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Fatigue Strength and Failure Mechanisms of Nitrided


Small Parts of a 30CrMoV9 Steel
a a a
Ivo Černý , Dagmar Mikulová & Ivan Fürbacher
a
SVÚM a.s., Strength Department , areál VÚ Běchovice , Prague, Praha, Czech Republic
Published online: 03 Mar 2011.

To cite this article: Ivo Černý , Dagmar Mikulová & Ivan Fürbacher (2011) Fatigue Strength and Failure Mechanisms of Nitrided
Small Parts of a 30CrMoV9 Steel, Materials and Manufacturing Processes, 26:1, 1-6, DOI: 10.1080/10426910903388499

To link to this article: http://dx.doi.org/10.1080/10426910903388499

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Materials and Manufacturing Processes, 26: 1–6, 2011
Copyright © Taylor & Francis Group, LLC
ISSN: 1042-6914 print/1532-2475 online
DOI: 10.1080/10426910903388499

Fatigue Strength and Failure Mechanisms of Nitrided


Small Parts of a 30CrMoV9 Steel
Ivo Černý, Dagmar Mikulová, and Ivan Fürbacher

SVÚM a.s., Strength Department, areál VÚ Běchovice, Prague, Praha, Czech Republic

An investigation of nitriding effect on fatigue behavior of small-size specimens of a 30CrMoV9 (ČSN 15330) nitriding steel heat treated to
high strength was carried out, and fatigue damage mechanisms were evaluated. Circular cross-section specimens either smooth or notched, with
the diameter approximately 2 mm in gauge section were used. Axial fatigue tests were carried out at constant load amplitude, loading was of
repeated type—load asymmetry R = 0. The program was carried out as a separate part of the complex evaluation of fatigue resistance of gears
against failure. The nitriding process resulted in unforeseen, mostly negative effects—in a strong reduction of fatigue life and fatigue limit in most
Downloaded by [Eindhoven Technical University] at 08:49 20 October 2014

cases. Fatigue limit only was slightly increased, namely, by 10% in case of smooth specimens. However, further small increase of load amplitude
resulted in strongly reduced fatigue strength in comparison with specimens without nitriding. Nitriding applied on notched specimens reduced their
fatigue limit by more than 40%. Fractographical and metallographical analyses showed an extensive brittle cracking of nitriding layer particularly
in the vicinity of fatigue crack initiation sites and an existence of multiple deep fatigue cracks besides the main crack. A likely reason of premature
failure was a superposition of external stress, which were close to yield strength, with tensile residual stresses under the nitrided layer, resulting
in a contribution of the small specimen size in a local subsurface plastic deformation and brittle cracking of the thin nitrided layer. Once brittle
cracks in the layer arose, fast fatigue crack growth occurred.

Keywords Crack initiation; Fatigue limit; Fatigue strength; Nitriding.

Introduction salt bath process [5] which confirms further physical


Nitriding is a well-known thermochemical surface reasons than only surface hardness and residual stresses.
treatment frequently used to improve mechanical surface Experiments with nitrided and denitrided steel investigating
properties of specific machinery parts exposed to combined the role of interstitial hydrogen showed a reduction of
contact fatigue, wear, and fatigue loading in operation. Gear fatigue strength after denitriding, which could not be only
wheels are probably one of the most typical examples. In explained by the loss of surface hardness [7]. Nitriding
operation, gear teeth are loaded by contact fatigue on the definitely results in a significant hardening of surface layer
side surface, whilst in their root, fatigue bending load is and microstructure changes which become a barrier against
dominant. Numerous cases where failure of gear wheels formation of surface intrusions and extrusions of persistent
were caused by fatigue damage as a dominant mechanism slip bands as a predominant mechanism of surface fatigue
and not by contact fatigue were shown [1]. Therefore, both crack initiation [9].
failure mechanisms have to be studied independently, if Due to the surface resistance of nitrided steels against
effects of nitriding of gears are to be determined. fatigue crack initiation, fatigue cracking is typically initiated
Two main physical reasons of an improvement of in subsurface layers, either at the boundary between nitrided
fatigue resistance by nitriding can be specified and layer and core material [3] or at subsurface inclusions
have been presented in the recent literature: (i) higher [10] or discontinuities [11]. Particularly in case of possible
microhardness and surface strength [2, 3] and (ii) higher subsurface initiation, early stages of fatigue damage can be
surface compression residual stresses. Unlike some works, interpreted and explained as a competition between short
where a close relationship between the two characteristics, crack growth in the surface layer in compression residual
namely microhardness and residual stresses is described stress field and subsurface crack growth in vacuum [12].
[4], other literature sources indicate that physical substance Another factor affecting fatigue strength is thickness of
of the fatigue damage process in nitrided steels is more nitrided layer. A dependence between fatigue strength and
complicated. A typical improvement of fatigue resistance case depth, but no effect of compound layer is described
of steels by nitriding in terms of fatigue limit is between in [10]. Similar results, i.e., effect of case depth on fatigue
50% and 100% [5–8]. Even if properties of case and core performance are described in several other sources [2, 4, 5].
materials are equivalent, fatigue strength can be affected The latter work is interesting among others by the fact that
by a different nitriding technology like ion or conventional, fatigue properties were studied on quite small specimens,
hour-glass shaped with just 4 mm in diameter, and maximum
improvement of fatigue strength corresponded to no more
Received October 6, 2009; Accepted November 25, 2009 than 50%, indicating possibilities that fatigue strength can
Address correspondence to Ivo Černý, SVÚM a.s., Strength be affected not only by the thickness of nitrided layer
Department, areál VÚ Běchovice, Podnikatelská 565, Prague, 19011 but also by volume of core material, if parts are of small
Praha 9, Czech Republic; E-mail: Ivo.Cerny@seznam.cz dimensions.
1
2 I. ČERNÝ ET AL.

