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Surface & Coatings Technology 202 (2008) 1668 – 1673

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Surface characterization of AISI 316L biomaterials obtained

by electropolishing in a magnetic field
T. Hryniewicz a,⁎, R. Rokicki b , K. Rokosz a
a
Politechnika Koszalinska, Division of Surface Electrochemistry, Raclawicka 15-17, PL 75-620 Koszalin, Poland
b
ElectroBright, Macungie PA, USA
Received 12 April 2007; accepted in revised form 16 July 2007
Available online 7 August 2007

Abstract

The paper deals with comparison of the results obtained by electropolishing AISI 316L surfaces in an externally applied magnetic field with those
of a standard electropolishing process. All electrochemical investigation methods, electrochemical impedance spectroscopy (EIS), polarization curve
measurements, and surface analytical methods such as surface roughness measurements and scanning electron microscopy were carried out to
determine the efficacy of electropolishing in a magnetic field.
© 2007 Elsevier B.V. All rights reserved.

Keywords: Magnetoelectropolishing; Modes of treatment; Stainless steels; Surface roughness comparison; Corrosion behaviour

1. Introduction and standard electropolished metallic surfaces. The most prom-

Electropolishing (ECP) [1–7] is one of the most important
surface treatment processes used for stainless steels. The ECP
process is governed by many different mechanisms and depends
on many parameters [1–4,6]. Given its variability, no single
theory for attaining the best electropolish covers all the com-
plexities. A modified technology [8–10] is proposed to obtain
bare metal surfaces for implants, stents and medical devices.
The effects of an externally applied magnetic field during ECP
(magnetoelectropolishing) of biomaterials, such as 316L vm
stainless steel, on their surface properties were investigated. The
results have been compared with standard electropolished bio-
materials in the same electrolyte under the same process con-
ditions. To evaluate surface properties, the following techniques
were used: SEM (Scanning Electron Microscopy), CAM (Contact
Angle Measurement), AES (Auger Electron Spectroscopy),
polarization curves, EIS (Electrochemical Impedance Spectros-
copy), and surface roughness measurements. These analyses
showed significant differences between magnetoelectropolished
⁎ Corresponding author.
E-mail addresses: Tadeusz.Hryniewicz@tu.koszalin.pl (T. Hryniewicz),
info@electrobright.com (R. Rokicki).
0257-8972/$ - see front matter © 2007 Elsevier B.V. All rights reserved.
doi:10.1016/j.surfcoat.2007.07.067
inent difference, which will likely have the most profound
implications on bio- and haemocompatibility, is difference in
static water contact angle as reported previously by the authors
[8]. The magnetoelectropolished surfaces show a remarkable
reduction of water contact angle, which in case of NitinolT,
resembles the water contact angle of pure titanium oxide.
2. Metallic biomaterials surface characteristics
In recent years, interest in metallic biomaterials such as
medical grade austenitic stainless steels, tantalum, and NitinolT
applications has been steadily growing [8–14]. The main reason
for this is their remarkable haemo- and biocompatibility prop-
erties and high corrosion resistance. The good biocompatibility
originates from their chemical surface film composition. The
medical grade AISI 316L vm stainless steel after electrolytic
polishing forms very thin, of a few-nanometer, compact oxide
film resistant against corrosion in the presence of physiological
human body fluids environments. A content of around 44%
titanium in NitinolT is responsible for the spontaneous creation
of very titanium rich oxide, which is also present on pure tita-
nium [7] and other titanium containing alloys. The oxide films
formed on metallic biomaterials are of paramount importance for
its biocompatibility in orthopaedic, dental and biliary [11–20]
 T. Hryniewicz et al. / Surface & Coatings Technology 202 (2008) 1668–1673
applications as well as haemocompatibility in cardiovascular
and peripheral stents and heart valves.
Whether it is a bare stent or with a coating material, 316L SS
is the most commonly used metal for stents. It has well-suited
mechanical properties and excellent corrosion resistance (carbon
content below 0.030 wt.%) making it the preferred material for
this application [21–26]. According to Mani et al. [26], out of the
eight coronary stents approved by the US Food and Drug
Administration (FDA), seven are made from 316L SS. However,
even if the supremacy of 316L SS platforms for making stents is
evident, biocompatibility is an issue with bare SS stents.
