Materials Science and Engineering A315 (2001) 28 – 34

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Wear resistance of pulse plasma nitrided AISI 4140 and

A355 steels
B. Podgornik *, J. Vižintin
Centre for Tribology and Technical Diagnostics, Uni6ersity of Ljubljana, Bogišiče6a 8, SI-1000 Ljubljana, Slo6enia

Received 8 August 2000; received in revised form 6 February 2001

Abstract

In this study, the wear resistance of pulse plasma nitrided AISI 4140 and A355 steels was evaluated under dry and lubricated
sliding conditions and compared with conventional plasma nitrided samples. After surface characterisation using metallographic,
microhardness and surface examination techniques, sliding wear tests were performed on a pin-on-disc machine in which hardened
ball bearing steel discs were used as the counterface. The influence of surface treatment, steel composition, and testing conditions
on the wear resistance of the surface treated pins was determined. The test results showed that the wear resistance of the
investigated steels could be improved by means of plasma and pulse plasma nitriding. However, compared with conventional
plasma nitriding, pulse plasma nitriding lead to very similar wear properties of the nitrided steel surface. Also, the steel
composition has an important effect on the properties and wear resistance of the plasma nitrided steel surface. Addition of Al,
an alloying element with a high affinity to nitrogen, increased the hardness and residual stresses, and improved the wear resistance
of the nitrided steel surface. © 2001 Elsevier Science B.V. All rights reserved.

Keywords: Wear resistance; AISI 4140 and A355 steels; Plasma and pulse plasma nitriding

1. Introduction usually below 570°C. The minor probability of sur-

Surfaces of engineering components are often ni-
trided to improve their corrosion, fatigue, and wear
properties prior to use in different types of applica-
tions [1]. During nitriding, nitrogen diffuses into the
steel surface, where it combines with alloying ele-
ments such as chromium and aluminium to form a
fine dispersion of alloy nitrides. These precipitates
strengthen the surface region and introduce beneficial
compressive stresses at the surface [2]. Therefore, the
response of steel to the nitriding treatment depends
principally on its composition and the process tem-
perature [3].
A significant advantage of nitriding is that it causes
less distortion than hardening and carburising, be-
cause of the relatively low processing temperature,
* Corresponding author. Tel.: + 386-1425-1188; fax: +386-1425-
1188.
E-mail address: bojan.podgornik@ctd.uni-lj.si (B. Podgornik).
face distortion and dimensional variations also makes
it possible to reduce or even to eliminate the need for
expensive finishing operations before the component
is put into service [4]. On the other hand, nitriding
causes the formation of a compound or white layer
of iron nitride, e.g. Fe2…4N, at the surface. Although
this layer has a relatively high hardness of 900 –1100
HV and good frictional characteristics, high internal
stresses make it friable and brittle, which can often
lead to spalling during service [5]. This fact somewhat
restricts the use of nitriding processes.
Technologically advanced pulse plasma technology,
employing pulse duration and duty cycle control, en-
sures a more uniform temperature distribution in the
components [6] and at the same time, allows the use
of higher plasma power without the risk of overheat-
ing the surface. Using a higher plasma power short-
ens the nitriding time [7].
The aim of the present work was to investigate and
to compare the mechanical and tribological properties
of two structural steels after either conventional
plasma or pulse plasma nitriding.

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 B. Podgornik, J. Vižintin / Materials Science and Engineering A315 (2001) 28–34 29

Table 1
Chemical composition of the tested steels, wt.%

Steel C Si Mn Cr Mo Ni Al

AISI 4140 (42CrMo4) I 0.47 0.30 0.71 1.01 0.18 0.15 –

AISI A355 (34CrAlMo5) II 0.33 0.25 0.58 1.10 0.18 – 1.08
AISI O2 (90MnCrV8) III 0.93 0.25 1.98 0.28 0.08 0.18 –

Table 2
Details of the surface treatment processes

Process Gas mixture Temperature (°C) Pressure (kPa) Time (h) Pulse (operating/soaking) time (s)

Hardening A Oil 870/180 – 2/1 –

Plasma nitriding B 99.4%H2, 0.6%N2 540 0.254 17 –
Pulse plasma nitriding C 99.4%H2, 0.6%N2 540 0.254 17 0.48/0.02

2. Experimental procedures were carried out using contact profilometry, while sur-
face residual stresses caused by thermochemical treat-
2.1. Sample preparation ment were measured using the hole drilling method [11].

