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Structural surface characterization of ion nitrided AISI 4340 steel

Article  in  Materials and Design · April 2012

DOI: 10.1016/j.matdes.2011.12.025

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 Materials and Design 36 (2012) 741–747

Contents lists available at SciVerse ScienceDirect

Materials and Design

journal homepage: www.elsevier.com/locate/matdes

Structural surface characterization of ion nitrided AISI 4340 steel

Sule Yildiz Sirin a, Erdinc Kaluc b,⇑
a
Vocational School of Asim Kocabiyik, Kocaeli University, 41800 Hereke-Kocaeli, Turkey
b
Engineering Faculty, Mechanical Eng. Dept., Kocaeli University, 41380 Izmit-Kocaeli, Turkey

a r t i c l e i n f o a b s t r a c t

Article history: AISI 4340 steel was ion nitrided using different time and temperature and the gathered properties were
Received 2 June 2011 assessed by evaluating hardness profile, compound layer thickness, case depth and surface roughness by
Accepted 12 December 2011 using microhardness tester, optical microscopy, surface profilometer and X-ray diffraction. It has been
Available online 21 December 2011
found that the thickness of the compound layer increases with increasing treatment time and tempera-
ture. The surface roughness, the surface hardness, the hardness profile, the case depth, the compound
Keywords: layer thickness, and phase content of the compound layer depend on nitriding parameters such as treat-
C. Surface treatments
ment time and temperature. Optimum ion nitriding parameters of component should be determined
G. X-ray analysis
H. Selection for material properties
depending on the service conditions. For this reason, the effect of ion nitriding treatment parameters
on structural properties of AISI 4340 steel was investigated.
Ó 2011 Elsevier Ltd. All rights reserved.

1. Introduction more desirable than a mixture of these crystalline structures of

Ion nitriding, also referred to as plasma nitriding, is a process
of surface hardening using glow discharge technology to intro-
duce nascent (elemental) nitrogen to the surface of a metal part
for subsequent diffusion into the material. In vacuum, high-volt-
age electrical energy is used to form plasma, through which nitro-
gen ions are accelerated to impinge on the workpiece. Nitrogen
ions are combined with alloying elements such as chromium to
form a fine dispersion of alloy nitrides. This ion bombardment
heats the workpiece, cleans the surface, and provides active nitro-
gen [1]. Nitrogen diffusion modifies surface and near surface
microstructure producing hard layers with altered mechanical
properties. The layer on the ion nitrided steel consists of two
parts, compound layer and diffusion layer. The outer and thinner
layer consists of mainly c0 -Fe4N and/or e-Fe2,3N inter-metallic
phases. Therefore, it is commonly called as ‘compound layer’
[2]. On the other hand, it is also referred to as ‘white layer’ be-
cause of its white color after Nital etch on the microscopy. Thick-
ness and phase content of compound layer depend on the
treatment parameters such as specific gas composition, time
and temperature [1–3]. The carbon content of the steel has also
a significant influence on the formation of the compound layer
[4,5]. The growth rate of e-Fe2,3N is greater than c0 -Fe4N owing
to the wider homogeneity range of the e-Fe2,3N phase [4]. It is
important for some applications that the compound layer may
be comprised of c0 -Fe4N or e-Fe2,3N phases or a mixture of both.
The formation of a homogeneous mono-phase compound layer is
⇑ Corresponding author. Tel.: +90 262 303 34 05; fax: +90 262 335 34 43.
E-mail addresses: ekaluc@kocaeli.edu.tr, erdinckaluc@yahoo.com (E. Kaluc).
iron–nitrogen alloys because the different unit cell parameter of
the cited crystalline phases can generate stress at the grain
boundary, increasing the fragility of the layer. Also, the character-
istics of the crystalline phases present in the compound layer is
important for some applications such as the hard coating depos-
ited onto nitrided materials [6]. The layer, beneath the compound
layer, is known as ‘diffusion layer’ which consists of mainly inter-
stitial atoms in solid solution and fine coherent nitride precipi-
tates when the solubility limit is reached. Diffusion layer
thickness is also referred to as ‘case depth’. The hardness and
the depth of the diffusion layer depend on the amount of nitride
former elements in the steel [7,8], the initial microstructure of the
material [8,9], the time and the temperature of the ion nitriding
treatment [10] and the specific gas composition used in ion
nitriding system [5,8,9]. The case-core boundary is also influenced
by the concentration of the alloying elements present in the
steels [8].
The ion nitriding process is more economical than all the other
conventional nitriding processes such as gas nitriding and salt bath
nitriding because of faster nitrogen diffusion, lower nitriding tem-
perature, shorter treatment time and lower gas consumption. Eas-
ier control of compound and diffusion layer formation and also
suppressed compound layer formation are reported to be the other
advantages of ion nitriding [4,10]. Thanks to a number of advanta-
ges, the ion nitriding process, which is extensively used to improve
the surface properties, wear, fatigue, corrosion, friction properties,
and also load bearing capacity of dynamically loaded components,
is widely used in the manufacturing and machining industries pri-
marily in engine components, tools for hot/cold work, machine
tools, gears and forging dies.