Figure 1.—Preparation of contact fatigue test on rolling analogon.


Figure 2.—Homogenous core microstructure of tempered martensitic type.
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Besides special applications, e.g., in biomedicine [13],


nitriding is a very suitable method to increase total life of Fatigue specimens selected for the program had a
gears, where teeth are exposed to contact fatigue loading on circular cross-section and were small: 2.1 mm in diameter
sides and bending fatigue loading at roots. Fatigue strength in gauge length of smooth specimens, and 1.9 mm of
of nitrided gears obviously does not exceed properties of minimum nominal diameter of notched specimens, notch
surface hardened gears [14]. On the other hand, unlikely radius 0.5 mm. The notched specimen is shown in Fig. 3.
surface hardening, shape deformations connected with Theoretical stress concentration factor was 1.7. Parameters
nitriding are minimum. Moreover, parameters of nitriding of the notch were selected to simulate and model actual
can be exactly optimized [15, 16]. stress concentration factor occurring at roots of typical gear
When surface treatment effects on complex fatigue teeth. Thermochemical treatment was carried out by pulsed
properties of gears are studied, it is advantageous to evaluate ion nitriding method with the aim not to exceed the nitrided
the two damage mechanisms, namely, fatigue and contact depth 0.3 mm, due to the small specimen dimensions.
fatigue, separately. Separate methods of experimental Fatigue tests were performed on a simple fatigue machine
modeling not only simplify the work program, but also SCHENCK PHG with load asymmetry R = 0 and frequency
provide an information on the decisive failure mechanism 38–40 Hz. Detail of a smooth specimen attached in the
in the specific case. Whilst contact fatigue mechanisms are machine is in Fig. 4.
usually studied and experimentally modeled on a so-called The nitrided layer was analyzed both by metallographical
rolling analogon, Fig. 1, where two rollers are loaded in method and microhardness measurement. The actual
an oil environment with a specific Hertzian pressure and thickness of the layer was somewhat lower than desired.
slip [17], an effect of treatment on pure fatigue properties According to microhardness measurement, when maximum
values on the specimen surface and in the center were
in teeth roots can be modeled by fatigue tests of smooth or
HV 004 = 1118 and HV 004 = 400, respectively, the
notched specimens under cyclic tension or bending.
thickness evaluated from the 50% microhardenss reduction
This article contains results and discussion of an
corresponded to 0.1 mm, Fig. 5. The thickness of the layer
experimental evaluation of nitriding effects on pure fatigue
evaluated from microstructure was approximately 0.2 mm.
properties, i.e., the second part of the complex program, Microstructure of the nitrided layer was of a good quality,
whilst results of contact fatigue evaluation are described uniform, and homogenous, of the tempered martensite type
elsewhere. The work is fairly exceptional by the fact that with typically finely dispersed particles of nitrides, Fig. 6.
fatigue properties and failure mechanisms were evaluated White surface layer (-layer) was very thin, of the thickness
on small specimens, even with smaller diameter than in [5], less than 4 m or even negligible in several areas, which is
modeling small dimension parts. characteristic for pulsed ion nitriding. The white layer was
not removed from the specimen surface to model the real
Experiments
Experimental program was performed on a ČSN
15330 (30CrMoV9) steel, typical for manufacture of
gear wheels. Base material was heat treated to the
maximum strength Rm = 1163 ± 21 MPa and yield strength
Rp 02 = 1036 MPa, which are considerably high values.
Ductility was A = 16% and area reduction Z = 59%.
Microstructure of core material was of tempered martensite
type, homogenous, and of a good quality (Fig. 2). Just single
small inclusions of dimensions up to 8 m were present in
the microstructure. Figure 3.—Specimens with notch used for experimental program.
FATIGUE STRENGTH AND FAILURE MECHANISMS 3