The materials used for this study were AISI 4140 2.2. Wear tests
steel (42CrMo4) and AISI A355 steel (34CrAlMo5), the
chemical compositions of which are shown in Table 1. Wear tests were performed on a pin-on-disc machine
In the specimen preparation phase flat-ended pin sam- in which two stationary pins were loaded on a rotating
ples (f2 mm) were cut out from cylindrical bars with a counterface disc (Fig. 1). Before a test, test couples
hardness of 300 HV, and subsequently machined and were cleaned with benzene in an ultrasonic cleaner.
ground in order to obtain the desired shape and surface Wear tests were carried out at two sliding speeds of 0.1
roughness. Plasma and pulse plasma nitriding were and 1 m s − 1, with two different loads (i.e. 60 and 100
carried out using a commercial unit from Metaplas N) under dry and lubricated conditions at room tem-
Ionon GmbH, while hardening, which was used as a perature and in air with a relative humidity of about
reference, was carried out in a commercial furnace for 50%. In the case of lubricated tests, the base oil VG68
vacuum hardening. without additives was used and it was introduced to the
A compound-free diffusion layer can be produced contact zone by wetting. During wear tests, the fric-
during plasma nitriding by limiting the content of nitro- tional force and linear wear of the pins were recorded
gen in the treatment atmosphere [1,8,9]. Preliminary continuously; the sliding distance was up to 2000 m,
calculations using computer software developed by Sun depending on the wear test conditions involved.
and Bell [10] indicated that a 99.4%H2 – 0.6%N2 gas After completion of the wear test the worn surfaces
mixture should be used to obtain a compound-free were analysed by means of profilometry, as well as by
diffusion zone approximately 0.3 mm thick after optical and scanning electron microscopy.
plasma or pulse plasma nitriding with a duration of 17
h. The details of the nitriding and hardening processes
used in this study are listed in Table 2.
Throughout the series of wear tests disc samples
made from AISI O2 (90MnCrV8) steel were used. The
discs were quenched and tempered to give a hardness of
700 HV.
After surface treatment the pin samples were exam-
ined using a scanning electron microscope. A Vickers
microhardness tester was used to measure surface hard-
ness, as well as to determine the variation in hardness
with distance from the surface. The hardness distribu-
tion with depth was used to determine the nitriding
depth, defined as the depth at which the hardness is 50
HV above the core hardness [5]. Surface roughness and
topography measurements before and after wear tests Fig. 1. Schematic representation of the pin-on-disc test configuration.
30 B. Podgornik, J. Vižintin / Materials Science and Engineering A315 (2001) 28–34
Fig. 2. SEM micrograph of plasma nitrided AISI 4140 steel nitrided
in a 99.4%H2 – 0.6%N2 gas mixture for 17 h at 540°C.
Fig. 3. Microhardness distribution of the steels subjected to different
thermochemical treatments (Table 1 Table 2).
Fig. 4. Residual stress distribution for different surface treatments
and materials (Table 1 Table 2).
3. Results and discussion
3.1. Surface properties
Fig. 2 shows the microstructure of plasma nitrided
AISI 4140 steel nitrided in a 99.4%H2 –0.6%N2
gas mixture for 17 h at 540°C. Microstructural analy-
ses showed that for both steels nitrided in the
99.4%H2 –0.6%N2 gas mixture for 17 h a very thin
(B 1 mm) compound layer was formed over a
diffusion zone of approximately 0.3 mm. A compari-
son of the sample microstructures after conventional
plasma and pulse plasma nitriding showed completely
identical microstructures, as well as compound layer
thicknesses for both the steels used in this investiga-
tion.
The surface hardness, as well as subsurface hard-
ness distribution obtained by hardening, plasma ni-
triding, and pulse plasma nitriding is shown in Fig. 3.
Compared with hardened surfaces with a surface
hardness of approximately 650 HV, plasma nitrided
AISI 4140 and AISI A355 steels showed a surface
peak hardness of approximately 700 and 770 HV, re-
spectively. The same diffusion layer thickness (0.3
mm) was obtained for both materials. Fig. 3 shows
that conventional plasma and pulse plasma nitriding
gave practically the same surface hardness, as well as
diffusion zone thickness on both steels.
For all surface treatments the residual stresses were
found to be compressive. The residual stresses of ni-
trided surfaces are much higher, between 200 and 250
MPa, than those measured for hardened ones (ap-
prox. 50 MPa). However, no essential difference in
residual stresses was observed between conventional
and pulse plasma nitrided steels.
Comparison of plasma nitrided AISI 4140 and
A355 steel shows up to 100 HV higher hardness val-
ues (Fig. 3) and approximately 50 MPa higher com-
pressive residual stresses in the case of AISI A355
steel (Fig. 4). The content of Al, an alloying element
with a very high affinity to nitrogen, leads to both
higher residual stress and higher surface microhard-
ness [12] observed in the case of A355 steel (Figs. 3
and 4).
Results of 3-D topography measurements and a
backscattered SEM photograph of the AISI 4140
steel surface after plasma nitriding are shown in Fig.
5a and b. Nitriding causes the formation of specific
topography characterised by conically shaped asperi-
ties, which in turn increase the surface roughness
(Table 3). After plasma nitriding in a 99.4%H2 –
0.6%N2 gas mixture for 17 h at 540°C, the average
roughness of the ground surface (Ra =0.35 mm)
changed to approximately 0.65 mm for AISI 4140
steel and to 0.61 mm for AISI A355 steel samples.
However, comparison of conventional plasma and
pulse plasma nitrided surfaces showed practically no
difference in surface roughness regardless of the mate-
rial used.
 B. Podgornik, J. Vižintin / Materials Science and Engineering A315 (2001) 28–34 31

