Saipta Metallurgicaet Materialia,Vol. 32, No. 4, pp.

535-540,1995
Copyright 0 1994 Elsevier Science Ltd
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EFFECT OF NITROGEN IMPLANTATION ON FATIGUE CRACK

INITIATION IN FERRITIC Fe-24Cr-4Al ALLOY
S.C. Tjong and S.M. Zhu
Department of Physics and Materials Science
City Polytechnic of Hong Kong, Tat Chee Avenue,
Kowloon, Hong Kong
(Received June 2,1994)
(Revised September 19,1994)

In recent years there has been much interest in modification of the surface properties of materials by ion
beams. Ion beams can be used to create a highly non-equilibrium surface alloy layer without any change in the
bulk properties. In the process, the energetic ions penetrate the solids, displace the host atoms from their positions
and they eventually come to rest with an approximate Gaussian distribution about a mean projected range. Ion
implantation has been used to improve the fatigue, corrosion and wear properties of materials.
Fatigue failure in metals occurs by crack initiation and propagation. In general, the cyclic strain localization
in the persistent slip bands (PSBs) is the main cause of fatigue failure in f.c.c. metals since the PSBs act as
preferential sites for fatigue crack initiation. The emergence of PSBs at the free surface during low cycle fatigue
(LCF) leads to the formation of intrusions and extrusions. It has been reported that the hardened surface layers
produced by ion implantation can inhibit the emergence of PSBs at the free surface, thereby increasing crack
initiation resistance of the f.c.c. metals and alloys, e.g. Ni, Al, Cu, Ni-20Cr and austenitic stainless steel (2-6).
In contrast, fewer studies have been made on the LCF behavior of ion implanted b.c.c. alloys. Previous studies
have shown that the labyrinth structures and ladders which are typical substructures of PSBs developed in fatigued
f.c.c. metals also tend to form in ferritic Fe-Cr-Al and Fe-Cr alloys (7-9). Thus ion implantation can be expected
to retard the emergence of bulk PSBs to the free surface of ferritic Fe-Cr-Al alloys. This paper aims to investigate
the effect of nitrogen implantation on the fatigue behavior of ferritic Fe-24Cr-4Al alloy.

Exnerimental
Ferritic Fe-24Cr-4Al alloy used in this investigation has a composition of 24.16 wt. % Cr, 3.88 wt. % Al,
0.009 wt. % C and the balance iron. The alloy was melted in a vacuum induction furnace and then hot forged into
plates of 25 mm thickness. Fatigue specimens were machined from these plates. They were then solution treated
at 1323 K for 2h and subsequently quenched into oil. The average grain size of the specimens is -600 pm. Each
specimen was wet ground with silicon carbide paper and 1 pm diamond paste to get a mirror surface.
Nitrogen implantation were carried out with an energy of 65 keV and a dose of 2~10~ ions/cm2 (-2x10*
atoms/cm3 peak concentration). The specimens were rotated to ensure uniformity of implantation. The distribution
of implanted ions was calculated using the TRIM computer simulation program developed by Biersack and
Haggmark (10). The specimens were not masked during implantation. The TRIM calculations are for normal ions
incidence.
Fatigue tests were conducted at room temperature under total strain control mode with a total strain rate
of 3.2~10~~ and a total strain amplitude of 3~10~ in a closed-loop servohydraulic testing machine. A 10.0 mm
gauge length clip-on extensometer was used to measure and control total strain amplitude. All tests were conducted
twice in order to confirm the reproducibility. Optical microscopy and scanning electron microscopy (SEM) were

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used to observe the crack initiation process and the characteristics of slip. The Vickers hardness (HV) was measured
with a digital microhardness tester under a 10 gf load.

