International Journal of Fatigue 26 (2004) 1129–1136

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Technical Note
Effect of precipitates on the corrosion–fatigue crack initiation
of ISO 5832-9 stainless steel biomaterial
E.J. Giordani a,
, V.A. Guimarães b, T.B. Pinto a, I. Ferreira a
a
Departamento de Engenharia de Materiais, Faculdade de Engenharia Mecânica, Universidade Estadual de Campinas, Caixa Postal 6122,
CEP 13083-970 Campinas, SP, Brazil
b
Faculdade de Engenharia e Arquitetura, Universidade de Passo Fundo, Caixa Postal 611, CEP 99001-970 Passo Fundo, RS, Brazil

Received 7 July 2003; received in revised form 21 January 2004; accepted 3 March 2004

Abstract

The correlation between the microstructure and fatigue crack initiation behavior (in air and 0.9% NaCl solution) of ISO 5832-9
austenitic stainless steel biomaterial was investigated. A combination of techniques such as extraction of precipitates, SEM, EDS
and X-ray diffraction was found to be very useful to characterize Z-phase precipitates, which are abundant in this steel. An analy-
sis of fatigue crack initiation, using SEM, revealed that fatigue and corrosion–fatigue cracking initiate preferentially in the elon-
gated Z-phase precipitates, which are parallel to the tensile direction, and in coarse precipitates usually associated with Al-rich
nonmetallic inclusions. Crack initiation is caused by particle rupture rather than by separation of the particle/matrix interface.
The findings indicate that coarse Z-phase precipitates and nonmetallic inclusions are detrimental to the fatigue properties of the
steel. These microstructural constituents accelerate the initiation of fatigue and especially corrosion–fatigue cracks.
# 2004 Elsevier Ltd. All rights reserved.

Keywords: Biomaterial; Stainless steel; Corrosion–fatigue; Crack initiation

1. Introduction in orthopedic applications, mainly when the implanted

Some metals and alloys that combine high strength
with reasonable corrosion resistance are favorite bio-
materials for the fabrication of orthopedic implants,
which are subjected to severe mechanical loading inside
the human body. The metallic biomaterial most com-
monly used for orthopedic applications today is the
austenitic stainless steel classified as ASTM F138
(a special type of 316L steel for medical applications)
[1]. Its utilization is particularly justified by the combi-
nation of properties such as good acceptance by the
body; low cost; good machinability; good formability;
high strength, especially when cold worked, and
reasonable corrosion resistance. However, some aspects
such as low strength in the annealed condition and sus-
ceptibility to localized corrosion (pit and crevice cor-
rosion) often limit the wider use of this type of material


