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Effect of ion nitriding on fatigue behaviour of AISI 4140 steel

Article  in  Materials Science and Engineering A · February 2000

DOI: 10.1016/S0921-5093(99)00689-9

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 Materials Science and Engineering A279 (2000) 207 – 216
www.elsevier.com/locate/msea

Effect of ion nitriding on fatigue behaviour of AISI 4140 steel

Kenan Genel a, Mehmet Demirkol b,*, Mehmet Çapa b
a
Mechanical Engineering Department, Sakarya Uni6ersity, Adapazari 54040, Turkey
b
Faculty of Mechanical Engineering, Istanbul Technical Uni6ersity, Gümüssuyu, Istanbul 80191, Turkey

Received 30 March 1999; received in revised form 26 August 1999

Abstract

Ion nitriding has become a popular thermo-chemical surface treatment, which is being used to develop fatigue and wear
characteristics of steels. Besides the increased strength, the formation of high compressive residual stresses in the case region
causes remarkable improvement in fatigue properties of steels. In this study, the effect of case depth on fatigue performance of
AISI 4140 low alloy steel has been investigated by conducting a series of rotary bending fatigue tests at the frequency of 95 Hz,
on hour glass shaped, 4 mm diameter specimens, which had been ion nitrided at 748 K for 1, 3, 8 and 16 h. Up to 50%
improvement in fatigue strength of the steel has been attained by ion nitriding, depending on the case depth formed during the
process. The comparison of test results between ion and liquid nitrided specimens having the same case and core properties, has
shown that a 12% increase in fatigue strength could be reached by ion nitriding with respect to conventional, salt bath nitriding
process. An attempt was made to establish some empirical relationships between the parameters defining relative case depth, which
consider case depth and specimen size together, and fatigue strength of ion nitrided steel. It was obtained that the subsurface ‘fish
eye’ type crack formation is the dominant fatigue crack initiation mechanism in ion nitrided AISI 4140 steel, and a map has been
constructed to illustrate the locations of crack origins depending upon the case depth and the cyclic stress acting on specimens.
It was also tried to explain the conditions promoting the ‘fish eye’ crack formation by analysing the combined effects of residual
and applied stress patterns as well as inclusion size. © 2000 Elsevier Science S.A. All rights reserved.

Keywords: Ion nitriding; Fatigue strength; Low alloy steel; Relative case depth; Fish eye crack

1. Introduction with high compressive residual stresses on the surface of

steel components such as gears, crankshafts, dies and
The machine components working under cyclic loads tools [2,6]. Plasma or ion nitriding process is being
are severely subjected to the threat of fatigue failure [1]. preferred recently in most surface hardening applica-
It is well known that some thermo-chemical and/or tions of machine parts, to the conventional techniques
mechanical surface treatments improve the fatigue per- such as gas or liquid nitriding, since the process have
formance of machine parts. These processes cause in- the characteristics of faster nitrogen penetration, sim-
crease in surface hardness and strength of material plicity in application, cleanliness and economical as-
resulting the creation of high compressive residual pects, as well as easier control of compound and
stresses on or near the surface of machine parts, as well diffusion layer formation. The requirement of lower
as low tensile residual stresses in the core. The residual process temperatures, shorter process periods and sup-
stresses affect the net distribution of stresses under pressed compound layer formation are said to be the
cyclic loading, resulting consequently a decrease in the other advantages of ion nitriding [6,8,10].
tensile stress, which is effective on the surface [2–7]. The prior investigations on ion nitrided steels have
Nitriding is one of the most widely used thermo-chemi- revealed that fatigue limit increases with increasing case
cal methods, which produces strong and shallow case depth of nitrided layers, emphasising the effectiveness
of case depth or case area in the cross-section of
* Corresponding author. Tel.: +90-212-293-1300, ext. 2582; fax:
specimens by the use of dimensionless parameters defin-
+90-212-245-0795. ing relative case depth [11–13]. Some models predicting
E-mail address: [email protected] (M. Demirkol) the fatigue strength of nitrided steels have been pro-

