditions on
et al. 153 removed the tarnishing and roughness of copper NiTi alloy. The quantity of the electropolishing ally sur-
surface with electropolishing treatment. The copper foil face was evaluated by AFM.
surface contamination and morphology were analysed In addition to the electropolishing surface roughness
by an SEM equipped with an energy-dispersive X-ray evaluation, AFM is also an important tool to characterise
(EDX) spectroscopy. the surface morphology of the electropolished metal sur-
In order to evaluate the corrosion behaviour of the 304 face. For instance, R.M. Metzger et al. 157 created highly
stainless steel at high temperature, hydrogenated water, ordered nanotopographies on aluminium single crystals
Paul C. Sander et al. 154 used SEM to observe the surface by electropolishing method. The ordered nanoscale mor-
nanocrystallinity of the stainless steel oxide layer. They phology on the single Al crystals was studied in details by
found that the stainless steel surface had small size (ran- AFM. Muhammad Aslam et al. 158 use the porous anodic
ging between 10 and 26 nm) chromite-based crystals rela- alumina pretreated by electropolishing process. Under
tive to the machined (i.e. cold worked) process. The different electropolishing voltage, they were able to create
electropolishing process, which removed surface macro- 100–150 nm random features (4–5 nm high) and 50 nm
strain by cold working, as stated by Paul C. Sander ordered nano stripes (1–2 nm high), which was confirmed
et al., exhibited a preferred reference surface condition. by the AFM images.
In another study on AISI-314 stainless steel electropolish-
ing, Sonia R. Biaggio et al. 83 employed the SEM at mag-
nification of 1000× to determine surface structure of the Electropolishing applications
electropolished samples. The surface of the samples, As aforementioned, electropolishing facilitates polishing
which were classified as opaque, semi-bright and bright the metal surface roughness, thus dramatically reducing
exhibited different surface morphology according to the the negative outcomes by the surface metallic dirt or pro-
corresponding SEM sample images. duct residues. For instance, the metal surface irregularities
often serve as the nucleation sites form cracks and
corrosion. Thus, the current stainless steel industry often
Atomic force microscope utilises electropolishing technique to enhance the anticor-
Despite the capability of determining small morphologi- rosion properties of the workpiece.90 Delstar Metal Fin-
cal features, SEM only provides two-dimension (2D) ishing Company is currently applying electropolishing
information of the surface finishes. In order to get through to some of its metallic products to reduce the coefficient
knowledge on the height profile, or roughness of the work- of the friction of metals, which improves the metal work-
piece after electropolishing, AFM is often used. Contrary piece life time. The surface rough irregularities can also be
to optical microscope and SEM, AFM does not use opti- nucleation for the bacterial attachment.89 Therefore, the
cal/electrical lenses or light/electron irritation. Instead, electropolishing on related metallic facility surface is of
the surface morphology information of the sample is great importance to pharmaceutical, food, beverage and
gathered by AFM tip (with the diameter in the order of biomedical industries to reduce the attachment of bac-
10 nm). By scanning on the sample surface, the mechan- teria. As an electrochemical surface finishing technique,
ical interaction between the tip and the sample is new commercial applications of electropolishing will be
converted to electric signal through a piezoelectric constantly found.
element, thus the sample topographical information is
recorded. The resolution of the AFM is not restricted
by light diffraction limit, and can reach the order of Finish
0.1 nm. Therefore, it becomes an important tool to Electropolishing is a reverse plating procedure that entails
study the microsmoothing of the workpiece after the electrochemical removal of metal impurities (includ-
electropolishing.43,155 ing carbon, silica and free iron) from a stainless steel