Corresponding author. Tel.: +55-19-3788-3312; fax: +55-19-3289-
3722.
E-mail address: enricogiordani@uol.com.br (E.J. Giordani).
0142-1123/$ - see front matter # 2004 Elsevier Ltd. All rights reserved.
doi:10.1016/j.ijfatigue.2004.03.002
device must remain in the human body for a relatively
long time (more than 12 months). The combination of
such aspects favors the failure of orthopedic implants
by a synergy called as corrosion–fatigue. This synergy,
which combines the electrochemical effects of corrosion
and the mechanical effects of cyclic loading, has been
cited in specialized technical reports as the main cause
of fracture of metallic orthopedic implants [2–4], parti-
cularly those used in the lower extremities of the
human body, where implants are subjected to more
severe cyclic loading. The fatigue or corrosion–fatigue
life of a device is the time or number of cycles required
for cracking to initiate and to propagate until the final
fracture occurs. Fatigue life takes longer to produce a
crack measuring just a few micrometers than does the
propagation of that crack; thus, detailed studies of the
mechanisms which rule fatigue or corrosion–fatigue
crack initiation are extremely important.
Research aimed at developing new metallic materials
to offset the limitations of austenitic stainless steel led
1130 E.J. Giordani et al. / International Journal of Fatigue 26 (2004) 1129–1136
to the development of the chromium–cobalt alloys
in the 1930s and of titanium and its alloys in the 1960s.
However, high cost, low formability and poor machin-
ability were some of the limitations preventing the
unrestricted use of these metallic materials for orthope-
dic applications. More recent studies have led to the
development of a new type of high nitrogen austenitic
stainless steel, ISO 5832-9, which combines high
strength, even in the annealed condition, and high cor-
rosion resistance, making it a promising substitute for
F138 steel in the manufacture of orthopedic implants,
particularly for applications involving heavier loading
and longer periods inside the human body.
Based on the constant need to gain a better under-
standing of the fatigue and especially the corrosion–fati-
gue crack initiation mechanisms, which have been
reported as the main mechanisms of crack failures
in orthopedic implants, this paper reports on the micro-
structural characterization and study of fatigue crack
initiation mechanisms of an austenitic stainless steel, ISO
5832-9, in both neutral and aggressive environments.
2. Materials and methods
The material used in this study was an austenitic
stainless steel, ISO 5832-9 (ASTM F 1586), annealed at
v
1030 C for 1 h, used for orthopedic implants. The
chemical composition and the main mechanical proper-
ties of this steel are listed in Table 1.
The study to characterize this steel was motivated by
the significant amount of precipitated particles in its
microstructure. The study involved the precipitate
extraction technique with electrolytic dissolution of the
austenitic matrix in a methanol solution containing
10% HCl. The extracted residue was analyzed using a
JEOL JSM-5900LV scanning electron microscope
(SEM) to characterize the precipitate morphology, a
Noran Voyager 3050 energy dispersive spectroscope
(EDS) to identify the phase composition, and a Philips
PW-1700 X-ray diffractometer to determine its unit cell
dimensions.
Axial fatigue tests were conducted based on the
ASTM E 466 standard. Fig. 1 shows the dimensions of
the specimens. The gage sections were mechanically
polished with diamond paste (1 lm). S–N curves
Table 1
Chemical composition and mechanical properties of ISO 5832-9 stainless steel
Chemical composition (mass %)
C Mn Ni
0.0316 3.83 11.0
Mechanical properties
Yield strength ðoffset ¼ 0:2%Þ (MPa) Tensile strength (MPa)
496 861
were determined using a computer-controlled servo-
hydraulic MTS machine and the tests were carried out
with sinusoidal loading control, with a stress ratio of
0.01 and a frequency of 10Hz. The test environments
were neutral (air) and aggressive (0.9%NaCl aqueous
v
solution at 37  1 C). An acrylic chamber was
developed to conduct the aggressive environment tests,
where the specimen gage length was immersed in the
aqueous solution while it was cyclically loaded (Fig. 2).
Electrolyte (1500 ml) was heated in a bath and pumped
through the chamber. The electrolyte was replaced for
each new test. The specimens were used both to deter-
mine the S–N curves and to carry out fatigue and cor-
rosion–fatigue tests which were interrupted after the
first cycle at 10, 20, 30, and 50% of the expected life
span for a cyclic load of 600 MPa.
The fatigue crack initiation mechanisms were studied
microscopically, using secondary electron imaging
(SEI) and backscattered electron imaging (BEI) in the
SEM. Gage sections of the specimens tested in air and
in aqueous environments were extracted and their lat-
eral polished surfaces and fracture surfaces were ana-
lyzed. Some of the specimens were electrolytically
etched with HNO3 to reveal grain boundaries.
3. Results and discussion
3.1. Microstructure
Fig. 3 illustrates the microstructure of the ISO 5832-
9 steel in the longitudinal section, revealing the presence
of a large amount of precipitated particles dispersed
in the austenitic matrix. Coarser particles were pre-
ferentially elongated and were mostly located along the
grain boundary and parallel to the rolling direction.
EDS analyses revealed that these precipitates were rich
in Nb and Cr. Fig. 4 shows an aspect of the steel’s
microstructure: the presence of coarse Nb and Cr-rich
precipitates associated with nonmetallic Al-rich inclu-
sions (probably alumina–slag resulting from the deoxi-
dation process), revealed by EDS.
The technique for extracting precipitates by phase
dissolution associated with SEM helped to morphologi-
cally characterize the precipitates present in the micro-
structure of the ISO 5832-9 steel. Fig. 5a shows some
Cr Mo N Nb Fe
22.6 2.41 0.291 0.42 balance
Elongation (in 25 mm) (%) Vickers hardness
46 244
 E.J. Giordani et al. / International Journal of Fatigue 26 (2004) 1129–1136 1131

Fig. 1. Shape and size of the axial fatigue specimen (in mm).

