Received: 10 February 2017

| Revised: 10 February 2017

| Accepted: 6 March 2017

DOI: 10.1002/maco.201709478

ARTICLE

Corrosion properties of bioresorbable FeMn-Ag alloys prepared

by selective laser melting

M. Wiesener1 | K. Peters1 | A. Taube2 | A. Keller1 | K.-P. Hoyer2 |

T. Niendorf3 | G. Grundmeier1
1 UniversityPaderborn, NW-C, TMC, Warburger
Str. 100, D-33098 Paderborn, Germany
2 University
Paderborn, LWK, Warburger Str. 100,
D-33098 Paderborn, Germany
3 University
of Kassel, IfW-MW, Mönchebergstr. 3,
D-34125 Kassel, Germany
Correspondence
G. Grundmeier, University Paderborn, NW-C, TMC,
Warburger Str. 100, D-33098 Paderborn, Germany.
Email: guido.grundmeier@uni-paderborn.de
FeMn-Ag alloys as potential bioresorbable implant materials were prepared by
selective laser melting (SLM) from mixed powders of FeMn and Ag. The
microstructure of the samples is characterized by presence of few micrometers to
several tens of micrometer large Ag-phases within the FeMn matrix. The
microstructure dependent corrosion and biomineralization processes in simulated
body fluid (SBF) were studied in-situ by means of electrochemical impedance
spectroscopy (EIS). The microstructure and local surface film formation were
analyzed by electron microscopy (FE-SEM) and Raman microscopy. The results
clearly show that the Ag-phase acts as a local cathode within the FeMn matrix.
However, surface film formation is observed both for the Ag- and the FeMn-phases,
which potentially lowers the self-corrosion as well as the galvanic coupling of the
two phases. The formation of AgCl on the Ag-phases and mixed metal phosphates
on the FeMn-phases can be observed by local Raman spectroscopic analysis in
combination with FE-SEM characterization.

KEYWORDS
bioresorbable implant materials, corrosion and biomineralization, FeMn-Ag alloys, selective laser
melting, simulated body fluid

1 | INTRODUCTION the corrosion under physiological conditions. Hermawan et al.

The corrosion of bioresorbable metal alloys is of high interest
for the design of non-permanent implants such as stents.[1] In
many studies the corrosion of bioresorbable Mg-alloys has
been discussed.[2–4] In this case, the aim is to reduce the
corrosion current density in the early phase after implantation
as a too high corrosion rate with proton reduction as the main
cathodic process leads to an incompatibility of the implant.[5]
For Mg-alloys the change in the alloy composition and the
application of biocompatible inorganic or polymeric coatings
has been discussed.[2,6,7]
In comparison to Mg-alloys, iron based alloys show higher
mechanical strength and would allow for the design of smaller
implant structures.[8] On the other hand, the corrosion of pure
iron based alloys is much slower.[9] This motivated different
activities focusing on iron alloy design with the aim to increase
reported that FeMn alloys show an increased rate of corrosion
in physiological buffers in comparison to pure iron as
measured for example, by linear sweep voltammetry.[10,11]
However, so far it is not proven that dynamical electrochemical
measurements can predict long term static exposure of the
metal alloy in-vitro or even in-vivo.[5]
In addition to Mn as an alloying element the introduction
of additional phases of noble metals such as Pd or Ag has been
discussed.[12] The idea is that the noble metal acts as a cathode
thereby promoting the anodic corrosion of the matrix metal.
Indeed, Pd as nanoparticles in iron alloys proved to accelerate
the corrosion of the base metal at least in dynamic
electrochemical studies.[13,14] Recently, it was reported that
Ag-phases in iron alloys do not show a similar enhancement
in the corrosion within physiological electrolytes.[15] The
authors suggested that insoluble silver chloride forms at the

