Corrosion Engineering, Science and Technology

The International Journal of Corrosion Processes and Corrosion Control

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Study of plasma nitriding and nitrocarburising

of AISI 430F stainless steel for high hardness and
corrosion resistance

J. Alphonsa, S. Mukherjee & V. S. Raja

To cite this article: J. Alphonsa, S. Mukherjee & V. S. Raja (2018) Study of plasma nitriding and
nitrocarburising of AISI 430F stainless steel for high hardness and corrosion resistance, Corrosion
Engineering, Science and Technology, 53:sup1, 51-58, DOI: 10.1080/1478422X.2017.1396648

To link to this article: https://doi.org/10.1080/1478422X.2017.1396648

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CORROSION ENGINEERING, SCIENCE AND TECHNOLOGY, 2018
VOL. 53, NO. S1, 51–58
https://doi.org/10.1080/1478422X.2017.1396648

Study of plasma nitriding and nitrocarburising of AISI 430F stainless steel for high
hardness and corrosion resistance
J. Alphonsaa, S. Mukherjeea and V. S. Rajab
a
Institute for Plasma Research, FCIPT, Gandhinagar, Gujarat, India; bDepartment of Metallurgical Engineering and Materials Science, Indian Institute
of Technology, Mumbai, India

ABSTRACT ARTICLE HISTORY

In order to improve both the hardness and corrosion resistance properties of AISI 430F stainless steel, Received 2 March 2017
plasma nitriding (PN) and nitrocarburising processes were carried out at different temperatures Accepted 17 August 2017
ranging from 350 to 500°C for 4 h. After PN, the nitrided layer was found to be thicker compared to
KEYWORDS
that obtained by plasma nitrocarburising process. There was an increase in microhardness values Plasma nitriding; hardness;
by a factor of six to seven compared to the plasma nitrided and nitrocarburised specimens plasma nitrocarburising; AISI
respectively, treated at 500°C. The electrochemical corrosion behaviour of the plasma nitrided and 430F; corrosion
nitrocarburised AISI 430F specimens show that the plasma nitrided and nitrocarburised specimens
treated at 400°C for 4 h showed better corrosion resistance and higher surface hardness than the
untreated AISI 430F stainless steel specimens. This is mainly attributed to the presence of nitrogen
in the modified layer existing as a solid solution in the ferrite phase.

This paper is part of a supplementary issue from the 17th Asian Pacific Corrosion Control Conference (APCCC-17).

Introduction [11] at temperatures lower than 450°C indicated that along with
iron nitrides, αN phase too appeared, which is considered to be
Ferritic stainless steels are iron–chromium alloys containing
a supersaturated solid solution of nitrogen in the ferritic phase.
16–30 wt-% Cr along with alloying elements like Mo and Si,
This phase was responsible for improving the corrosion resist-
which are added to stabilise the ferrite phase for a body centred
ance of the ferritic stainless steel [11].
cubic structure at all temperatures as well as to improve proper-
Furthermore, there seem to be no published results as per
ties such as corrosion resistance [1]. Ferritic stainless steels are
the author’s knowledge on PN and nitrocarburising of AISI
being increasingly used in car exhaust pipes, interior and
430F stainless steel, which is a nickel free ferritic stainless
exterior decoration, kitchen utensils, food industry, automotive
steel containing sulphur. Hence, in the present investigation
industry, petrochemical and chemical industries and other
PN and nitrocarburising are carried out on AISI 430F ferritic
functional applications, due to their low cost, workability and
stainless steel at various temperatures in order to obtain high
corrosion resistant properties [2]. These steels are not frequently
surface hardness along with corrosion resistance.
used in conditions requiring resistance to wear because they are
softer relative to austenitic and martensitic stainless steel grades.
The wear resistance of these stainless steels can be improved Experimental
by modifying the surface using different surface modification
Material
techniques. In the past few decades, plasma nitriding (PN)
and nitrocarburising processes have been widely studied by sev- Cylindrical discs of 20 mm diameter and 5 mm thickness
eral authors [3–6] to improve the surface performance, such as were cut perpendicular from an AISI 430F ferritic stainless
hardness, wear as well as corrosion resistance of austenitic and steel rod of diameter 20 mm for this study. The chemical
martensitic stainless steels. Compared to PN where only nitro- composition of AISI 430F ferritic stainless steel used is
gen is used, plasma nitrocarburising (PNC) involves a simul- given in Table 1. The specimens were prepared using stan-
taneous introduction of nitrogen and carbon into the steel. dard metallographic techniques to obtain a final mirror finish
The carbon atmosphere mostly employed in PNC is methane of a mean roughness (Ra) value better than 0.01 µm.
or acetylene. However, only a few published works are available
on PN and PNC of ferritic stainless steels like AISI 439, AISI
Surface modification techniques
405, AISI 441 and AISI 430 [7,8]. It was reported by Oliveira
et al. [9] and Tuckart et al. [10] that PN of AISI 439 and Both PN and PNC processes were conducted in a PN setup as
AISI 405 ferritic stainless steels at 500°C produced thick uni- described elsewhere [12]. The specimens were cleaned with
form layers consisting of iron and chromium nitride phases acetone before placing them on the specimen holder present
compared to that of austenitic stainless steels due to the higher in the vacuum chamber. The specimen holder acted as a cath-
diffusivity of nitrogen in the ferrite network than in the auste- ode and the grounded vacuum chamber wall acted as an anode.
nite phase. Another study on PN of AISI 409L by Gontijo et al. Initially, the vacuum chamber was evacuated to a base pressure