Surface characteristics of a stent material, which influence
thrombosis and neointimal hyperplasia, include surface energy,
surface texture, surface potential, and the stability of the surface
oxide layer [26,27]. The surface properties of a material usually
depend on the surface treatment. Different surface treatments
can produce different surface textures and surface chemistries on
the same material surface [27]. This can provide different surface
energies to the material surface. To improve the corrosion re-
sistance, different films (Ti or Ta) are coated on 316L SS
substrate by physical deposition sputtering [28]. However, when
the material is plastically deformed, cracks appear in the coating
[28]. This kind of acute change (cracking) in surface mor-
phology might pose a serious threat when the material is exposed
to in vivo conditions. The nature of the coating may be bio-
compatible, but, if the coating loses its integrity during the stent
placement and expansion, it may cause adverse effects.
The stability of the surface oxide layer directly influences the
biocompatibility of a material as the surface layer acts as a barrier
to the release of ions from the bulk materials underneath the
surface. Also the endothelial cell damage caused by the release
of very low concentration metal ions may be considered as a
potentially toxic effect [27]. The stability of oxide layer is also a
key to several of the surface characteristics. It influences surface
energy by providing hydrophilicity to a material surface [8,9]
and surface potential by preventing the release of electrons.
Since the stability of the natural surface oxide layer in 316L SS
(and NiTi) is not very high, the possibility of metal ion release is
enhanced.
The quest to develop totally passive metallic biomaterials, with
improved fatigue resistance properties continues. Among the new
approaches used to achieve this goal are: electrolytic polishing,
anodization, acidic and/or basic chemical etching, chemical
passivation, heat treatment in different gas atmospheres, ion
implantation, etc. [14–36]. All of these processes concentrate on
creating almost 100% Ni free amorphous, thin oxide film, which,
at least theoretically, should not create negative body response,
should be mechanically compatible with bulk constituents, and
should minimize Ni release to the host environment. Here we
would like to present some advantages and specific features
obtained after magnetoelectropolishing (MECP) [8–10], in
comparison with the surface after a standard electropolishing
(ECP).
The process of ECP in the presence of magnetic field has
been investigated by the authors previously [8–10,37–39]. The
ECP system with an externally applied magnetic field has been
utilized to enhance, or retard, the dissolution process. In this
1669
study, the ECP process has been carried out, first, on the plateau
level, and then under oxygen evolution regime. The purpose
of the work was to achieve an electropolished surface of the
sample exhibiting advantages of the treatment under different
conditions, concerning reduced microroughness, better surface
wetting and increased surface energy, reduced and more
uniform corrosion resistance, minimization of external surface
soiling and improved cleanability in shorter time periods.
3. Material and experimental procedures
3.1. Materials
The medical grade AISI 316L vm stainless steel, as the most
frequently used biomaterial, was used for the study. Two sets of
AISI 316L vm stainless steel samples punched of a sheet-steel of
about 2 mm thick and 18 mm in diameter have been used for the
investigations of mass loss vs. magnetic field strength, surface
film, roughness, wettability, corrosion behaviour, Auger and
other surface examinations. Also the standard ECP experiments
were carried out in parallel under the same conditions on the
same material cut to evaluate the differences between these two
processes. Mass loss study results, concerning the effect of a
magnetic field strength have been reported elsewhere by the
authors [8,9].
3.2. Electropolishing treatment
The studies of electropolishing were carried out under two
modes: (1) on the plateau level, and (2) beyond plateau, under
oxygen evolution regime (Fig. 1).
The electrolytic polishing was performed both in the absence
and in the presence of a magnetic field. For processing, both
rigid or flexible permanent magnets and electromagnets may be
applied. The effective magnetic field is assumed to be in the
range between 0.1 T and up to 1 T. For the experiments, a
constant external magnetic field below 1 T was applied to the
ECP system by neodymium ring magnets (Fig. 2). For both
processes, standard ECP and MECP, the same type of a pro-
prietary electrolyte was applied, being a mixture of sulphuric
and orthophosphoric acids. The bath was unstirred during the
process.