Materials and Corrosion. 2017;9999:1–9. www.matcorr.com © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim | 1
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| WIESENER
surfaces of the silver particles and acts as a barrier that
inhibits the microgalvanic corrosion.[15]
Selective laser melting (SLM) is an emerging technique
for the fabrication of highly complex components and metal
alloy implants based on the principal of additive manufactur-
ing.[16–18] It allows a design of metal alloys under non-
equilibrium conditions and a high variability of geometries.
SLM of iron alloy-based bioresorbable implants has been
recently introduced. In particular, Niendorf et al. showed that
Ag-phases can be well dispersed in FeMn-alloys using SLM
of mixed metal powders.[19] However, such complex alloys
have so far not been intensively studied with regard to their
corrosion mechanisms and kinetics in physiological electro-
lytes. Therefore, the aim of the presented work is the analysis
of the corrosion of FeMn-Ag alloys fabricated by SLM in
simulated body fluid (SBF). Time-resolved electrochemical
impedance spectroscopy (EIS) at open circuit potential has
been combined with the local analysis of the surface structure
by means of field emission scanning electron microscopy
(FE-SEM), energy dispersive X-ray spectroscopy (EDX), and
Raman imaging. The results reveal the role of phosphates and
chloride anions on the corrosion of the heterogeneous alloy
surface.
F I G UR E 1 Time resolved electrochemical analysis of the corrosion of
FeMn steel in SBF over 38 h; a) OCP transient; b) Bode plot of the EIS
data
ET AL.
2 | EXPERIMENTAL
2.1 | Materials
Samples of FeMn steel were fabricated by SLM as previously
described in ref.[19] Gas atomized powder was obtained from
commercial X-IP 1000 blanks, the initial chemical composition
is provided in ref.[20] Main alloying elements of X-IP 1000 are
about 22.4 wt% Mn, 0.6 wt% C, 0.3 wt% V, 0.2 wt% Cr, and
0.3 wt% Si. The SLM processed FeMn-Ag samples contained
5 wt% silver. A pure silver sample (99.999%, Goodfellow) and a
pure conventionally processed FeMn steel (X-IP 1000) sample
were used as references. All samples were polished iteratively
with SiC sandpapers having grit sizes P240, P600, P1000,
P2500, and P4000 to achieve a mirror-like finish. After
polishing, the sample surfaces were cleaned with cotton wool
soaked with ethanol abs. (p.a., Merck KGaA, Darmstadt,
Germany), followed by ultrasonic cleaning in ethanol abs. (p.a.,
Merck KGaA, Darmstadt, Germany) for 10 min in an ultrasonic
bath (Ultrasonic Cleaner, 45 kHz, 120 W, VWR International
GmbH, Darmstadt, Germany). Finally, the samples were rinsed
with ethanol abs. (p.a., Merck KGaA, Darmstadt, Germany) and
dried in a nitrogen stream.
F I G UR E 2 Time resolved electrochemical analysis of the corrosion of
FeMn steel in SBF over 38 h; a) development of the impedance at 0.1 Hz
and b) development of the impedance at 5 kHz
WIESENER ET AL.
| 3

2.2 | Chemicals FE-SEM imaging and EDX mapping of the samples before
and after the electrochemical treatment was performed to
For the electrochemical investigations, simulated body fluid
characterize the topography and composition of the surface
(c-SBF) containing 8.036 g/L NaCl (>99.5%, Merck KGaA),
and the passive layers, respectively, using a NEON 40 FE-
0.352 g/L NaHCO3 (>99.5%, VWR International), 0.225 g/L
SEM (Carl Zeiss SMT AG) at an acceleration voltage of 20 kV.
KCl (>99.5%, Merck KGaA), 0.23 g/L K2HPO4*H2O (>99.0%,
Raman spectra were measured by means of an InVia
Merck KGaA), 0.311 g/L MgCl2*6H2O (>98.0%, Merck
Raman spectroscope and a Leica DM 2500 M microscope
KGaA), 40 ml/L HCl (1 mol/L, Gruessing GmbH), 0.293 g/L
(Renishaw, Pliezhausen, Germany) with a He/Ne-Laser
CaCl2 (>98.0%, Merck KGaA), and 0.072 g/L Na2SO4
(532 nm) and a 50× objective to characterize the corrosion
(>99.0%, Merck KGaA), buffered at pH 7.40 at 36.5 °C with
products and the composition of the passive layers in addition
6.063 g/L TRIS (>99.9%, Merck KGaA) and 0.2 ml/L HCl
to the EDX investigations. Imaging Raman was based on the
(1 mol/L, Gruessing GmbH), was prepared according to
“Streamline-Mode” of the InVia system.
literature.[21]