0921-5093/00/$ - see front matter © 2000 Elsevier Science S.A. All rights reserved.
PII: S 0 9 2 1 - 5 0 9 3 ( 9 9 ) 0 0 6 8 9 - 9
208 K. Genel et al. / Materials Science and Engineering A279 (2000) 207–216

posed by regarding the strength and residual stress stress patterns as well as the results of fracture surface
distribution in the cross-section of specimens examinations of fatigue test specimens.
[4,5,12,13]. It has been determined that the increase in
fatigue strength by ion nitriding was roughly 25%
higher than conventional gas nitriding [14]. It has also 2. Experimental work
been determined that the subsurface fatigue crack for-
mation is dominant failure initiation mechanism in A standard medium carbon, CrMo low alloy AISI
conventional [4,15], and ion nitrided steels excluding 4140 steel has been used in the study and the chemical
low cycle fatigue regime [11 – 13,16 – 19]. Considering composition of the steel was given in Table 1. The 22 mm
diameter steel bar was received in hot rolled condition
the geometry of test specimens, it has also been re-
and austenitized at 1123 K, for 1 h, quenched in oil, and
ported that the increase in fatigue performance of
then tempered to a hardness of 320 Vickers Hardness
notched specimens is higher than of the smooth speci-
scale (VHN) with ASTM austenite grain size number 9.
men [17].
The hourglass shaped, rotating bending fatigue test
In this study, a series of fatigue tests on ion nitrided specimens were machined to the dimensions given in Fig.
AISI 4140 steel with different case depths were con- 1, and the stress concentration factor Kt was determined
ducted and some efforts were made to construct empir- as 1.02 [20]. The surface of the reduced section was
ical relationships between relative case depth and mechanically polished by using alumina slurry to an
fatigue limit of ion nitrided steel. A comparison of average roughness in the range of 0.01–0.05 mm, then
fatigue performance was also made between ion and ultrasonically cleaned in alcohol and degreased in
liquid nitrided specimens having the same hardness thrichloroethylene.
profiles in their cross-sections. Finally, a special atten- The schematic representation of ion nitriding
tion was given to the crack initiation behaviour of equipment is given in Fig. 2. A 200-mm diameter quartz
nitrided specimens by analysing applied and residual glass tube was used as the vacuum vessel and AISI 304
stainless steel sheet was employed as the anode, while the
Table 1 fatigue specimens were cathode. Temperatures of
The chemical composition of AISI 4140 steel used in the study specimens were measured by thermocouples, which were
embedded in the specimens. A single stage rotary vane
C% Si% Mn% P% S% Cr% Mo% Fe% pump maintained vacuum pressure of 1300 Pa, with the
0.41 0.21 0.83 0.025 0.027 0.91 0.18 Bal.
capacity of 8 l min − 1. The gas mixture of 30% N2 and
70% H2, and the temperature of 748 K were used in ion
nitriding for 1, 3, 8 and 16 h. The process time was
accounted after the completion of a glow discharge of 0.5
h duration with pure H2, which allows the specimens to
reach process temperature. A group of specimens were
liquid nitrided in a KCN salt bath at 848 K for 2 h, in
order to compare the fatigue properties with ion nitrided
specimens. The specimens were quenched in water after
nitriding. In order to investigate the effect of white layer
on fatigue properties, particularly crack initiation
characteristics of the steel, a number of specimens were
Fig. 1. Fatigue test specimen, dimensions in mm. polished further until the complete removal of white layer
was maintained. This procedure was applied to
specimens ion nitrided at 748 K for 16 h and to specimens
salt bath nitrided at 848 K for 2 h.
The hardness profile of the nitrided case was
determined by using Karl Frank microhardness tester
with 0.98 N load in terms of VHN, and the effective case
depth was defined as the distance below the surface,
where the hardness was equal to 400 VHN.
Rotating fatigue tests were performed on a cantilever
bending test machine, at a frequency of 95 Hz (5700 rpm)
in laboratory air atmosphere and carried out until
complete fracture of specimens occurred. There was no
observation of heating effect on specimens during fatigue
Fig. 2. Schematic representation of ion nitriding equipment. testing and pure rotating bending conditions were
 K. Genel et al. / Materials Science and Engineering A279 (2000) 207–216 209

ing residual stresses on the surface of the specimens

were calculated respectively [21]. Compressive residual
stress measurements were realised for all nitriding treat-
ments and an error estimate can be given in the range
of 5–2% depending on the case depth of specimens
from the thinnest to the thickest case depth in the study
respectively.
The fracture surface of specimens were examined
under optical and scanning electron microscopes in
order to evaluate the crack initiation and growth char-
acteristics of the materials in the core and nitrided case
regions of specimens. The phases, which are present on
the surface of nitrided specimens, were identified by
X-ray diffraction equipment using Cu Ka radiation.