3.2. Tribological properties

The average coefficients of friction for variously

treated pins made from the test steels mated with a
hardened ball bearing steel disc under different testing
conditions are shown in Fig. 6. It can be seen that for
both materials and all testing conditions, the coefficient
of friction is largely independent of the type of surface
treatment used in this study.
In the case of dry sliding (Fig. 6a), the coefficient of
friction had a relatively constant value during the test
and lay between 0.5 and 0.65 for a low sliding speed
(0.1 m s − 1) and between 0.25 and 0.35 for a high
sliding speed (1 m s − 1). This indicates that for both
materials an increase in sliding speed results in a change
of contact conditions.
Lubrication of the contact (Fig. 6b) decreased the
coefficient of friction to approximately 0.1 in the case
of low load (60 N) and to approximately 0.17 at 100 N
load, with no difference between the sliding speeds
used. The higher coefficient of friction in the case of the
higher load can be attributed to the increased number
of steel-steel contacts. Comparison of AISI 4140 and
Fig. 5. Three-dimensional surface topography (a) and BEI-SEM AISI A355 steel shows that lower values of the coeffi-
photograph of a plasma nitrided AISI 4140 steel surface (b). cient of friction (up to 10%) were obtained in the case
of AISI A355 steel. This can be attributed to its higher
surface microhardness and consequently the better
abrasive resistance of the treated surface.
Table 3
Average surface roughness of investigated steels after surface treat-
Fig. 6a and b also shows that compared with harden-
ment ing, the nitriding process slightly decreases the coeffi-
cient of friction observed for both materials used in this
Material 4140 A355 investigation. However, there was practically no differ-
ence between the friction coefficients of conventional
Treatment A B C A B C
plasma and pulse plasma nitrided surfaces.
Ra (mm) 0.35 0.65 0.67 0.36 0.61 0.64 The amount of wear was determined as the change in
Rmax (mm) 2.86 9.52 9.80 2.73 8.73 9.17 the pin length, monitored during each wear test by a
linear variable differential transducer. With the configu-

Fig. 6. Average coefficient of friction as a function of load and sliding speed for dry (a) and lubricated (b) sliding.
32 B. Podgornik, J. Vižintin / Materials Science and Engineering A315 (2001) 28–34

Fig. 7. Linear wear of surface treated steel pins as a function of test load and sliding speed for dry (a) and lubricated (b) sliding.