Fig. 2. Cell used in the axial fatigue test in the aggressive environ-
ment.

Fig. 5. Precipitates extracted from ISO 5832-9 steel: (a) coarse

plate-like precipitates (SEM/BEI); (b) varied morphology and size of
precipitates (SEM/SEI).

of the extracted precipitates on the filter’s membrane.

As can be observed, the larger precipitates show a
plate-like morphology. These particles appear to be
elongated and parallel to the rolling direction on the
longitudinal surface (Fig. 3). Fig. 5b shows a large
amount of precipitates of varied sizes and shapes. EDS
analyses revealed that the extracted precipitates had a
relative chemical composition of metallic elements close
to 63% Nb, 32% Cr and 5% Fe (wt%) or 49% Nb, 44%
Cr and 7% Fe (atomic%), irrespective of the particles’
size or morphology. Therefore, it is logical to suppose
Fig. 3. SEM/BEI micrograph of a longitudinal section of ISO 5832-
that all the analyzed precipitates were of the same phase.
9 steel. An X-ray diffraction analysis of the extracted residue
confirmed the existence of Z-phase precipitates with a
tetragonal structure and lattice parameters of a ¼ 3:035 G
and c ¼ 7:380 G, which were first identified by Hughes [5]
and later reformulated by Jack and Jack [6]. Z-phase is a
complex nitride of niobium and chromium with unit cells
containing Nb2Cr2N2. In the present work, the chemical
composition of the extracted precipitates showed a small
amount of Fe replacing the Cr atoms in the lattice, as did
Örnhagen et al. [7], who investigated two alloys in con-
formity with ISO 5832-9 standard, but unlike those
authors, no evidence of Mo replacing some of the Nb
atoms was found. The most probable composition of the
Z-phase in the present steel is Nb2(Cr, Fe)2N2.