Fig. 1. Anodic polarization curve for AISI 316L stainless steel and the
modes of electropolishing: (a) on the plateau level, (b) in the range of oxygen
evolution.
1670 T. Hryniewicz et al. / Surface & Coatings Technology 202 (2008) 1668–1673
Fig. 2. Magnetoelectropolishing system schematic: A — anode, K — cathode,
M — magnet or electromagnet, W — steel wire of cylindrical shape.
3.3. Roughness measurements
A computerized HOMMEL TESTER T800 system of
Hommelwerke GmbH for roughness measurement was used
for the study of surface roughness. The comparison of the
roughness after both standard ECP and MECP were carried out
on the samples in two perpendicular directions.
3.4. Corrosion measurements
Corrosion studies after electropolishing on the plateau level
and beyond in the oxygen evolution regime were carried out in a
3% NaCl and in Ringer's solutions at 25 °C, both in the
presence (MECP) and absence (ECP) of a magnetic field.
During the study, both electrochemical impedance spectroscopy
(EIS) and measurement of polarization curves were performed
on the electropolished 316L samples surfaces. The electro-
chemical system used for the corrosion measurements consisted
of the potentiostat ATLAS 98 with the software IMP98, current
platinum electrode Ept-101, and the saturated calomel electrode
EK-101P used as a reference. The EIS results were obtained
each time after holding the samples at an open circuit potential
for 60 min.
Electrochemical impedance spectra can be evaluated using
so-called Nyquist plots in which the impedance Z is usually
Fig. 3. Results of surface roughness parameters Ra and Rz on AISI 316L vm
stainless steel samples, after: ECP — electropolishing, and MECP — magneto-
electropolishing (the plateau level mode).
Fig. 4. Results of surface roughness parameters Ra and Rz on AISI 316L vm
stainless steel samples, after: ECP — electropolishing, and MECP — magneto-
electropolishing (the oxygen evolution mode).
represented as a vector Z(ω) whose real part Re(Z) is plotted on
the x-axis and the imaginary part Im(Z) on the y-axis of the
complex plane whereby the vector Z(ω) forms an angle ϕ with
the real axis. A straight line parallel to the y-axis indicates a
perfect surface coating with zero corrosion whereas any cor-
roding surface displays a semicircle as the geometrical locus of
the impedance Z(ω) at one and only one frequency ω. Hence
the radius of the semicircle provides a measure of the corrosion
rate, i.e. a small radius is indicative of a high corrosion rate and
vice versa a larger radius signifies an increase in corrosion
resistance.
3.5. SEM surface examinations
Scanning electron microscopy was used to investigate the
surfaces of the stainless steel samples after ECP and MECP. The
apparatus used was Jeol ISN-550LV.
4. Experimental results
The magnetic field used in the electrolytic polishing is
affecting the surface roughness. Results of surface roughness
Fig. 5. EIS characteristics: corrosion results of 316L in Ringer's body fluid.
Electropolishing on the plateau level: a — after standard electropolishing, b —
after magnetoelectropolishing.
 T. Hryniewicz et al. / Surface & Coatings Technology 202 (2008) 1668–1673
Fig. 6. Polarisation curves: corrosion characteristics of 316L in Ringer's body
fluid. Electropolishing on the plateau level: a — after standard electropolishing,
b — after magnetoelectropolishing.
measurements, comprising two modes of electropolishing, on
the plateau level (a), and in the oxygen evolution regime (b), are
shown in Figs. 3 and 4, respectively.
The roughness measurements were performed on three pairs
of stainless steels samples electropolished in the absence (ECP),
and in the presence of magnetic field (MECP). Comparison of
the surface roughness results obtained after electropolishing
indicate no improvement in case of magnetic field used in the
process carried out on the plateau level (Fig. 3). On the other
hand, all surface roughness parameters (Ra, Rz, etc) have been
reduced after MECP beyond the plateau level, under oxygen
evolution mode of treatment (Fig. 4).