Fig. 8. Wear rate of surface treated steel pins for the region of stable wear for dry (a) and lubricated (b) sliding.

ration described, the disc wear depth was very small
relative to the pin wear and, therefore, the disc wear
was ignored in this study.
In the case of lubricated wear tests, a linear wear rate
was observed for all surface treated pins up to a final
sliding distance of 2000 m. Similar wear behaviour was
observed under dry sliding conditions at a sliding speed
of 0.1 m s − 1, where the same sliding distance of 2000 m
was reached. However, in the case of dry sliding, car-
ried out at a sliding speed of 1 m s − 1, the running-in
period (up to 200 m of sliding) was followed by a severe
wear regime. Due to excessive wear of the pins these
tests were stopped after approximately 500 m of sliding.
Fig. 7 shows pin linear wear for the region of stable
wear as a function of surface treatment and test condi-
tions used. Pin linear wear after 300 m of dry sliding is
shown in Fig. 7a, and after 2000 m of lubricated sliding
in Fig. 7b. For both materials and all surface treat-
ments, the wear increased with the test load and sliding
speed, as expected. The wear rate k for the region of
stable wear is shown in Fig. 8.
The results shown in Figs. 7 and 8 indicate that
conventional plasma and pulse plasma nitriding im-
prove the wear resistance of the steel surface compared
with the hardened samples, and this is true for both dry
and lubricated test conditions. As the test conditions
become increasingly severe, the advantage of the ni-
trided steel surface over the hardened one became more
and more apparent, with the best wear resistance being
obtained in the case of AISI A355 steel, as shown in
Figs. 7 and 8. However, comparison of conventional
plasma and pulse plasma nitriding did not reveal any
noticeable difference in the wear resistance of the inves-
tigated steels.
In the case of dry sliding, the prevailing wear mecha-
nism found for both materials and all surface treat-
ments was subsurface fatigue, confirmed by the
existence of cracks observed a few micrometres under
 B. Podgornik, J. Vižintin / Materials Science and Engineering A315 (2001) 28–34
the surface and in a different growth stage (Fig. 9), a
finding which is in agreement with earlier results [13].
Fig. 9. Cross section of plasma nitrided AISI 4140 steel pin after a
dry sliding wear test at 100 N and 1 m s − 1.
Fig. 10. Surface topography of a hardened (a) and pulse plasma
nitrided (b) AISI A355 steel pin after a lubricated sliding wear test
(6s = 1 m s − 1, FN =100 N, sliding distance 2000 m).
33
However, especially in the case of a high sliding speed
(1 m s − 1), the effect of tempering was observed for all
surface treated pins, indicated by a quick drop in pin
hardness with depth. Worn surfaces of hardened and
pulse plasma nitrided AISI A355 steel pins tested under
lubricated conditions (FN = 100 N, 6s = 1 m s − 1) are
shown in Fig. 10. As a result of mixed lubrication,
traces of abrasive wear were found on the contact
surfaces regardless of the material and surface treat-
ment used. However, superior abrasive wear resistance
with the smallest and shallowest scratches was observed
in the case of plasma nitrided AISI A355 steel (Fig. 10a
and b), which is attributed to its highest surface hard-
ness and residual stresses.
4. Conclusions
Compared with hardening, plasma nitriding improves
the wear resistance of the investigated structural steels
under dry as well as under lubricated sliding, and this
becomes more and more apparent, when testing condi-
tions become increasingly severe.
Compared with conventional plasma nitriding, pulse
plasma nitriding of AISI 4140 and A355 steel results in
practically the same surface roughness, hardness and
residual stresses, as well as compound layer thickness.
At the same time, very similar wear resistance can be
obtained by pulse plasma nitriding.
Addition of alloying elements with a very high
affinity to nitrogen, e.g. Al, increases the hardness and
residual stresses of plasma nitrided steel and, therefore,
improves its wear resistance. This is very important in
the case of mixed or boundary lubrication with a higher
probability of metallic contact appearance.
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