2.3 | Analytical methods

3 | RESULTS AND DISCUSSION
The open circuit potential (OCP) and the electrochemical
impedance (EIS) were measured for 38 h in m-SBF at
37 °C with a Gamry Ref. 600 galvanostat/potentiostat (Gamry
3.1 | Electrochemical corrosion analysis
Instruments) and an Ag/AgCl (sat. KCl) reference electrode. The corrosion kinetics and the formation of surface layers
EIS was done in the frequency range from 10 000 Hz to 0.1 Hz were electrochemically analyzed by time resolved OCP and
with 10 points/decade versus OCP at an AC voltage of 10 mV EIS measurements over 38 h in SBF solution at a
rms employing a custom-made electrochemical cell with a cell temperature of 37 °C. The results of the electrochemical
diameter of 5 mm to pursue the build-up of the passive layers
and hence to characterize the electrochemical properties.

F I G UR E 4 Time resolved electrochemical analysis of the corrosion of

F I G UR E 3Time resolved electrochemical analysis of the corrosion of Ag in SBF over 38 h; a) development of the impedance at 0.1 Hz and b)
Ag in SBF over 38 h; a) OCP transient; b) Bode plot of the EIS data development of the impedance at 5 kHz
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| WIESENER
investigations of the FeMn steel alloy are shown in
Figures 1a,b and 2a,b).
The OCP of FeMn steel in SBF electrolyte shifted
anodically from a value of −0.35 V(SHE) to −0.10 V(SHE)
within 10-12 h of immersion. This could indicate a surface
layer formation, which decreases the anodic dissolution rate.
However, the EIS data showed an initial increase followed by
a decrease in the impedance at low frequencies reflecting an
acceleration of the interfacial corrosion process. In contrast,
the impedance at 5 kHz reveals that the surface layer
formation simultaneously increased over time from 13 to
22 Ω × cm2. Such a behavior might be explained by a change
from homogenous corrosion to pitting induced by the
promotion of the cathodic oxygen reduction current density.
The bare silver electrode showed a behavior that can be
interpreted by a porous surface film formation (see Figures 3a,
b and 4a,b). The OCP increased only slightly from 0.10 V(SHE)
to a limiting value of 0.12 V(SHE) (see Figure 3a). The EIS data
presented in the Bode plot (Figure 3b) shows only one time
constant. The polarization resistance increased from
1000 Ω × cm2 to 1700 Ω × cm2 within 38 h (Figure 4a)
indicating a blocking of the surface by a very thin film. The
corresponding EIS data are shown in Figure 4b.
F I G UR E 5 Time resolved electrochemical analysis of the corrosion of
the FeMn-Ag in SBF over 38 h; a) OCP transient; b) Bode plot of the EIS
data
ET AL.
As can be seen in Figure 5, the FeMn-Ag alloy shows a
rather constant OCP of −0.42 V(SHE) indicating an acceler-
ated metal dissolution and an only slightly increasing low
frequency impedance starting at 600 Ω × cm2 rising to
1300 Ω × cm2 over 38 h. At the same time, the impedance
at 5 kHz showed a surface layer formation similar to the
FeMn steel substrate indicated by an increase of the
impedance from 15 to 25 Ω × cm2 (Figure 6).
3.2 | Microstructure analysis
FE-SEM images of the surface morphology of FeMn steel,
Ag and FeMn-Ag before and after 38 h of immersion in SBF
are shown in Figure 7a–f.
The electron microscopic analysis (Figure 7) shows
pitting especially for the FeMn steel alloy. However, also the
pure Ag-substrate shows pitting along with a distinct surface
roughening. The FeMn-Ag substrate shows enhanced pitting
in the FeMn-areas while the surface morphology of the Ag-
phase is almost not affected by the corrosion process. These
results are in good agreement with the electrochemical data
F I G UR E 6 Time resolved electrochemical analysis of the corrosion of
the FeMn-Ag alloy in SBF over 38 h; a) development of the impedance at
0.1 Hz and b) development of the impedance at 5 kHz
WIESENER ET AL.
| 5