3.2. Fatigue properties

Fig. 6 illustrates the S–N curves for the ISO 5832-9

Fig. 4. SEM/SEI micrograph of coarse Nb-rich precipitates associa- steel obtained from fatigue tests in air and in the
ted with Al-rich nonmetallic inclusions. aggressive environment.
1132 E.J. Giordani et al. / International Journal of Fatigue 26 (2004) 1129–1136
Fig. 6. S–N curves for ISO 5832-9 steel in air and in 0.9% NaCl sol-
v in air and in aggressive environments have been found.
ution at 37 C.
It is important to state that the levels of maximum
cyclic stress used to determine the fatigue curves were,
in every case, equal to or higher than the yield strength
of the steel (Table 1). Hence, the specimens underwent
plastic deformation mainly in the first loading cycles.
As can be observed, the aqueous environment exerts a
marked influence on the steel’s fatigue life which is
further reduced with an increasing number of cycles to
failure or even with longer testing time, since the fre-
quency used is the same for all the specimens. This
aspect is considered attributable to the corrosion–fati-
gue synergy. It is presumed that corrosive environ-
ments merely help the formation of geometrical
discontinuities on the previously smooth surface of the
specimen, thereby favoring crack initiation [8]. Because
this process is time-dependent, it is logical to assume
that the influence of the aggressive environment on the
material’s fatigue life increases as the metal is subjected
to prolonged exposure in a given environment.
3.3. Fatigue crack initiation mechanisms
Understanding how a metal’s microstructure influ-
ences fatigue and corrosion–fatigue endurance is parti-
cularly important for the development of alloys and of
thermal or thermomechanical treatments aimed at
improving the performance of the material under cycli-
cal loading conditions in neutral or aggressive environ-
ments through microstructural modifications. A good
understanding of the correlation between the micro-
structure and corrosion–fatigue behavior can also be
useful to identify the mechanism whereby the aggress-
ive environment contributes to the initiation and
propagation of a fatigue crack [9].
The study of the fatigue and corrosion–fatigue crack
initiation mechanisms aimed to identify the preferential
sites for crack initiation and the microstructural parti-
cularities and/or peculiarities associated to these sites
that are possibly responsible for precocious fatigue or
corrosion–fatigue crack initiation, thus contributing to
reducing the fatigue life of ISO 5832-9 steel.
A point worth noting is that no evidence of localized
corrosion (pits) was found on the surface of specimens
tested in the aggressive environment. Therefore, the
hypothesis that the crack initiation mechanism resulted
from the formation of corrosion pits, as verified by
Qian and Cahoon [10] in a commercial type 316 stain-
less steel in an aggressive environment (0.5 M NaCl at
pH ¼ 4:2), was discarded for the test condition used
here. However, some researchers have observed the
occurrence of the corrosion–fatigue synergy in environ-
ments where pit corrosion does not usually occur [11].
Another important aspect is the fact that no relevant
differences between fatigue crack initiation mechanisms
The analysis of secondary cracks on the lateral surface
of the specimens revealed that the preferential sites for
both fatigue and corrosion–fatigue crack initiation
were coarse Z-phase precipitates associated or unasso-
ciated with Al-rich inclusions as shown in Fig. 7. An
analysis of the surface of a specimen loaded in air with
a maximum cyclic stress of 600 MPa revealed the pres-
ence of geometric discontinuities, which already
occurred in the first loading cycle and were associated
with the fracture of elongated Z-phase precipitates
(Fig. 8a) and nonmetallic inclusions surrounded by Z-
phase precipitates (Fig. 8b). These geometric dis-
continuities act as stress and strain concentrators and
contribute to precocious fatigue crack initiation.
No fatigue cracking was found propagating into the
matrix in specimens tested in air at 10% (17,500 cycles)
and 20% (35,000 cycles) of expected fatigue life. Crack-
ing was observed only in tests interrupted at 30%
(52,500 cycles) and 50% (87,500 cycles) of expected
fatigue life, as illustrated in Fig. 9. Cracking in speci-
mens tested in the aggressive environment was already
visible at 10% (6000 cycles) of the expected fatigue life,
as illustrated in Fig. 10a. Both in air and in the
aggressive environment, the larger and more precocious
cracks were found to initiate in coarse elongated pre-
cipitates or clusters of precipitates usually associated
with Al-rich inclusions.
The aggressive environment caused the crack
initiation period to drop from approximately 50,000
cycles to about 6000 cycles. In the aggressive environ-
ment, the larger cracks displayed an average length of
approximately 100 lm (Fig. 10b) 24,000 cycles (40% of
the expected fatigue life under this condition) beyond
the period required for the initiation of the first cracks
(at 10% of the expected fatigue life). On the other
 E.J. Giordani et al. / International Journal of Fatigue 26 (2004) 1129–1136 1133

Fig. 7. Sites of corrosion–fatigue crack initiation at a maximum

cyclic stress of 550 MPa: (a) elongated Z-Phase precipitate (SEM/ Fig. 9. Crack initiation sites in ISO 5832-9 steel in air for interrup-
BEI); (b) coarse Z-Phase precipitate associated with Al-rich inclu- ted tests at a maximum cyclic stress of 600 MPa: (a) at 30% (52,500
sions (SEM/SEI). cycles) of expected fatigue life; (b) at 50% (87,500 cycles) of expected
fatigue life (SEM/BEI).