3. Results and discussion

The hardness profiles of nitrided cases are given in

Fig. 3. Hardness profiles of AISI 4140 steel, ion nitrided at 748 K for Fig. 3. The surface hardness of specimens is in the
1, 3, 8 and 16 h. range of 660–710 VHN, while the core hardness re-
mains unchanged. The effective case depth of nitrided
specimens based on 400 VHN is given in Table 2,
together with the details of applied heat treatment.
When the graphical representation given in Fig. 4 is
examined, it is possible to say that the effective case
depth is increased with the process time of ion nitriding,
and it can also be concluded that the effective case
depth is described by a power function for all process
times up to 16 h such as;
t (mm) =126{ion nitriding time [h]}0.365 (1)
If the kinetics of case progress for the process periods
between 1 and 16 h is considered, it can also be
recognised that the effective case depth changes linearly
with the square root of time as indicated in some earlier
Fig. 4. Progress of case depth with the process time for ion nitrided
AISI 4140 steel at 748 K.
studies [9–11].
One of the objectives of this study is to compare the
fatigue properties of ion nitrided and conventional liq-
maintained properly. The fatigue limit of specimens was
uid nitrided AISI 4140 steel, having the same hardness
used to define and evaluate the fatigue strength of steel
profile. After several attempts of liquid nitriding prac-
in all conditions.
tices, it was determined that the process at 848 K in
Mechanical residual stress measurements were re-
KCN bath, for 2 h was the most suitable one to
alised by measuring the strain changes at one surface of produce the same case properties with ion nitriding at
4×20×50 mm plate type specimens, after removing 748 K, for 3 h. The similarity of the hardness data of
the whole nitrided surface layer from the other side by these two different nitriding treatments can be seen in
delicate, stepwise grinding not to cause any additional Fig. 5. Although a temperature of 100 K higher than
stress. First of all, the specimens were nitrided in the the temperature of ion nitriding was used in liquid
same manner with the fatigue test specimens and then nitriding, the time required by the processes were close
thin foil strain gages were bonded properly onto one to each other. The combination of high kinetic energy
large surface of these specimens. Considering the elastic of ions with the thermal activation results deeper pene-
strain relaxation after the removal of nitrided layer tration in ion nitriding. The effect of surface cleaning of
from one surface determines the residual stress on the steels by glow discharge of H2 is another important
opposite surface, the maximum values of released feature of plasma treatment [9,22]. As a result of both
strains were measured after the complete removal of effects, it was concluded that the activation energy of
nitrided layer by a Whetstone Bridge and correspond- ion nitriding was lower than conventional techniques,
 210
Table 2

K. Genel et al. / Materials Science and Engineering A279 (2000) 207–216

Heat treating details, structural and fatigue properties of AISI 4140 steel

Heat treatment Case deptha Relative case (D/D−2t) Relative case Surface residual Core residual Fatigue strengthe Improvement in fatigue
(t, mm) depthb (t/D) areac (AR) stress (srs, MPa) stressd (src, MPa) (sf, MPa) strengthf (%)

Austenitized at 1123 K per oil – – – – – – 630 –

quenched/tempered at 873 K, for
1h
Quenched and tempered/ion nitrided 0.120 0.030 1.063 0.131 −210 15 773 23
at 748 K, for 1 h
Quenched and tempered/ion nitrided 0.210 0.053 1.117 0.248 −330 43 816 30
at 748 K, for 3 h
Quenched and tempered/ion nitrided 0.260 0.065 1.150 0.321 −370 64 865 37
at 748 K, for 8 h
Quenched and tempered/ion nitrided 0.350 0.088 1.212 0.469 −300 80 954 51
at 748 K, for 16 h
Quenched and tempered/liquid ni- 0.205 0.051 1.114 0.241 −355 45 730 16
trided in KCN bath at 848 K, for
2h

a
For 400 VHN.
b
Specimen diameter is D= 4 mm.
c
AR = case area/core area.
d
Predicted by force balance in the cross-section.
e
Fatigue limit.
f
With respect to the quenched and tempered condition.
 K. Genel et al. / Materials Science and Engineering A279 (2000) 207–216 211

allowing higher penetration rates [23]. The thickness of

compound layer was observed as 6 mm for the longest
process time in ion nitrided specimens, while this layer
was 22 mm in liquid nitrided specimens. The X-ray
diffraction patterns measured at the surface of the
specimens are given in Fig. 6, for 1 and 16 h of ion
nitriding process times and two different phases of iron
and chromium nitrides were detected.