F I G UR E 7 FE-SEM images of the FeMn steel sample (a,b), the pure silver sample (c,d), and the FeMn-Ag sample (e,f) before (left) and after (right)
the electrochemical investigations

shown before. The Ag-phase in the FeMn-Ag substrate is
cathodically protected by the actively dissolving FeMn-
phase.
Table 1 shows the integral composition of the substrates
before and after the immersion as measured by EDX.
Concentrations of Fe and Mn in the area of the silver particle
in the silver containing FeMn steel sample are due to the high
penetration depth of the electron beam.
Before the exposure to SBF (“as prepared”), the substrates
show the expected compositions. Neither P nor Cl were
detectable on any of the studied substrates. The EDX analysis
did not allow for a perfect separation of the Ag-phase in the
FeMn-Ag alloy. This explains the simultaneous detection of
Ag, Fe, and Mn. However, the observed increased Mn/Fe ratio
could hint at a partial alloying of Mn with Ag. After the
immersion in SBF for 38 h, the Ag-substrate shows a strong
contribution of chlorides indicating the formation of a AgCl
layer. Phosphates and oxides were not detected on the bare Ag-
substrate. In comparison, the FeMn steel substrate shows
substantial concentrations of oxygen and phosphor which are
assigned to oxide and phosphate formation on the FeMn-alloy.
Only negligible chloride concentrations were observed in this
case which can be explained by the high solubility of Fe- and
Mn-chlorides.[22]

TABLE 1 Composition of the substrate surface near regions for the various materials tested
Metal substrates as prepared (at%) Metal substrates after 38 h immersion in SBF (at%)

Fe Mn Al Ag O P Cl Fe Mn Al Ag O P Cl
FeMn steel 71.4 20.5 2.0 – – – – 65.5 18.3 1.9 – 3.5 0.6 –
Ag – – – 99.1 – – – – – – 51.6 – – 48.1
FeMn-Ag (Ag-phase) 3.5 14.5 0.6 80.9 – – – 1.6 9.8 0.3 42.7 44.1 0.6 –
FeMn-Ag (FeMn-phase) 72.8 21.6 – 0.2 – – – 55.0 16.8 0.1 0.4 12.7 0.7 0.1

For the SLM processed sample in particular the silver particles as well as the Fe/Mn area were characterized; difference to 100 at% are due to trace elements (e.g., Na, Ca, C,
etc).
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| WIESENER
Finally, the Ag-phase in the FeMn-Ag sample also shows
the expected element concentrations for a galvanic couple of
FeMn and Ag. The negligible chloride concentrations even in
the analyzed volume containing the Ag-phase can be explained
by the cathodic polarization of the Ag-phase which is polarized
to a potential more negative than the free corrosion potential of
silver in SBF. This inhibits the anodic dissolution of Ag which
would be necessary for the formation of a AgCl surface layer.
Instead, the local oxygen reduction on the Ag-phase leads to
the deposition of mixed metal oxides and phosphates caused by
the locally increased interfacial pH-value.
The EDX mapping of the FeMn-Ag substrate within
the area shown in the FE-SEM image (see Figure 8)
proves that a corrosion product layer formation takes
place covering both the matrix and the Ag-phases. While
the low concentrations of P and Cl did not allow for the
clear distinction between the FeMn- and the Ag-phase, the
substantially increased oxygen concentration on the Ag-
phase indicates that oxygen reduction on the Ag-phase
during galvanic coupling leads to the . Based on the low
solubility of iron and manganese oxides and phosphates it
F I G UR E 8 EDX mappings of the FeMn-Ag sample after immersion in SBF for 38 h showing the distribution of Fe (a), Mn (b), Ag (c), O (d), P (e), and Cl (f)
ET AL.
is likely that Fe and Mn ions dissolved from the FeMn-
phase are redeposited as oxides and phosphates on the Ag-
phase acting as local cathode.
3.3 | Raman spectroscopic investigations
Complementary to the FE-SEM EDX data, Raman micros-
copy illustrates the local corrosion product formation at a
similar length scale, however, with an improved surface
sensitivity. The spectra are shown in Figures 9 and 10. Table 2
provides an overview of the assignments of the observed
peaks.
The FeMn steel substrate shows iron[23] and manganese
oxides[24] even in the as-prepared state. This is due to the
fast atmospheric oxidation of the FeMn steel. After
immersion in SBF over 38 h, in addition to Fe and Mn-
oxides phosphates could be detected on the surfaces,
indicating the formation of a passivating surface film as
detected by EDX.[25]
The pure silver substrate shows the formation of silver
chloride[26] after the immersion in SBF in agreement with the
WIESENER ET AL.
EDX-data. Moreover, the spectra show carbon D/G-bands
most probably caused by atmospheric contamination and
Raman laser induced degradation to graphite-like species.[27]
The rough Ag-phase might in this case even enhance the
signal due to surface plasmon resonance effects.[28]
In Figure 10, the Raman spectra for the FeMn-Ag sample
before and after the 38 h immersion in SBF are shown. In the
area of the FeMn-phase, clearly Mn-, and Fe-oxides cause
the dominating peaks. In combination with the EDX-mapping
the peaks in the area of the Ag-phases are mainly assigned to
Ag, Fe-, and Mn-oxides. The reason for the formation of the
Ag-oxides is assumed to be induced by the local alkaline pH
that forms during the cathodic oxygen reduction.[29]
Moreover, a Raman image of the area including the Ag-
phase shows the inhomogeneous distribution of the phos-
phates (see Figure 11a,b) based on the intensity distribution of
the PO2 symmetrical stretching mode at 1050 cm−1.[25] The
phosphate peak did not overlap with the oxide peaks which
allowed for the imaging analysis. A preferential phosphate
formation is observed in the vicinity of the Ag-phases. This
F I G UR E 9 Raman spectra of the FeMn steel (a) and the pure silver
sample (b) before and after the exposure in SBF over 38 h
| 7
observation can be explained by the contribution of the
electrolytic resistance of the SBF electrolyte to the galvanic
coupling. With increasing distance to the Ag-phase the FeMn
is more and more decoupled. This leads to an inhomogeneous
corrosion current density distribution with an enhanced
corrosion of the FeMn-phase next to Ag as the local cathode.
The high ion transfer rate in this area promotes the deposition
of quite insoluble metal phosphates.
4 | CONCLUSIONS
The electrochemical and microscopic results prove that the
Ag-phase in the FeMn-alloy performs as a local cathode
which promotes the anodic dissolution of FeMn mainly in the
initial phase of corrosion in SBF solution. In the early states of
corrosion, the oxygen reduction on the Ag-phase leads to both
an increase in the dissolution of the FeMn-alloy especially
close to the Ag-phase and to a local increase of the pH-value
on the Ag-phase. This local pH-increase and the cathodic
F I G UR E 1 0 Raman spectra of (a) the FeMn surface (about 50 µm
distance to the Ag-phase) and (b) a Ag particle of the FeMn steel sample
containing 5 wt% silver before and after the immersion in SBF for 38 h
8
| WIESENER ET AL.