Fig. 8. Geometric discontinuities created from the fracture of Z-

phase precipitates in air in the first cycle at a maximum cyclic stress Fig. 10. Crack initiation sites in ISO 5832-9 steel in the aggressive
of 600 MPa: (a) associated with an elongated Z-phase precipitate; (b) environment for interrupted tests at a maximum cyclic stress of 600
in a coarse Z-phase precipitate associated with Al-rich inclusions MPa: (a) at 10% (6000 cycles) of expected fatigue life; (b) at 50%
(SEM/BEI). (30,000 cycles) of expected fatigue life (SEM/BEI).
1134 E.J. Giordani et al. / International Journal of Fatigue 26 (2004) 1129–1136
hand, the average length of the larger cracks in the
neutral environment reached approximately 20 lm
(Fig. 9a) 35,000 cycles (20% of the expected fatigue life)
beyond the time required for initiation of the first vis-
ible cracks (at 30% expected fatigue life). Hence, the
aggressive environment evidently exerts a strong influ-
ence on the initiation of fatigue cracking and on the
early stage of crack growth.
The purpose of the SEM analyses of the fracture sur-
face was to define the fatigue and corrosion–fatigue
crack initiation mechanism by identifying the main
crack initiation sites that led to the fracture of the spe-
cimens. These analyses demonstrated the participation
of Z-phase precipitates in the initiation of the main
cracks, confirming the relevance of the coarse pre-
cipitates and clusters of precipitates, usually associated
with Al-rich inclusions, in the fatigue crack initiation
process (Fig. 11a). The fractographic analysis also
highlighted the participation of plate-like Z-phase pre-
cipitates as preferential sites for fatigue crack initiation,
particularly in the aggressive environment (Fig. 11b).
Most investigators agree that fatigue cracking
usually begins in or close to regions with particular
characteristics, on or just under the surface of the
metals. These characteristics may be inclusions, pre-
cipitates, brittle grain boundaries, severe scratches, pits
or slip bands [12]. Fatigue crack initiation in particles
Fig. 11. Sites of corrosion–fatigue crack initiation: (a) in coarse Z-
phase precipitates associated with Al-rich inclusions, at a maximum
cyclic stress of 650 MPa (SEM/BEI); (b) in coarse plate-like Z-phase
precipitates, at a maximum cyclic stress of 550 MPa (SEM/SEI).
on the material’s surface may occur through the separ-
ation of the matrix/particle interface, separation of
internal boundaries in complex particles, or even
through fracturing of the particle itself [13]. The latter
usually occurs when the concentration of stress around
the particle exceeds its own strength but not the cohes-
ive strength in the matrix/particle interface [14]. In the
present work, the main and secondary fatigue cracks in
both air and the aggressive environment were associa-
ted with the fracture of Z-phase precipitates, which
undoubtedly favored precocious fatigue and especially
corrosion–fatigue crack initiation. According to Örnha-
gen et al. [7], Z-phase is an inherent phase in this type
of austenitic stainless steel. Fracturing of precipitates
already in the first cycle of loading, where plastic
deformation occurs, introduces geometric dis-
continuities similar to microcracks in the austenitic
matrix (Fig. 8). These geometric discontinuities cause
stress and strain concentration, helping fatigue crack
initiation in these regions.
In the presence of an aggressive environment, apart
from the mechanical effect associated with the stress
concentration in the fracture region of the Z-phase pre-
cipitates, the effect of electrochemical corrosion exerts a
special influence. Already in the first cycle of loading,
plastic deformation causes the rupture of many pre-
cipitates, particularly the coarser ones. Due to the brit-
tle nature of Z-phase particles, the rupture of particles
probably occurs by cleavage and the geometric dis-
continuity associated with this rupture propagates
instantly throughout the particle and is interrupted
only when it reaches the ductile austenitic matrix on
the other side of the particle. In this way, the aggress-
ive environment penetrates into the discontinuity
immediately following rupture of the precipitates. The
aggressive environment therefore immediately comes
into contact with the bare metal (devoid of a passive
film), which acts as an anodic site in relation to the rest
of the passive surface, promoting a process of anodic
dissolution of the metal until it becomes repassivated.
An occluded cell is then created inside this disconti-
nuity. It is known, however, that anodic dissolution
occurs through the release of metallic Mn+ ions and
that an increase in the concentration of these cations in
the electrolyte inside the discontinuity favors the elec-
trostatic attraction of aggressive Cl anions, which
abound in the used electrolyte. It is also known that
the hydrolysis of Mn+ ions leads to a great release of
H+ ions [15], resulting in a considerable drop in the pH
inside the discontinuity. With cyclic loading, the stress
and strain concentrations inside the discontinuity can
lead to an intermittent breakdown of the passivity in
this location. As a result, there is a continuous increase
in the concentration of Cl- ions and an accentuated