surface.40 The goal is a smooth surface, devoid of burrs or remove free iron or other foreign matter from the surface
crevices that attract and trap contaminants. During elec- of the metal and to create a chromium rich surface that is
tropolishing, the workpiece is fitted with electrodes, resistant to corrosion. However, passivation is generally
immersed in an electrolyte solution and subjected to a not effective in removing imbedded free iron and contami-
direct electrical current. During this electrolytic process, nants and will not remove heat tint or oxide scale on stain-
the metallic surface of the anodic part is preferentially dis- less steel.8
solved ion by ion, yielding a smooth surface.1 Optimal The electropolishing process dissolves the outer skin of
results depend on careful control over the current density, metal, removing deeply imbedded contamination.160
the precise chemical composition of the electrolytic sol- Heavily contaminated surfaces such as machined parts,
ution, the temperature and agitation of the bath and the welded or brazed assemblies or other components that
duration of current exposure.9 Finally, selected surfaces typically respond poorly to passivation alone, are good
are mechanically buffed to a smooth finish. candidates for electropolishing.161 Unlike passivation,
all stainless alloys including the 400 series and precipitat-
ing grades can be processed without distortion, flash
Corrosion resistance
attack or hydrogen embrittlement. Just as electropolishing
Electropolishing is widely specified to enhance corrosion is used to enhance corrosion resistance on stainless steel, it
resistance on a wide variety of metal alloys.36 Although offers corrosion resistance on other alloys as well. Electro-
most commonly used on stainless steels, electropolishing polishing can be used to delay or retard the corrosion
offers corrosion resistance on other alloys as well.159 properties of copper, brass, aluminium and carbon steels.
Due to the versatility and superior effectiveness, electro- On these and other alloys, the removal of surface skin and
polishing is fast becoming a replacement process for pas- impurities enhances the corrosion resistant properties of
sivation, a chemical process that has been used for years the component.162
to help restore contaminated stainless steel to original The following figure shows type 303 stainless steel
corrosion specifications. The intent of passivation is to (Fig. 9). After a series of machining operations, the
parts needed to be decontaminated to remove imbedded
steel and other impurities.
Under 40× magnification using the SEM, the passi-
vated part is actually rougher, due to the chemical attack
of the 303 stainless steel by normal passivation. In con-
trast, the electropolished part is smooth and clean. By
carefully monitoring the amount and rate of metal
removal, electropolishing dissolves the surface skin and
its impurities, including impinged steel flecks and other
contaminants.
Surface improvements
The most noticeable benefit of electropolishing is that it
provides an immediate brightening of a metal finish.1
By eliminating or minimising stains, heat discolouration
and minor scratches, electropolishing can bring out the
metal’s natural shine, which enhances the appearance of
the piece. In addition, electropolishing offers remarkable
ultracleaning capabilities through the removal of rust,
imbedded scale and other foreign debris.163 This can be
accomplished without stressing the piece or negatively
affecting surface hardness and integrity. By removing sur-
face imperfections, electropolishing can increase the
piece’s resistance to corrosion. That is because the elimin-
ation of imperfections can prevent the moisture that leads
to corrosion from accumulation. In fact, some salt spray
tests have indicated that electropolished pieces experience
greater corrosion resistance than passivated and raw
parts. Electropolishing can also effectively remove the
microscopic peaks resulting from processes such as weld-
ing, forming and stamping.164 The reduction of microfin-
ish values and accompanying increases in surface
smoothness can be extremely beneficial in the production
of valves and gears.165 The ability of electropolishing to
remove surface metal from a part makes it extremely
effective in the elimination of edge breaks. That is why
electropolishing is often preferable to vibratory finishing
9 SEM images of the stainless steel Type 303 before (upper or tumbling for use on delicate parts. Because electropol-
panel), during (middle panel) and after (lower panel) elec- ishing creates a smooth, clean surface that promotes
tropolishing process adhesion, it is sometimes used to prepare surfaces for