0261-3069/$ - see front matter Ó 2011 Elsevier Ltd. All rights reserved.
doi:10.1016/j.matdes.2011.12.025
742 S.Y. Sirin, E. Kaluc / Materials and Design 36 (2012) 741–747

The properties of a nitrided steel component are determined by steel was ion nitrided in NH3 environment under different process
both the core strength and the structural characteristics of the conditions. The process variables investigated include time (2 h,
compound layer and the diffusion layer [11]. While the compound 4 h, 8 h and 16 h) and temperature (500 °C, 520 °C, 540 °C). The ef-
layer determines the corrosion resistance [12], the diffusion layer fect of ion nitriding process parameters on structural properties
determines the strength of the component, as well as its fatigue such as surface roughness, hardness profile, diffusion layer thick-
resistance [3,4,10,11,13,14]. Tribological characteristics of the ness, compound layer thickness and phase content of compound
component are determined by compound layer, diffusion layer layer were investigated by using a microhardness tester, optical
and surface hardness. microscopy, surface profilometer and X-ray diffraction (XRD).
The wear behavior of component is determined only in early
stage by compound layer, after that the diffusion layer becomes
2. Material and experimental studies
dominant [4,15]. The compound layer can have either a positive ef-
fect thanks to high hardness or a negative effect because of
The material used in this study was CrMoNi low alloy AISI 4340
brittleness and relatively earlier spalling of the surface on the wear
steel and the chemical composition of the steel was given in Table
resistance of the nitrided surface [16]. Retention of the compound
1. AISI 4340 steel was received in hot-rolled condition and
layer on the nitrided surface depends on the loading mode and on
austenitized at 840 °C for 30 min, quenched in oil and then tem-
the magnitude of the main loading parameters, the compound
pered at 600 °C for 1 h. The core hardness of AISI 4340 steel was
layer thickness and its brittleness, etc. [16]. The presence of com-
obtained 315 HV0.2. Disc specimens about 20 mm in diameter
pound layers on nitrided components can improve the resistance
and 15 mm thick were cut from the incoming bar of 22 mm diam-
to scuffing, seizure and galling under lubricated conditions. Since
eter, and ground with SiC paper from 240 down to 1200 grit to pro-
the outer porous part of the compound layer is able to absorb a
duce a fine surface finishing. The surface roughness was
quantity of oil, the compound layer leads a reduction in the friction
maintained below approximately 0.03 lm. After polished, the
coefficient [15]. Although compound layer is generally hard and
specimens were degreased in trichloroethylene and then placed
brittle, thin mono-phase c0 -Fe4N compound layer produced by
in an industrial DC glow discharge ion nitriding furnace. The ion
ion nitriding is extremely ductile and wear resistant according to
nitriding furnace employed in this study is similar to that de-
e-Fe2–3N phase; therefore, there is no need to remove it [17]. While scribed by Genel et al. [10]. The specimens were employed as the
the compound layer has a considerable effect on the amount of
cathode. The furnace was evacuated by the vacuum pump and then
wear loss in the initial part of the service, the wear rate is a func-
pure NH3 (ammonia) treatment gas was admitted into the furnace
tion of the surface hardness and case depth. Surface hardness is
through a gas distribution valve. The specimens were ion nitrided
more important than case depth in preventing wear loss; however,
for 2 h, 4 h, 8 h, 16 h at a temperature of 500 °C, 520 °C or 540 °C,
a certain thickness of diffusion layer is necessary to support the
voltage between 480 V and 540 V depending on the desired tem-
hard surface layer. Long treatment time produces lower surface
perature. Temperatures of specimens were measured by thermo-
hardness and deeper diffusion layer which are less effective in pre-