drop of the pH of the electrolyte stagnated there. This
combination, allied to the shortage of oxygen in this
 E.J. Giordani et al. / International Journal of Fatigue 26 (2004) 1129–1136
region, consumed especially by the metal repassivation
reactions, creates a highly aggressive localized compo-
sition that lowers the stability of the passive film, con-
tributes to the acceleration of the anodic dissolution
and renders repassivation of the damaged region diffi-
cult, thus establishing an autocatalytic process by crev-
ice corrosion. Additionally, anodic dissolution can be
accelerated by the highly deformed condition of the
matrix due to the concentration of strain in the vicinity
of the discontinuity. The atoms in this region are in a
higher energy state, needing less activation energy to be
removed from the crystalline lattice than the less
damaged regions of the material. To complement this
extremely unfavorable condition, anodic dissolution
inside the geometric discontinuity can unblock the slip
interrupted by the accumulation or piling up of dis-
locations present in this region [12,16], favoring sub-
sequent slipping and rendering the process
autocatalytic. According to Parkins [17], electrochemi-
cal factors associated with geometric discontinuities
may be as important as or even more significant than
the factors relating to stress concentration, particularly
at the initiation and in the early stage of fatigue crack
propagation.
The condition of anodic dissolution is more effective,
the more aggressive the environment inside the dis-
continuity. Considering the principle that leads to the
phenomenon of crevice corrosion, the geometric dis-
continuity (crevice) that keeps the electrolyte more
stagnated in its interior contributes to the development
of a more aggressive electrolyte. Hence, it is logical to
assume that the discontinuities generated from the frac-
ture of precipitates in fine plate-like form, such as the
one illustrated in Fig. 11b, are more effective as they
keep the electrolyte stagnated and, consequently, main-
tain the aggressiveness in its interior. In these cases, the
electrochemical factor of the localized corrosion is an
important fatigue crack initiation factor. This may
explain the higher incidence of secondary cracks asso-
ciated with fine and elongated precipitates (probably in
plate-like form) in specimens cyclically loaded with a
lower stress in the aggressive environment when com-
pared to the specimens tested in air at the same stress
levels.
The results obtained from the study of the fatigue
crack initiation in ISO 5832-9 stainless steel, in air and
in the aggressive environment, led to the supposition
that the rupture of Z-phase precipitates, exhaustively
verified in the present work, when the material is plasti-
cally deformed—even with a very small plastic strain—
may limit the use of cold work processes in the manu-
facture of orthopedic implants for applications involv-
ing severe and heavy long-term cyclic loading inside the
human body, e.g. lower extremity prostheses. However,
provided the integrity of the Z-phase precipitate parti-
cles is maintained, the combination of high strength
1135
and high corrosion resistance of ISO 5832-9 steel [18],
attributed mainly to nitrogen in solid solution [15,19–
25], suggests that this steel is very promising for high
performance orthopedic applications. The integrity of
these particles could be kept through hot deformation
of the steel. The results also suggest that refining and
controlling the morphology of the Z-phase precipitates
would improve the fatigue and corrosion–fatigue
properties of this steel. A possible alternative to aid
this refinement would be to reduce the amount of Al-
rich inclusions, which apparently serve as a substrate
for the coarse Z-phase precipitation. However, control-
ling the size and morphology of Z-phase precipitates,
associated or not with nonmetallic inclusions, would
certainly involve a more complex study of the steps of
the melting and remelting processes, as well as of the
thermomechanical treatments to obtain the material.
4. Conclusions
The study of fatigue crack initiation mechanisms
conducted with the help of a SEM contributed to the
elaboration of fatigue and corrosion–fatigue crack
initiation mechanisms, based on the development of
stress and strain concentrations associated with geo-
metric discontinuities, which were generated by the
fracture of coarse particles characterized as Z-phase
precipitates, associated or not with Al-rich nonmetallic
inclusions. In the presence of an aggressive environ-
ment, the electrochemical effects of corrosion take on a
special importance due to the establishment of very
aggressive conditions of the stagnated electrolyte inside
these geometric discontinuities. This creates favorable
conditions for the crevice corrosion process, thereby
contributing considerably to reduce the fatigue crack
initiation stage and to accelerate the early stage of fati-
gue crack propagation.
Acknowledgements
This research was partially performed at LME/
LNLS—National Synchrotron Light Laboratory, Bra-
zil. The authors are also indebted to Baumer S/A for
supplying the stainless steel for this study, and to
CNPq for its financial support of this work.
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