Fig. 7. Fatigue curves of heat treated, liquid and ion nitrided AISI
4140 steel for various process times.

The S–N curves obtained from rotating bending

fatigue tests are given in Fig. 7 for all nitrided and
quenched and tempered steels. Distinct fatigue limit
characteristics were observed for all types of materials
considered in the study, and an absolute progress in
fatigue limit with increasing case depth was observed.
The fatigue strength of steel is strongly affected by the
thickness of nitrided case. Increase in case depth causes
Fig. 5. Hardness profiles of AISI 4140 steel, ion nitrided at 748 K for higher fatigue resistance, and an improvement of 51%
3 h and liquid nitrided at 848 K for 2 h. in fatigue strength was developed for 16 h ion nitrided
specimens, which have the heaviest nitrided case in the
study, when the fatigue performance of quenched and
tempered steel is assumed to be the reference. A statisti-
cal evaluation of fatigue test data is given in Table 3, in
which the extreme values of endurance limit satisfying
95% confidence limit are given together with the aver-
age values for all conditions of heat treatments.
Since the section size is one of the most important
factors determining the fatigue performance of machine
components, some dimensionless parameters were
defined to express the proportion of nitrided case zone
in the whole cross-section such as, relative case area AR,
which is defined as the ratio of case area to core area
and the ratio of specimen diameter to core diameter
D/(D − 2t) for round specimens [12,13]. The ratio of
case depth to specimen diameter t/D can also be pro-
posed for simplicity to overcome this difficulty. The
change in fatigue performance and the improvement in
fatigue strength, as functions of dimensionless parame-
ters D/(D − 2t) and relative case depth t/D, are given in
Fig. 8, referring to the fatigue performance in quenched
and tempered condition of steel. Increased values of
both parameters tend to enhance the fatigue lives and
increase endurance limits accordingly with a noticeable
parallelism. Empirical relationships between fatigue
Fig. 6. X-ray diffraction patterns from the surfaces of specimens ion strength and the dimensionless parameters of relative
nitrided for (a) 1 h; (b) 16 h. case depth t/D, relative case area AR and D/(D −2t)
212 K. Genel et al. / Materials Science and Engineering A279 (2000) 207–216

Table 3
Statistical analysis of fatigue test results

Heat treatment Correlation coefficient R 2 95% confidence limit for 107 cycles (MPa) Mean fatigue strength (MPa)

Quenched and tem- 0.90 601–659 630

pered
Ion nitrided, 1 h 0.91 753–793 773
Ion nitrided, 3 h 0.98 785–846 816
Ion nitrided, 8 h 0.95 845–884 865
Ion nitrided, 16 h 0.96 927–980 954
Liquid nitrided, 2 h 0.96 713–747 730