couples, which were embedded in the specimens. The treatment
venting wear [15].
time was accounted after treatment temperature was reached.
After ion nitriding, the corrosion resistance increases due to the
After ion nitriding, the specimens were cooled to the room temper-
formation of a compound layer consisting of highly dense c0 -Fe4N
ature in the vacuum chamber. The composition, surface roughness,
and e-Fe2–3N nitrides. The e-Fe2,3N nitride exhibits better corrosion
microstructure and hardening effect of the nitrided specimens
resistance when compared with c0 -Fe4N nitride due to its crystal-
were characterized by using metallographic examination, XRD,
line structure and higher nitrogen content [18]. However another
surface profilometer and microhardness tests.
research showed that c0 -Fe4N nitride is relatively more stable in
Surface profilometer was used to determine of the surface
corrosive medium than e-Fe2–3N nitride [19]. Thus, the corrosion
roughness before and after ion nitriding. Surface roughness was
resistance of the nitrided layer depends on the type of nitride
characterized by measuring the average roughness Ra, according
formed in the compound layer and the type of corrosive environ-
to the ISO 4287:1997 standard [24]. During the surface roughness
ment [18]. Although the compound layer provides the materials
measurements, the measurement length was chosen as 0.75 mm.
with good physical properties against wear and corrosion, in the
For each specimen, surface roughness was determined by ten mea-
case of a very hard and brittle layer in a construction subjected
surements and the average was plotted.
to stresses, a thinner compound layer or no compound layer is nec-
Optical microscopy was used to characterize the microstruc-
essary. When the material is subjected to stresses, cracking begins
tures. Cross sections from nitrided specimens were ground, polished
in the layer [2,3].
and etched using Nital 2% immersion reagent. The compound layer
The high cycle fatigue strength can be significantly improved by
thickness was measured, after etching, using an optical microscopy.
ion nitriding. While some investigations on ion nitrided steels have
X-ray diffraction (XRD) with Cu Ka radiation (k = 1, 5405 Å) was
revealed that fatigue limit increases with increasing diffusion layer
used to determine the phases present in the modified layer.
thickness [3,4,10,14], the others have revealed that fatigue limit in-
Microhardness measurements were used to determine diffusion
creases with the strength and residual stress distribution in the
layer thickness as well as to aid in characterizing the physical
cross-section of specimens [13]. The compound layer has no dom-
properties of the diffusion layer as a function of depth [8]. The sur-
inant effect on the fatigue behavior of ion nitrided specimens [3].
face hardness and the microhardness profile of ion-nitrided speci-
The surfaces become rougher due to the nitrogen ion
mens were evaluated using a microhardness tester with a load of
bombardment and the formation of a nitride layer [20,21]. The de-
200 g, according to the ASTM E384-99 standard [25]. The hardness
gree of the increase in the surface roughness varies with the ion
at 20 lm depth was chosen for comparison of surface hardness, so
nitriding parameters such as gas compositions, time, temperature
that any possible effects from a compound layer would be negligi-
and applied voltage [20,22,23].
There have been many investigations aiming the prediction of
the resulting structures of ion nitrided components and their ser- Table 1
vice behavior. However, the studies on the effects of ion nitriding Chemical composition of AISI 4340 low alloy steel.
on AISI 4340 steel and the phenomena involved in the structural C Si Mn P S Cr Mo Ni Fe
evolution of compound layer and diffusion layer, their thickness
0.38 0.26 0.69 0.016 0.004 0.80 0.22 0.69 Bal.
and surface topography are very scarce. In this study, AISI 4340
 S.Y. Sirin, E. Kaluc / Materials and Design 36 (2012) 741–747 743