Results and Discussion

Figure 1 shows the computer simulated ion range distribution of 65 keV nitrogen ions in the Fe-24Cr-4Al
alloy. The mean projected range is 76 ML The ion distribution is slightly skewed for light ion (N+) implantation
due to the surface backscattering and sputtering. Figure 2 shows the cyclic stress response versus number of cycles
for both implanted and unimplanted specimens under a constant total strain amplitude of 3~10-~. It can be seen that
both specimens exhibit initial cyclic softening followed by subsequent slight hardening. However, the nitrogen
implanted specimen exhibits a slightly higher stress amplitude than that of the unimplanted during cycling. Thus
an implanted layer with a depth of - 152 nm leads to a substantial change in bulk mechanical behavior of the Fe24Cr-4Al alloy.
Figures 3(a)-3(c) are optical micrographs showing surface deformation of the un-implanted alloy cycling
at a total strain amplitude of 3~10~ for various cycles. It can be seen that a high density of slip bands is formed
in the specimen after cycling for 500 cycles. Furthermore, fine microcracks are observed in this specimen after
500 cycles only. As the number of cycles is increased to 5000 cycles, the cracks can be seen initiated primarily
at grain boudaries (Fig.f(b)). It has been reported by Mughrabi that intergranular cracks can initiate where PSBs
impinge on the grain boundary (11). Kim and Laird also indicated that the interactions of grain boundaries with
the surface are the most favorable sites for fatigue crack nucleation (12). The crack nucleation was preceded by
the formation of a small step at a sensitive grain boundary in very early stages of the fatigue life and this small
step continued to grow with increasing number of cycles until a microcrack developed in f.c.c. copper (12). They
further pointed out that grain boundaries which are preferred for crack initiation are also preferred for stage I
propagation. Stage I growth gives way to stage II growth when the increasing stress intensity of the growing crack
is sufficient to initiate slip on new systems (13). In the present work, the crack initiation and propagation process
in b.c.c. Fe-24Cr-4Al alloy is analogous to that in f.c.c. copper. Fatigue failure in Fe-24Cr-4Al alloy occurs by
propagation of a microcrack initiated at the grain boundary into major transgranular cracks (Fig. 3(c)). Figure 4
shows the SEM micrograph of the un-implanted specimen surface at failure. It is apparent that multiple-trackings
are observed in the slip bands of the Fe-24Cr-4Al alloy cycled to failure. The microcrack initially nucleated at the
grain boundary advances by linking together with the microcracks developed in the slip bands. In this case,
intergranular and transgranular propagation is evident for the un-implanted Fe-24Cr-4Al alloy.
Figures 5(a)-5(c) are optical micrographs showing surface deformationof the nitrogen-implanted Fe-24Cr-4Al
alloy during fatigue. The primary features to note in these micrographs are that surface slip lines seem to be more
homogeneous than those of the un-implanted specimen. The density of slip bands in the implanted alloy is
substantially lower than that of the un-implanted alloy. Moreover, the implanted alloy shows a delay in the
impingement of PSBs at the surface. This leads to a slight increase in fatigue life for nitrogen implanted alloy (Fig.2).
As the PSBs generated in the bulk alloy impinge on the implanted layer, they induce deformation and cracking of
the implanted layer, leading to the formation of surface cracks. These cracks have a brittle appearance as evidenced
by SEM observation (Fig.5). The implanted specimen has a hardness value of HV 175, whereas the hardness of
the un-implanted alloy is HV 140. It should be noted that nitrogen implantation can result in the formation of nitrides
in the surface layer of Fe-24Cr-4Al alloy. Nitride formation in nitrogen implanted 304 stainless steels has been
observed by Fayeulle et al. (14,15). The nitrides are expected to restrict dislocation motion through precipitate
pinning. This can results in higher cyclic flow stress , homogeneous slip band formation and eventually delay the
initiation and growth of cracks. Further work on transmission electron microscopy is needed to elucidate this
problem.

Conclusions
Nitrogen implantation

in a ferritic Fe-24Cr-4Al

alloy results in cyclic hardening behavior and a slight

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537

improvement in fatigue life. Optical and SEM observations reveal that the slip bands are more homogeneous in
the implanted alloy than those of the un-implanted specimen. Furthermore, the density of slip bands is significantly
lower at the surface of implanted alloy. For the un-implanted alloy, impingement of PSBs at the free surface leads
to the initiation of intergranular cracks. However, the emergence of PSBs at the free surface is retarded in the
implanted alloy due to the interaction between PSBs and nitrides of the implanted layer. The surface cracks exhibit
a brittle appearance for the ion beam modified specimen.

Acknowledgements
This research was supported by UPGC Competitive Earmarked Grant (Grant No. 904054, CPHK 227/92E).
Ion implantation was performed at State Key Laboratory for Materials Modification by Laser, Ion and Electron
Beams at Dalian University of Technology, China. Appreciations are also expressed to Mr. C.S. Ren and Mr. K.H.
Fu for technical assistances. S.M. Zhu is on leave from Dalian University of Technology, China.

References
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11. H. Mughrabi, Proc. 2nd. Int. Symp. on Defects, Fracture and Fatigue, Eds. G.C. Shih and J.W. Provan,
1983, p.139
12. W.H. Kim and C. Laird, Acta Metall. 26, 777(1978).
13. W.H. Kim and C. Laird, Acta Metall. 26, 789(1978).
14. S. Fayeulle, D. Treheux and C. Emouf, Appl. Surf. Sci. 25, 288(1986).
15. S. Fayeulle and D. Treheux, Nucl. Instr. Meth. B19/20, 216(1987).

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Vol. 32, No. 4

6000

1000
,_I._

Th WET

DEPTH

Fig. 1 Computer simulated range distribution of nitrogen ions in

Fe-24Cr-4Al alloy with an accelerating voltage of 65 keV.

--c

Ion-implanted
Un-implanted

100

101

102

103

104

alloy
alloy

105

CYCLES
Fig.2

Cyclic stress responses versus number of cycles for nitrogen implanted and
un-implanted Fe-24Cr4AI alloy cycled at a total strain amplitude of 3~10~.

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No. 4

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FATIGUECRACKINITL4TION

Fig.3

Optical micrographs showing surface

deformation and crack development
features in un-implanted Fe-24Cr-4Al
alloy cycled at a total strain amplitude
of 3x10. for (a) 500 cycles, (b) 5OOQ
cycles and (c) after cycling to failure.

Fig.4

SEM micrograph of the surface of unimplanted Fe-24Cr-4Al alloy cycled

at a total strain amplitude of 3x10
up to failure.

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Vol. 35 No. 4

Fig.5

Optical micrographs showing surface

deformation and crack development
features in implanted
Fe-24Cr-4Al
alloy cycled at a total strain amplitude
of 3~10~ for (a) 500 cycles, @) 8000
.
_ .

Fig.6

SEM micrograph of the surface of

implanted Fe-24Cr-4Al alloy cycled
at a total strain amplitude of 3x1W3
up to failure.