have been developed by using least square regression The surface compressive residual stress is increased with
analysis. Table 4 presents the results of the analysis for increasing effective case depth in a decreasing rate, and
different mathematical models and it can be accepted the maximum compressive residual stress is obtained
that the relative case depth t/D has enough accuracy in for specimens ion nitrided for 8 h. Prolonged nitriding
predicting the fatigue strength of ion nitrided AISI 4140 time has a tendency to decrease compressive residual
steel. Improvement in fatigue strength of liquid nitrided stresses on or near the surface of specimens, and this
specimens has reached 16%, based on the fatigue per- phenomenon can be explained by the formation of
formance of quenched and tempered steel, while the thicker case and further precipitation in the nitrided
gain was 30% in ion nitrided specimens having the same layer causing relaxation of the stresses in the case [25].
case properties as the liquid nitrided specimens. If the The core counteracts to the expansion of nitrided case
fatigue test results of ion and liquid nitrided specimens and results tensile residual stress in the core. If a linear
are compared with each other, it can be concluded that change of residual stresses through the cross-section is
the fatigue strength increment in ion nitrided specimens assumed, the corresponding tensile stress in the core
is twice as the liquid nitrided specimens having the can simply be calculated by taking the force balance in
same hardness distribution in their cross-sections. In the cross-section of specimens into account. Although,
other words, an improvement of 12% was obtained by the magnitude of tensile residual stresses is much
ion nitriding with respect to liquid nitriding. An experi- smaller than compressive surface residual stresses, the
mental work on medium carbon Cr – Ni – Mo steel has tensile residual stress in the core is increased with
shown that, a relative improvement of 25% was at- increasing case depth. The calculated values of tensile
tained by ion nitriding referring to the results of gas residual stresses in the core are given in Table 2,
nitriding [14]. The difference may be tied up to the
process characteristics of liquid nitriding, in which
quenching is used as a post treatment after nitriding,
lack of information about the relative case depth in
nitrided specimens of cited reference and small differ-
ences in chemical compositions of test materials. The
effect of quenching can be explained by the role of
nitrogen atoms, which are entrapped in iron crystal
lattice producing supersaturated solid solution after
rapid cooling. The growth of metastable nitrides of iron
is also supported by diffusion of interstitial nitrogen
atoms in slow cooling, which naturally reduces the
distortion of the lattice and promotes the formation
and growth of nitrides [3,24]. Since the reduced popula-
tion of interstitial nitrogen atoms have an adverse effect
on fatigue characteristics of steel, fast cooling is pre-
ferred at the end of liquid nitriding process where
applicable [3].
Residual stress distribution has a major effect on
fatigue properties of case hardened steels. Particularly
high compressive residual stresses, which are formed on
the surface of nitrided steels, enhance the fatigue life
accordingly. The results of residual stress measurements Fig. 8. The effect of relative case depth t/D and the parameter
are given in Table 2, and Fig. 9 in graphical manner. D/(D− 2t) on the fatigue strength of ion nitrided AISI 4140 steel.
 K. Genel et al. / Materials Science and Engineering A279 (2000) 207–216 213

Table 4
Empirical relationships to determine fatigue strength for ion nitrided AISI 4140 steel as functions of relative case depth t/D, relative case area AR
and parameter D/(D−2t)

Mathematical sf = f(t/D) (MPa) Coefficient of sf =f(D/D−2t) (MPa) Coefficient of sf =f(AR) Coefficient of

model correlation R 2 correlation R 2 (MPa) correlation R 2

Linear 641+3526 (t/D) 0.98 1484 (D/D−2t)−835 0.98 654+659AR 0.97

Power 633+2507 (t/D)0.86 0.99 654 (D/D−2t)2 0.97 632+538 (AR)0.71 0.99
Exponential 646 exp{4.52(t/D)} 0.97 99 exp{1.89(D/D−2t)} 0.96 658 exp{0.84(AR)} 0.95