ble. The hardness profile of each specimen was determined by 0,30

three measurements at the cross section and the average was AISI 4340
plotted. The case depth was defined as the depth at which the
0,25
hardness was 10% HV above the core hardness [22].

Surface Roughness (µm)

3. Results and discussion 0,20

The specimens are substantially rougher, as would be expected 0,15

from the formation of a nitride layer due to the nitrogen ion bom-
bardment [20,21]. The degree of the increase in the surface rough-
ness varies with the ion nitriding conditions [22,23,26,27]. The 0,10
surface roughness apparently increases with the square root of 2h
the treatment time [27] and increasing the treatment temperature
0,05 16 h
due to the severe sputtering of the substrate by nitrogen ions as
well as from the higher applied voltage required for the treatment unnitrided
[23]. The results of the surface roughness measurements are given 0,00
in Table 2. After the ion nitriding process, the surface roughness in- 500 540
creased up to 0.26 lm while it was 0.03 lm initially. Also, the test Ion Nitriding Temperature ( oC)
results show that higher surface roughness values can be obtained
Fig. 1. The effect of ion nitriding conditions on surface roughness.
with increasing ion nitriding time and/or temperature. For in-
stance, surface roughness value is increased from 0.12 lm to
0.26 lm as a result of increasing ion nitriding time, from 2 h to
16 h at 540 °C. It can be said that ion nitriding time and tempera-
ture are effective at surface roughness generation. The effect of ion
nitriding temperature on surface roughness increases with increas-
ing treatment time (Fig. 1). At low treatment temperatures, the
surface roughness is mainly due to the surface relief caused by vol-
umetric expansion associated with the formation of nitrides. More-
over, sputtering and redeposition of the sputtered material on the
surface may have played some minor role in the surface roughen-
ing. Surface roughness at higher temperatures is mainly due to
similar expansion effects as well as preferential sputtering com-
bined with the redeposition of iron nitrides on the surface. More
importantly, increasing the treatment temperature brings about
an increase in the applied voltage which in turn increases the ki-
netic energy of the incident ions. The sputtering yield which is
dependent upon the kinetic energy of the colliding ions increases
with increasing temperature, leading to an increase in the surface
roughness [23]. Corengia et al. also reported that, during ion nitrid-
ing the sputtering rate is much higher around the edges than at the
central region of the samples. They observed columnar microfor-
mations that, instead of being perpendicular to the substrate as
in the center of the sample, are leaning out of the center. This var-
iation in the growth direction can be explained as a result of the
change in the electric field direction close to the edge of the sample
[27].
The ion nitriding treatment time, temperature and gas compo-
sition as well as the amount of C in the steel influence the kinetics
of the formation of the compound layer [1–6,27,28]. The develop- Fig. 2. Optical microstructures of ion nitrided AISI 4340 steel (400) at 500 °C, 16 h
ment of the compound layer only approximates to a parabolic (a) and 540 °C, 16 h (b).
dependence on time for the first few hours of nitriding, until a lim-
iting thickness is reached, beyond which no further growth is
obtained [4]. In the case of ion nitriding, the growth rate of the compound layer thickness was from 4.8 lm to 8.8 lm at 540 °C
compound layer deviates from a parabolic diffusion law [11]. The (Table 3). It can be seen in Fig. 4 that the growth rate of compound
presence of a continuous and uniform compound layer could be layer is changed by temperature. In addition, some workers [27,28]
observed in Fig. 2. The compound layer thickness increases with have shown that the thickness of the compound layers increases
increasing time and temperature, Fig. 3. When the treatment time with time, at all temperatures, to a certain maximum value and
was increased from 2 h to 16 h, the compound layer thickness in- then to decrease. This behavior can be explained in terms of the
creased from 2.6 lm to 4.8 lm at 500 °C. This increase in sputtering, the denitriding and the role of the layer as a barrier

Table 2
Surface roughness of unnitrided and ion nitrided AISI 4340 at different conditions.