processes such as e-coating, plating, welding and phenomenon. Based on chronical order, the electropolish-
anodising.166 ing theorem includes Jacquet’s theory (resistance effect),
Conventional mechanical finishing systems tend to Elmore’s theory (diffusion effect), Edwards’ theory
smear, bend, stress and even fracture the crystalline (acceptor theory), Hoar and Farthings’ theory (passiva-
metal surface to achieve smoothness or lustre. Electropol- tion theory) and Darmois’ theory (ionic adsorption
ishing offers the advantages of removing metal from the theory).
surface producing a unidirectional pattern that is both For obtaining a better electropolishing result, the work-
stress- and occlusion-free, microscopically smooth and piece surface usually needs both pre-treatment and post-
often highly reflective. Additionally, improved corrosion treatment. After electropolishing process, the surface
resistance and passivity are achieved on many ferrous finishes can be evaluated by various microscopic tech-
and nonferrous alloys. The process micro- and macro- niques, depending on the surface roughness (i.e. micro-
polishes the metal part and micro-polishing accounts for electropolishing or microelectropolishing) and the needs
the brightness and macro-polishing accounts for the on the scale to be observed. The merits of electropolishing
smoothness of the metal part.167 includes the improvement of the metal surface smooth-
Deburring is accomplished quickly because of the ness, appearances, the surface corrosion resistance,
higher current density on the burr, and because oxygen removal of the contaminations and refinement of the sur-
shields the valleys, enabling the constant exposure of the face oxidation layer. Some of the surface feature of the
tip of the burr. Because the metal part is bathed in oxygen, metallic workpiece cannot be obtained by using tra-
there is no hydrogen embrittlement to the part.168 In fact, ditional mechanical polishing methods. Nowadays, the
electropolishing is like a stress-relieve anneal. It will application of electropolishing is not restricted to the
remove hydrogen from the surface.169 This is important improvement of the metal surface appearance for decora-
to parts placed under torque. Another benefit is that bac- tion purpose. The merits of electropolishing find much
teria cannot successfully multiply on a surface devoid of broader applications in metallic facility fabrication in
hydrogen, therefore, electropolishing is ideal for medical, food, beverage, pharmaceutic, biomedicine, electronic,
pharmaceutical, semiconductor and food-processing semiconductor, automotive, aerospace and many other
equipment and parts.170 The combination of no direc- industries. As time goes on, the electropolishing will con-
tional lines due to mechanical finishing, plus a surface tinue to play a vitally important role in processing various
relatively devoid of hydrogen, results in a hygienically metal surface finishes.
clean surface where no bacteria or dirt can multiply or
accumulate.
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Electropolishing of surfaces: theory and applications

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Guang Yang Kamal Tawfiq

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Electropolishing of surfaces: theory and

G. Yang, B. Wang, K. Tawfiq, H. Wei, S. Zhou & G. Chen

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© 2016 Institute of Materials, Minerals and Mining

1 Schematic illustration of a typical setup of the electrolytic

interphase. At the electrode surface, the dissolution

2 Surface Engineering 2016

Surface Engineering 2016 3

4 Surface Engineering 2016

Two potential issues are involved in the DC electrode-

also result in pitting issues. Taylor68 has developed a sur-

Surface Engineering 2016 5

the stainless steel would have a microscopically smoother

Table 1 Summary of major parameters of electropolishing process on copper workpiece

Current density Voltage Literature

Anhydrous orthophosphoric acid 25°C Not speciﬁed Not P.A. Jacquet81

6 Surface Engineering 2016

Table 2 Summary of major parameters of electropolishing process on stainless steel workpiece

Stainless Current Literature

 The effect of convection on the limiting current can be

Surface Engineering 2016 7

depression. In their study, an inverse relationship of cur-

Diffusion phenomena (Elmore theory)

importance of diffusion in the electropolishing process.

8 Surface Engineering 2016

is the coordinate parallel to the average surface plane. The

Surface Engineering 2016 9

area, and product of current density and time. It should

10 Surface Engineering 2016

A rinse serves two primary functions in a metal ﬁnish-

Surface Engineering 2016 11

12 Surface Engineering 2016

Surface Engineering 2016 13

14 Surface Engineering 2016

Surface Engineering 2016 15

5284554 A; 1994. production reproducibility of tungsten STM probe’, Sens. Actuat.

16 Surface Engineering 2016

83. L. S. Andrade, S. C. Xavier, R. C. Rocha-Filho, N. Bocchi and S. 291.

Surface Engineering 2016 17

18 Surface Engineering 2016

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The effect of convection on the limiting current can be