TABLE 2 Overview on the assignment of the observed peaks for the pure metal samples and the different metal areas on the FeMn-Ag sample before and after
exposure to SBF
Peak position/cm−1 Assignment Reference Peak position/cm−1 Assignment Reference
[23] [26]
210–220 FexOy/FeOOH 219 Ag-O stretching/bending mode
238/239 237
334 316
605–625 519
684 607/608
[26]
817 220–240 Ag-Cl stretching modes
1280–1290
[24]
270–285 Mn3O4
[25]
385–395 492 POx stretching mode
[30]
1285–1380 Carbon, D-band 1050
1084
[30]
1550–1600 Carbon, G-band

potential shift on the Ag-phase inhibits the formation of silver
chloride surface layers and promotes the deposition of mixed
metal oxides on the Ag-phase. Simultaneously the acceler-
ated anodic dissolution of the FeMn-phase galvanically
coupled to the Ag-phase leads to the formation of corrosion
scales based on oxides and phosphates. Phosphates are
mainly formed close to the Ag-phase as confirmed by Raman
imaging based on the inhomogeneous distribution of the
corrosion current density. However, this surface layer
formation leads to an inhibition of the galvanic corrosion
current densities with increasing time of immersion.
Moreover, the pitting observed for the isolated Ag-phase
and the concurrent AgCl-surface film formation might
suggest that released Ag-particles from the FeMn-Ag-alloy
are slowly resorbed based on a self-corrosion process that is
limited by the low solubility of surface chlorides.

ACKNOWLEDGMENT
The authors thank Dipl.-Chem.Ing. Nadine Buitkamp for the
support with the EDX measurements.

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sample after the exposure to SBF
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How to cite this article: Wiesener M, Peters K,
Taube A, et al. Corrosion properties of bioresorbable
FeMn-Ag alloys prepared by selective laser melting.
Materials and Corrosion. 2017;9999:1–9. https://doi.
org/10.1002/maco.201709478