Treatment conditions Unnitrided 500 °C/2 h 500 °C/16 h 540 °C/2 h 540 °C/16 h
Average surface roughness, Ra (lm) 0.03 0.11 0.16 0.12 0.26
744 S.Y. Sirin, E. Kaluc / Materials and Design 36 (2012) 741–747

10 8
AISI 4340 AISI 4340
9
Compound Layer Thickness ( m)
7

Compound Layer Thickness ( m)

8
6
7

6 5

5 4
4
3
3
2
2

1 500 ºC 1
540 ºC t = 4h
0
2 4 8 16 0
500 520 540
Ion Nitriding Time (h)
Ion Nitriding Temperature ( oC)
Fig. 3. The relationship between compound layer thickness and treatment time at
Fig. 4. The relationship between compound layer thickness and treatment
500 °C and 540 °C.
temperature for 4 h.

for the formation of free Fe atoms [2,4,22,27,28]. Not only the

phase: c0 -Fe4N and the thickness of compound layer increases with
thickness of compound layer but also the phase content of com-
increasing treatment time. The evolution of (e + c0 ) to c0 could be a
pound layer is influenced by the treatment parameters such as spe-
consequence of the sputtering and/or generated by a phase trans-
cific gas composition [1,7], time [2,4,10,18,26–28] and temperature
formation e-Fe2–3N ? c0 -Fe4N [27,28]. It is observed that, c0 -Fe4N
[4,12,19–21,23,26]. The unnitrided specimen shows only a-Fe
phase is present in all compound layers at all ion nitriding temper-
phase, whereas the ion nitrided specimen exhibits additional
atures and time. It is well known that better characteristics in duc-
phases, e-Fe2–3N and/or c0 -Fe4N, due to different nitrides [12,26].
tility and fatigue are found when the compound layer consists of
According to these patterns, it was obvious that the intensity of
only one nitride phase, i.e. either c0 -Fe4N or e-Fe2–3N. When the
the a-Fe phase progressively decreases and the intensity of the ni-
(c0 + e) dual phase is present, internal stresses develop as a conse-
tride phases progressively increase with increasing ion nitriding
quence of the difference in lattice structures [27]. The specimens
temperature and time [12]. Fig. 5 shows typical X-ray diffraction
ion nitrided at 540 °C are expected to present a better performance
spectra from ion nitrided specimens at 500 °C for 2 h (Fig. 5a), at
as they show a high homogeneity and consist of only one phase, c0 -
500 °C for 16 h (Fig. 5b), at 540 °C for 2 h (Fig. 5c) and at 540 °C
Fe4N. The variation in the structure and the thickness of the com-
for 16 h (Fig. 5d). Fig. 5a and b shows that the intensity of the e-
pound layer may be related to the decarburization, denitriding and
Fe2–3N phase gradually decreases with increasing nitriding time,
sputtering that take place during ion nitriding [28–30].
while the intensity of the c0 -Fe4N phase increases with increasing
Beneath the compound layer, in the diffusion zone, nitrogen is
nitriding time at 500 °C. Thus, the proportion of c0 -Fe4N to e-Fe2–
dissolved in ferrite at nitriding temperature and forms nitride pre-
3N-nitride phases increased with increasing nitriding time at
cipitates during cooling as a result of decreasing solubility of nitro-
500 °C. This increase is primarily ascribed to the increase of c0 -
gen [11]. The hardness decreases from surface to core, since the
Fe4N nitride. The higher amount of e-Fe2–3N in the beginning of
concentration of metal nitrides decreases towards core [3]. The
the process and gradual decrease in the amount of e-Fe2–3N in
hardness profiles of the ion nitrided specimens are given in Fig. 6.
the compound layer could be ascribed to the decrease in carbon
The surface hardness measurements of the samples treated at dif-
content of the steel due to sputtering [28]. Edenhofer [29] has also
ferent temperatures and times are given Table 2. The surface hard-
reported that, during ion nitriding, sputtering removes carbon to-
ness of AISI 4340 steel is increased up to two times by the ion
gether with other elements from the workpiece surface and carbon
nitriding process. The surface hardness of ion nitrided specimens
content degreases towards the surface of the samples during ion
is in the range of 510–634 HV0.2, while the core hardness remains
nitriding in carbon free plasma. The analysis shows that two ni-
unchanged, 315 HV0.2. The surface hardness increases to reach a
trides, e-Fe2–3N and c0 -Fe4N, are present at 500 °C, while the e-
maximum value at 8 h for both temperatures, 500 °C and 540 °C,
Fe2–3N phase cannot be detected at 540 °C. When treatment tem-
and then lower values are obtained in longer treatment period,
perature is 540 °C, the specimens have a compound layer of one