depending to the process time in nitriding and resultant nism is changed to mixed type of transgranular and/or
case depth respectively. intergranular cleavage fracture in case region.
In cyclic loading of machine components, the effec- The fatigue life of specimens is strongly affected by
tive stress acting on the specimen is the main con- the stress distribution in their cross-sections. The super-
trolling parameter and it depends strongly on the posed, net stress distributions in the cross-sections of
applied and residual stresses, which are extremely im-
portant for cyclic stressing in bending and/or torsion.
Using the principle of superposition of stresses, the
combination of residual and applied stresses produces a
net, effective stress distribution, which has generally a
maximum value in the case/core transition zone of
smooth specimen [12]. Since the initiation of fatigue
failure occurs primarily in the regions under the influ-
ence of highest cyclic stress, subsurface fatigue crack
formation called ‘fish eye’ is dominated in nitrided
steels with the contribution of inclusions [4,12,13,16,18].
Similar results have also been obtained in this study
and one of typical location of fish-eye crack is given
schematically in Fig. 10, with the hardness profile in the
cross-section of the specimen. It can easily be recog-
nised that the cracks are originated at inclusions in the
core and at positions near the case/core interface. The
fish eye cracks are in circular shape, which is a direct
consequence of pure rotating bending type of cyclic Fig. 9. The change in compressive residual stress on the surfaces of
stressing. On the other hand, the fatigue cracks were specimens with nitriding time and case depth respectively.
developed at inclusions on the surface of specimens in
quenched and tempered martensitic structure.
Scanning electron micrography (SEM) fractograph of
a typical subsurface fish eye crack formation is given in
Fig. 11(a). The specimen was ion nitrided for 8 h and
loaded under 900 MPa cyclic stress up to complete
fracture at the failure cycle of 3.8 × 106. The mi-
croprobe analysis of SEM indicated that the main
constituents in the inclusions, which are acting as the
sources of crack origin in the centre of fish eye crack,
are Al and Ca, and it is also possible to conclude that
they are primarily the particles of calcium aluminate as
seen in Fig. 11(b). The decohesion of inclusion with the
matrix is another important feature of non-metallic
inclusions, which is most probably a result of different
thermal expansion properties of oxides and steel. A Fig. 10. The location of fish-eye crack and hardness profile on the
typical transgranular ductile fracture characteristic is fracture surface of the specimen ion nitrided for 1 h, under the cyclic
dominated in core region of specimens, but the mecha- stress of 794 Mpa, resulting 4.5 ×106 cycles of fatigue failure.
214 K. Genel et al. / Materials Science and Engineering A279 (2000) 207–216

to play an important role in determination of crack

initiation point in this high stress zone. On the other
hand, the location of the peak value of superposed
stress is away from the case/core interface to the centre,
for the specimens with heavy case depth as seen in Fig.
12(b). The slope of the net stress distribution in the
nitrided case is much less than the slope in the core,
and it can be said that the case is under the influence of
high stresses. As a result of this type of net stress
distribution it can be expected that the crack origins
should be condensed in core neighbouring to case/core
interface. In other words, it is possible to say that,
crack initiation should take place in the core near to
case/core interface, considering the difference in the
strength of case and core.
The location of fatigue crack origins on the fractured
surfaces of test specimens is shown on a map given in
Fig. 13. It can easily be recognised that, besides the

Fig. 11. (a) SEM micrograph of fracture surface of the specimen ion
nitrided for 8 h, exposed to 900 MPa cyclic stress, resulting 3.9 ×106
cycles of fatigue life. (b) SEM image of a non-metallic inclusion at the
nucleation site in core region.

specimens, which had been ion nitrided for 1 and 16 h,

are given in Fig. 12(a) and (b), respectively. Although
two different applied stress levels were selected in the
analysis, the shape of superposed stress distributions
were similar to each other and the difference in stress
distribution is mainly originated from different case
depths of specimens, as well as their residual stress
patterns. It is clearly seen that for the specimen with
shallow case in Fig. 12(a), the peak value of superposed
net stress is very near to case/core interface. The slope
of net stress distribution between surface and case/core
interface is steeper than the slope between case/core
interface and the centre of the specimen. The net stress
in the core, which is equal to the net stress acting on the
surface of specimen, can be reached at distances ap-
proximately three times of the case thickness below the
core/case interface. Therefore, the location of crack
Fig. 12. Superposed stress distribution under the influence of high
origin may be shifted to interior of the specimen far and low cyclic stresses, in ion nitrided specimens for (a) 1 h and (b)
from the case/core interface, and the inclusion size start 16 h.
 K. Genel et al. / Materials Science and Engineering A279 (2000) 207–216 215