The corrosion behaviour of 316L vm sample surface was
also studied concerning two modes of electropolishing, on the
plateau level (a) and beyond (b), in the absence and in the
presence of magnetic field. The corrosion investigation results
obtained in Ringer's solution are presented in Figs. 5 and 6, and
show that there is no effect of the magnetic field, neither in the
EIS characteristics nor the polarization curves. Moreover, the
Fig. 7. EIS characteristics after electropolishing under the oxygen evolution
mode: a, b — corrosion results of 316L in 3% aqueous NaCl soln.: a — after
MECP, b — after ECP; c,d — corrosion results of 316L in Ringer's body fluid:
c — after ECP, d — after MECP.
1671
Fig. 8. Polarisation curves: corrosion characteristics of 316L SS in 3% aqueous
soln. NaCl after electropolishing under the oxygen evolution mode: a — after
standard electropolishing, b — after magnetoelectropolishing.
EIS results coming from the ECP on the plateau level appear to
be totally independent of the magnetic field applied during
electropolishing.
Hence more attention was paid to the process of electro-
polishing beyond the anodic curve plateau, under oxygen
evolution regime. The corrosion studies were carried out in two
solutions: Ringer's physiological fluid substitute solution, and
aqueous 3% NaCl solution, in both cases at 25 °C. The EIS
corrosion results of 316L vm sample, performed at a stationary
potential, are presented in Fig. 7.
The EIS results obtained for two different surface treatments
reveal a considerable difference in the corrosion behaviour of
the same 316L vm stainless steel sample surface. In case of 3%
NaCl solution, the Nyquist plots obtained indicate a better
corrosion resistance after ECP in the absence of magnetic field
(Fig. 7a,b), but, what is more important for biomaterials, a better
corrosion resistance after ECP in the presence of magnetic field
(Fig. 7c,d), is observed in the Ringer's solution.
Two pairs each of polarization curves, in 3% NaCl solution,
and in the Ringer's solution, are presented in Figs. 8 and 9,
respectively. A very slight change in the course of curve b
against curve a is observed in Fig. 8, meaning no basic corrosion
Fig. 9. Polarisation corrosion characteristics of 316L SS in Ringer's body fluid
after electropolishing under the oxygen evolution mode: a — after standard
electropolishing, b — after magnetoelectropolishing.
1672 T. Hryniewicz et al. / Surface & Coatings Technology 202 (2008) 1668–1673
Fig. 10. SEM micrographs of 316L vm samples: (a) after ECP, magnification
1000×, (b) after MECP, magnification 1000×.
improvement of 316L steel in 3% NaCl aqueous solution after its
magnetoelectropolishing. On the other hand, the same study
results in Ringer's body fluid (Fig. 9) show a considerable shift
on the potential axis, from − 1500 mV to about − 1000 mV
(curve b in Fig. 9), meaning there is an increase in corrosion
resistance of 316L after magnetoelectropolishing in comparison
with the same 316L SS after a standard electropolishing. These
polarization curves results well coincide with the results
obtained on Nyquist plots presented in Fig. 7.
Fig. 10 show SEM micrographs of 316L surfaces after
treatment in the oxygen evolution regime during ECP (Fig. 10a)
and MECP (Fig. 10b). A slightly smoother and darker 316L SS
sample surface has been obtained after magnetoelectropolishing
(Fig. 10b). The darker colour suggests (Fig. 10b) increased
surface energy as a result of a change in surface film composition
after MECP [39].
5. Discussion
The effect of an external magnetic field in ECP in two modes
of treatment was investigated. In the MECP process [8–10], an
externally applied magnetic field works in two distinctive ways:
either enhancing or retarding the rate of dissolution. The change
in dissolution rate does not depend on the magnetic properties of
the dissolved material or the composition of the electrolyte used.
Instead, it depends on the strength of the externally applied
magnetic field. It is important to note, however, that this effect
holds only when the electropolishing process is performed
below the oxygen evolution regime (plateau region), (see Fig. 1).
In the case of fixed-potential electropolishing performed beyond
the plateau current densities, in the oxygen evolution regime, the
experimental data show the process to be completely opposed to
the one described above.