Table 3
Structural characteristics of ion nitrided AISI 4340 steel.

Treatment details Surface hardness (HV0.2) Comp. layer (lm) Case depth, t (lm)
Austenitized 840 °C, 30 m/ 315 – –
oil quenched–tempered at 600 °C for 1 h (QT)
QT and 2 h, 500 °C ion nitrided 510 2.6 280
QT and 4 h, 500 °C ion nitrided 526 3.0 300
QT and 8 h, 500 °C ion nitrided 634 4.0 360
QT and 16 h, 500 °C ion nitrided 609 4.8 470
QT and 4 h, 520 °C ion nitrided 537 3.9 395
QT and 2 h, 540 °C ion nitrided 553 4.8 315
QT and 4 h, 540 °C ion nitrided 580 5.4 420
QT and 8 h, 540 °C ion nitrided 610 6.9 450
QT and 16 h, 540 °C ion nitrided 549 8.8 510
 S.Y. Sirin, E. Kaluc / Materials and Design 36 (2012) 741–747 745

Fig. 5. X-ray diffraction patterns of ion nitrided AISI 4340 steel for (a) 500 °C, 2 h; (b) 500 °C, 16 h; (c) 540 °C, 2 h; (d) 540 °C, 16 h.

700 700
2h
2h
4h
4h
600 600 8h
8h
16h
16h
Hardness (HV0.2)

500 500

400 400

300 300
T = 500 oC T = 540 oC

200 200
0 20 50 100 150 200 250 300 400 500 600 700 0 20 50 100 150 200 250 300 400 500 600 700
Distance from Surface ( m)

Fig. 6. Microhardness profiles of AISI 4340 steel, ion nitrided at different conditions.

16 h. The reduced surface hardness is obtained at longer nitriding
time because of the formation of large nitride precipitates
[8,13,14,23,26,27]. Precipitates with a certain size will be the most
effective in obstructing the movement of dislocations and in pro-
ducing the maximum strengthening and hardening [13,23,26,27].
At longer times, the precipitates particles are larger in size and
more prone to coarsening, leading to a lower precipitate density
and hence lower hardness [23,26,27]. This reduction of surface
hardness is more effective at high temperature (Fig. 7). To sum
up, an optimum nitriding time at which the highest hardness may
be achieved exists [14,23,26,27].
The case depth increases with increasing time and temperature
as expected for diffusion-controlled growth [3,4,10,14,22,23,
26,27]. The higher depth values of the case depth are obtained as
the treatment time increases. It can be seen in Fig. 8 that the case
depth has increased with the treatment time of ion nitriding at
both temperatures as indicated in some earlier studies
[4,14,22,23,26,27] and the generation of diffusion layer is much
746 S.Y. Sirin, E. Kaluc / Materials and Design 36 (2012) 741–747