origin/case depth ratio are dictated by larger size inclu-

sions and it can roughly be concluded that the inclusion
size, which causes fish eye fatigue crack nucleation with
origin/case depth ratio higher than 1.6, has values
greater than 20 mm. If the results of specimens ion
nitrided for 8 h are considered, it can be said that
critical inclusion size increases from 25 to 32 mm when
the origin/case depth ratio increases from 1.4 to 1.9
respectively, although the applied cyclic stress does not
change. In ion nitriding processes with longer process
time, the case depth would be thicker and the fish eye
crack origin was closer to the case than the thin cased
specimens. As an example, crack origins took place in a
Fig. 13. Fatigue crack origin distribution as function of applied stress band, which have values of crack origin/case depth
and case depth of ion nitrided AISI 4140 steel specimens.
ratio between 1 and 2, for moderate ion nitriding
process times, such as 3 and 8 h. In other words, cracks
inclusion size, the level of applied stress and the thick-
were initiated in core within a band starting at case/
ness of nitrided case of specimens are very effective on
core interface and with a maximum width of the case
determination of crack origins. First of all, there was
depth. When the applied cyclic stress was too high, the
no crack origin lying in case zone, and all cracks had
crack was initiated on the surface of specimen instead
been initiated in the core far away from the case/core
interface depending on case depth of specimen and of core and no fish eye crack formation could be
applied alternating stress. The crack origin/case depth observed. Due to the freedom of deformation on speci-
ratio lies between 1.5 and 3.5 for the specimens with men surface and the presence of very high stresses
shallow case as a result of shorter periods of ion acting on the surface, the crack origins preferentially
nitriding, under the strong influence of inclusion size. take place at the defects on the surfaces of specimens
Presence of heavy inclusions interior of specimens in- under the presence of low cycle fatigue conditions.
creases the probability of crack initiation far off the It was noticed that the fish eye crack formations
case, inheriting higher values of crack origin/case depth occurred very close to the case/core interface for the
ratio. specimens with the heaviest case depth produced in the
A detailed SEM investigation has been carried out on study. Crack origins took place in the core at a maxi-
the determination of mean inclusion size at the centre mum distance of one half of the case thickness, from
of fish eye crack sites of some fractured fatigue speci- the interface of case and core. The crack formation was
mens. Table 5 covers the data, which is constituted by again controlled by stress and surface conditions of
case depth, surface/crack origin distance, crack origin specimens under the application of high stresses.
case depth ratio, applied alternating stress and average White or compound layer formation depends on the
inclusion size at the centre of fish eye crack of some technology used in nitriding and different layer thick-
fatigue test specimens. The data punctuates the impor- ness may be obtained. It is believed that the easy crack
tance of inclusion size in fish eye crack nucleation, formation and propagation characteristics of white
particularly in low alternating stress applications with layer has a tendency to increase the probability of easy
shallow case depth specimens. High values of crack fatigue crack initiation and it was proposed that the

Table 5
The distance of fish eye crack origin to surface, crack origin/case depth ratio, applied cyclic stress and average inclusion size at the center of crack
of some fatigue specimens

Heat treatment Case depth Surface to crack origin distance Crack origin/case Alternating stress Average inclusion size
(t, mm) (mm) depth ratio (MPa) (mm)

Ion nitrided, 1 h 120 420 3.5 880 27

198 1.7 834 22
Ion nitrided, 3 h 210 267 1.3 893 12
336 1.6 955 16
Ion nitrided, 8 h 260 494 1.9 893 32
370 1.4 900 25
Ion nitrided, 16 h 350 495 1.4 1074 24
360 1.0 1040 19
 216 K. Genel et al. / Materials Science and Engineering A279 (2000) 207–216

complete removal of white layer has prime importance (6) Fish eye crack initiation is one of the main
to obtain best fatigue performance in nitrided steels [2]. characteristics of fractured ion nitrided specimens, par-
On the other hand, it has been emphasised that, there ticularly in high cycle fatigue regime. Depending on the
was no effect of white layer on fatigue properties of level of applied cyclic stress, cleanliness of steel, case
steels for smooth specimens, since the subsurface crack depth and compressive residual stress pattern of ion
formation dominates in nitrided steels under high cycle nitrided specimens, the subsurface crack initiation may
fatigue regime [12]. In this study, some fatigue work has take place in the core region with some multiples of case
also been carried out on the specimens without having depth, from case/core transition interface interior to the
any compound layer on their surfaces, in order to specimen.
investigate the effect of white layer on fatigue behaviour
of nitrided steels. Results of the study have shown that,
the presence of white layer did not have any significant
Acknowledgements
effect on fatigue life and crack origin characteristics of
specimens.
The authors are grateful for the help received from Dr
T. Gülmez regarding ion nitriding practices, Professor
Dr O. Addemir for the provision of SEM facilities,
4. Conclusions ASIL Çelik A.Ş. and Demireller A.Ş. for supply and
preparation of test specimens.
The following conclusions can be derived from the
results of this study:
(1) The progress of case depth in ion nitriding can be References
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