The use of an externally applied magnetic field in the ECP
process provides the treated surface with some new properties
and better characteristics, concerning microroughness, hydro-
philicity, corrosion resistance, and oxide film morphology. The
higher level of metal finishing seems to be very interesting for
multiple applications, such as e.g. medical stents and implant
devices. The addition of the external magnetic field also dras-
tically minimizes microtopography by lowering microroughness
(see Fig. 4) and minimizing actual surface area in micro and
nanoscales of the various metallic materials [8].
From a practical point of view the more important features of
influence of a magnetic field used during an ECP process are the
alteration of morphology and chemistry of the finished surface.
The main reason for utilizing an ECP process is to improve the
quality of the treated surface and the incorporation of a magnetic
field during the ECP process provides an enhanced opportunity
to accomplish the desired results. These modified features of the
process can be observed in Fig. 4 and Fig. 10. It improves
corrosion resistance (Fig. 7) and prevents Ni ion leaching from
the bulk material to the host environment, which can be a
potential cause of allergic reaction.
Some other important findings were the corrosion results
obtained on 316L SS samples in aqueous 3% NaCl solution in
comparison with the results in the Ringer's body fluid. It appears
that the ECP carried out in magnetic field improves corrosion
resistance of 316L SS surface in the Ringer's solution, but
unfortunately it decreases the corrosion resistance in aqueous
3% NaCl solution. It is worth to find out what is the reason of
such a change in magnetic field effects. This fact requires further
study.
The studies excluded any reason for conducting the ECP
process on the plateau level. Much bigger discrepancy in the
surface roughness in two perpendicular directions has been noted
(see Fig. 3). On the other hand, no change in corrosion behaviour
between standard ECP and MECP was observed (see Fig. 5). That
may mean no change in the surface film obtained after MECP
process on the plateau level (without oxygen evolution).
It is known [40] that the surface layer of 316L SS after
electrolytic polishing (ECP) consists of oxides and hydroxides
of chromium and iron. The atomic ratio of Cr: Fe in the 316L SS
bulk equals 1: 3.63, the same ratio after abrasive polishing is 1:
2.10, whereas after standard electropolishing it equals 1: 1.71
[39,40]. Our own investigation of the 316L SS surface layer after
magnetoelectropolishing indicates on the ratio Cr: Fe to be 1:
0.71 [39]. It is much better than after a standard ECP but the
thickness of the surface film has changed drastically. It is well
known [1,2,4] that the thickness of the surface layer after many
mechanical and chemical treatments are about two orders higher
 T. Hryniewicz et al. / Surface & Coatings Technology 202 (2008) 1668–1673
(∼10− 7 m) than after electrolytic polishing (∼10− 9 m). After a
standard ECP it is still two to three times higher than the
thickness after MECP. It seems to be not only the composition of
the surface layer, that is much better after MECP with higher
contents of Cr2O3, to have a decisive influence on the 316L SS
corrosion behaviour.
A considerable change in corrosion behaviour of biomater-
ials electropolished in the presence of a magnetic field is
meaningful. This improved corrosion behaviour well coincides
with the Auger results of AISI 316L SS presented elsewhere
[39].
6. Conclusion
This study shows the difference in physical and chemical
properties between standard electropolished and magnetoelec-
tropolished biomaterials surfaces. All the above discussed
changes were achieved by applying a magnetic field to an ECP
process. The obtained results indicate more uniform surface
roughness and better corrosion resistance of 316L SS in the
Ringer's body fluid. These improvements may have a pro-
found influence on bio- and haemocompatibility of metallic
biomaterials.
An improved surface technology has been developed which
is the use of a magnetic field in the process of electropolishing
much beyond the plateau level. The promising results have been
presented concerning the basic biomaterial, the medical grade
stainless steel of type 316L. Since the general mechanisms
underlying the interaction between a metal and tissue/blood are
still not completely understood, the biocompatibility and haemo-
compatibility of metallic stents still remains an issue. These tasks
are expected to become the next step of the studies.
Acknowledgement
Mr Zbigniew Kuklinski is acknowledged for providing SEM
micrographs of the biomaterials surface examined (Fig. 10).
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