700 diffusion layer is very thin. Increasing treatment temperature re-

AISI 4340 sults in an increase in the nitrogen diffusivity, leading to the forma-
tion of thicker layers [23]. The effect of treatment temperature on
Surface Hardness (HV0,2)

hardening behavior is displayed in Fig. 9. It shows that the case

depth increases as the temperature increases for the fixed treat-
600
ment time of 4 h because of the increased nitrogen diffusivity. It
can be seen that the case depth which is governed by the extend
of nitrogen atoms penetration into the sample, increases for
increasing temperature due to the increased nitrogen diffusion
500 coefficient [23]. While the case depth and surface hardness in-
crease strongly with increasing time and temperature, the surface
hardness decreases at longer nitriding time because of the forma-
500 ºC
tion of larger nitride precipitates, which are less effective in
540 ºC increasing hardness than smaller ones. The maximum hardness
400
2 4 8 16 and the maximum case depth do not occur together.
Ion Nitriding Time (h)
4. Conclusions
Fig. 7. Effect of ion nitriding temperature and time on surface hardness.

The basic aim of this study is to understand the effects of ion

550 nitriding process parameters such as treatment time and tempera-
AISI 4340 ture on the structural characteristic of quenched and tempered
500 AISI 4340 low alloy steel. Based on the results obtained, the follow-
ing conclusions can be derived.
450 The surface roughness is increased by ion nitriding and the de-
Case Depth ( m)

gree of the increase depends on the ion nitriding conditions. It

400 might be said that ion nitriding time and temperature are effective
in surface roughness generation and the effect of ion nitriding tem-
350 perature on surface roughness increases with increasing treatment
time.
300 The compound layer thickness and the diffusion layer thickness
500 ºC increase with increasing time and temperature. The increase in ion
250 nitriding time and temperature produce not only an increase of the
540 ºC
compound layer thickness and the diffusion layer thickness but
200 also a more uniform compound layer/diffusion layer interface.
2 4 8 16 The structure of the compound layer formed during the ion nitrid-
Ion Nitriding Time (h) ing of AISI 4340 steel is consisted of c0 -Fe4N and e-Fe2–3N phases
and the ratio of c0 /e increases with increasing the treatment time
Fig. 8. The relationship between case depth and ion nitriding time at 500 °C and
540 °C. at low temperature, 500 °C. The compound layer structure formed
during the ion nitriding of AISI 4340 steel shows an evolution from
a dual phase {e-Fe2–3N + c0 -Fe4N} to a mono-phase c0 -Fe4N with
450 increasing treatment temperature. While c0 -Fe4N phase is being
AISI 4340 formed at all temperatures and time, e-Fe2,3N is not formed at high
temperature. The specimens ion nitrided at high temperature are
expected to present a better performance as they show a high
400 homogeneity and consist of only one phase, c0 -Fe4N.
The surface hardness of ion nitrided specimen increases with
Case Depth ( m)

increasing time and temperature, but the reduced surface hardness

is observed at longer nitriding time because of the formation of lar-
350
ger nitride precipitates which are less effective in increasing hard-
ness than smaller ones. It can be said that the surface hardness
depends on the nitriding time when the temperature is constant.
The surface hardness increases in the first 8 h when it reaches a
300
maximum value at both temperature, 500 °C and 540 °C, and then
decreases at 16 h because of the formation of coarser nitride pre-
t=4h cipitates. This reduction of surface hardness is more effective at
250 540 °C than 500 °C. While the maximum surface hardness is ob-
500 520 540 tained at 500 °C at 8 h, the maximum diffusion layer thickness
Ion Nitriding Temperature (oC) forms at 540 °C at 16 h.

Fig. 9. The relationship between case depth and ion nitriding temperature for 4 h.
References

faster at 540 °C than 500 °C. In addition, some workers [10,27]
have found that there is a linear relationship between the case
depth and the square root of the nitriding time. Since the diffusion
coefficient of nitrogen atoms at low treatment temperature is low,
[1] O’Brien JM, Goodman D. Heat treating, plasma (ion) nitriding. In: Davis JR et al.,
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