Experimental results and discussion


Results of fatigue tests are summarized in Figs. 7–9.
Figure 7 shows an actual effect of stress concentration in the
notch on fatigue strength, which corresponds approximately
to the value 1.4. It is rather small in comparison with
the theoretical pure stress concentration factor. Such small
differences are, however, quite typical, because fatigue
strength in notches usually depends on further factors like
material notch sensitivity, etc.
The effect of nitriding on fatigue strength in the specific
case was unexpected and surprising. It was positive
just in case of smooth specimens in the high cycle
region over 200000 cycles, i.e., in the area of quite low
load amplitudes just exceeding fatigue limit of untreated
Figure 4.—Smooth specimen in grips of testing machine. specimens (Fig. 8). Fatigue limit of nitrided specimens was
higher by several percentage points. However, in case of
higher load amplitudes, fatigue life rapidly decreased in
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comparison with untreated specimens, by more than two


orders. In case of notched specimens, the nitriding effect
was unfavourable at all including fatigue limit, which was
reduced after nitriding by more than 40% (Fig. 9). The
results are in contradiction with typical positive results of
nitriding technology on fatigue strength, well known from
both the literature and practice.

Figure 5.—Microhardness in nitrided specimen as a dependence of depth


from surface.

Figure 7.—Actual notch effect on fatigue strength.

Figure 6.—Detail of homogenous microstructure of nitrided layer.

situation of gears, where white layer cannot be removed at


the teeth roots either. Microstructure analysis did not show
any imperfections either in the surface layer or in the core
material. Figure 8.—Effect of nitriding on fatigue properties of smooth specimens.
4 I. ČERNÝ ET AL.

Figure 9.—Effect of nitriding on fatigue properties of notched specimens.


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Fractographical analysis did not show any kind


of subsurface microcrack initiation. However, another
important feature of fracture surface was ascertained: Figure 11.—Distinct nitrided layer on fracture surface and circumferential
numerous brittle cracks in the nitrided layer near the main surface scratch-like formations.
fatigue crack. An example is shown in Fig. 10. Further
analyses helped explain the unusual unfavorable effect of
nitriding in the specific studied case. On the surface of actually represented a system of numerous very deep fatigue
some of the broken specimens (Fig. 11), distinct surface cracks in the late development stage, Fig. 12. This result
circumferential formations could be observed. When the indicated that fatigue cracking was abnormal. Unlike typical
fracture analysis was carried out, it was supposed that these formation of a single main fatigue crack and its growth
formations were surface scratches, imperfections arisen to final failure, in this case, numerous multiple fatigue
during specimen machining, and so their depth was no cracks arose with almost the same growing potential. In
more than several micrometers. On the other hand, there addition, fatigue growth of these cracks was very rapid.
was a distinct connection between these scratches and main As shown in Fig. 8, if nitrided specimens failed, their total
fatigue crack, like in Fig. 11. fatigue life was mostly shorter than 10000 cycles, namely,
To analyze actual depth of the scratches and reasons of at load amplitudes just several percent higher than fatigue
their connection with the main crack, a longitudinal cut was limit. These results demonstrated that fatigue crack initiation
made. It was surprisingly shown unlike the assumptions period, which is typically long in case of load amplitudes
that these scratch-like surface circumferential formations close to fatigue limit, was very short.
Further detailed analysis of the fatigue cracks on the
longitudinal cut showed a typically brittle transgranular
character in nitrided layer (Fig. 13), unlike mostly
intergranular fatigue growth in the core material (Fig. 14).
A considerable brittleness of the layer also was connected
with its distinct marginal relief on fracture surface, which
can be seen in Fig. 10 and particularly distinctly in Fig. 11.
The layer thickness evaluated from the fracture surface
corresponds to values 0.3–0.35 mm, more than the thickness
evaluated from microhardness or microstructure analysis.

Figure 10.—Numerous brittle cracks in nitrided layer in the vicinity of the Figure 12.—Multiple long fatigue cracks on longitudinal specimen cut after
main crack. fatigue failure.
FATIGUE STRENGTH AND FAILURE MECHANISMS 5

complex system of nitrided layer, subsurface core material,


and probably residual stresses are not strong enough to carry
the load amplitude, possible brittle microcracking of the
nitrided layer results in much more unfavorable conditions
in comparison with pure core material without the surface
treatment.
This hypothetical explanation is in consistency with some
results described in the literature. Paper [18] describes
several cases of rapid fatigue failure of nitrided crankshafts
of diesel engines which were ground after 300000 km of
service. After this general repair, some of them failed just
after less than 15000 lm of further service. It was found in
[18] that in critical sites of the failed crankshafts, thickness
of the nitrided layer was significantly reduced by grinding.
Fast cracking of the nitrided layer corresponded to a similar
damage mechanism like in the small specimens studied in
Figure 13.—Brittle transgranular character of crack in nitrided layer.
this work.
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Fast cracking of nitrided layer was also described in


[19], where not high, but low cycle fatigue behaviour
A hypothesis explaining premature fatigue failure of nitrided smooth specimens was investigated. In [19],
mechanisms can be formulated on the basis of the analyses different treatment time was used resulting in the layer of
carried out. Fatigue limit of smooth untreated specimens a sufficient thickness. However, increasing the treatment
800 MPa at the conditions used is very close to the yield duration was connected with a reduced fatigue behavior
strength 1036 MPa of the core material. The fatigue limit for high applied strains due to overstressing of the nitrided
800 MPa can be considered as unusually high and by layer. It was shown that only a single overload may be
nitriding even slightly increased. However, further increase sufficient to fracture the layer.
of load amplitude to values exceeding 900 MPa resulted A similar character of fatigue diagram like in Fig. 8
very likely in exceeding of yield stress in the subsurface was obtained in [20] investigating fatigue strength and
area under the nitrided layer, namely, due to a superposition fracture on plasma nitrided smooth and notched specimens
of external stress with subsurface tensile residual stresses, of a heat-treated AISI 15B21H steel. Notched specimens
which typically compensate compression residual stresses in had a similar stress concentration factor like in this work,
the nitrided layer [17]. Due to the stress superposition, yield Kt = 17. A different load and load asymmetry were used,
stress under the nitrided layer was locally exceeded. Such namely, reversed bending. The maximum positive stress
a subsurface plastic deformation, though local, resulted was not, therefore, so close to yield stress like in case of
in brittle cracking of the nitrided layer, which was not repeated loading with R = 0 used in this work. Fatigue limit
able to withstand the subsurface deformation because of was significantly increased by the nitriding. However, for
its low thickness and high brittleness; it was therefore, notched specimens, fatigue strength was increased just for
cracked by numerous brittle cracks. Once the extensive long fatigue lives. In [20], fracture toughness was evaluated
brittle cracking of the nitrided layer occurred, probably as a function of depth, and it rapidly decreased close to the
during several first load cycles, the microcracks or more surface. It can be supposed that a similar damage mechanism
exactly physically short cracks initiated fast fatigue cracking like in this work was responsible for the reduction of
at multiple sites. It can be concluded, therefore, that if the fatigue strength of notched specimens at higher loads: brittle
fracture of the nitrided layer followed by fast crack growth
to failure.
The explanation of failure mechanisms connected with
the fatigue strength reduction in this work is supported
also by results in [21] dealing with effects of hard
chromium plating on AISI 4140 steel. When just the
plating was used as the only surface treatment, fatigue
strength was significantly reduced, likely due to brittle
cracking of the layer and creating microcracks as initiating
sites of subsequent fatigue cracking. Plasma nitriding used
as a surface pretreatment before the plating significantly
improved fatigue strength in comparison with surface
untreated specimens due to supporting strengthening of the
layer and preventing against surface brittle microcracking.

Conclusions
An experimental programme of an investigation of
Figure 14.—Mostly intergranular fatigue crack in core material. nitriding effect on fatigue resistance of small size specimens
6 I. ČERNÝ ET AL.

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