CONTACT J. Alphonsa [email protected] Institute for Plasma Research, FCIPT, Gandhinagar, Gujarat 382 016, India
© 2018 The Author(s). Published by Informa UK Limited, trading as Taylor & Francis Group
This is an Open Access article distributed under the terms of the Creative Commons Attribution-NonCommercial-NoDerivatives License (http://creativecommons.org/licenses/by-nc-nd/4.0/),
which permits non-commercial re-use, distribution, and reproduction in any medium, provided the original work is properly cited, and is not altered, transformed, or built upon in any way.
52 J. ALPHONSA ET AL.

Table 1. Chemical composition of the alloy in wt-%. of the treated surfaces. After PN and PNC, the phases were
Material C Mn Si Cr S P Mo Fe identified using a glancing incidence XRD (3000 PTS X-ray dif-
AISI 430F 0.10 1.17 0.37 16.20 0.32 0.02 0.21 Balance fractometer) with Cu–Kα radiation (λ = 1.5406 Å) as the source
and scanned from 30 to 90° at 2° glancing angle. Mitutoyo (HM
of 8 Pa with the help a mechanical rotary pump. Before plasma 200) micro Vickers hardness tester was used to measure the
processing, sputter cleaning was done for 1 h using hydrogen surface hardness with 50 g load before and after the treatments.
gas at 100 Pa pressure and a temperature of 250°C to get rid
of the surface oxide layer. For PN, a gas mixture consisting
Electrochemical studies
of 80% N2 and 20% H2 was used whereas; a gas mixture of
78% N2, 20% H2 and 2% C2H2 was employed for PNC process. Corrosion behaviour of the untreated, plasma nitrided and
In both the processes a constant pressure of 500 Pa was main- plasma nitrocarburised 430F stainless steel specimens were
tained. During PN and PNC, under the influence of voltage studied using potentiodynamic polarisation technique. The
bias, nitrogen, hydrogen and acetylene gases get ionised and setup consisted of a Reference 600 Gamry potentiostat driven
accelerate to impinge on the specimens. The kinetic energy by a software. The electrochemical tests were carried out in a
of these ions is converted into thermal energy during this ion flat electrochemical glass cell having graphite as a counter
bombardment process, which in turn heats up the specimens. electrode, a saturated calomel electrode (SCE) as a reference
Hence, to get the substrate temperatures of 350, 400, 450 and electrode and the specimen as the working electrode. A speci-
500°C, the bias voltage was adjusted from 400 to 550 V. The men area of 2.85 cm2 was exposed to the solution. The elec-
temperature of the specimens was measured by a J-type ther- trochemical studies were carried out at ambient temperature
mocouple with an accuracy of ±2°C of the set value. The treat- (28°C). The tests were performed in a freely exposed 3.5 wt-
ment duration was kept constant in both the processes for 4 h. % NaCl solution, which was open to the atmosphere. After
After these processes, the bias voltage was reduced to zero and stabilising the open circuit potential (OCP) for 30 min,
the specimens were cooled down to room temperature in a when the drift in the potential became negligible, the poten-
nitrogen gas atmosphere to avoid oxidation before removing tiodynamic polarisation scan was started, by setting a poten-
them from the vacuum chamber. tial 500 mV below the OCP. Each experiment was repeated
at least three times to check for the reproducibility.

Surface characterisation
Results and discussion
Scanning electron microscopy (SEM) was used for studying the
Phase analysis
layer thickness and the surface morphologies after PN and
nitrocarburising processes. Further, Energy dispersive spec- Glancing incidence X-ray diffraction (GIXRD) patterns
trometry (EDS) was used to measure the elemental composition obtained with an incident angle of 2° are shown in Figure 1

Fe3N-Fe4N CrN 500PNC

CrN 500PN Fe3N
Fe4N Fe3N Fe3C Cr C
Fe3N 23 6 Cr23C 6 Fe3N
Fe4N

Fe3N-Fe4N CrN 450PN Fe3C CrN 450PNC

Fe3N
Fe3N Fe4N Fe3N Cr23C6 Fe3N
Fe4N
Intensity in arb. units
Intensity in arb. units

400PN a 400PNC
a a
N NC
Fe3N
Fe3N
Fe3N

a 350PN a 350PNC
N
a
NC
Fe3N Fe3N

Untreated a Untreated
a

35 40 45 50 55 60 35 40 45 50 55 60
2 Theta (Degree) 2 Theta (Degree)

(a) (b)

Figure 1. GIXRD patterns of the (a) plasma nitrided and (b) plasma nitrocarburised specimens treated at different temperatures.
 CORROSION ENGINEERING, SCIENCE AND TECHNOLOGY 53

Table 2. WDS analysis of chemical composition of plasma nitrided and plasma specimens. On the other hand, nitrides and carbides of iron
nitrocarburised layers in wt-% obtained at the cross-sectioned specimens
treated at 400°C for 4 h.
and chromium were found to be formed after PNC (Figure
Treatment Fe Cr Mo Si Mn N C
1(b)), at the above-mentioned temperatures which may be
attributed to the addition of acetylene gas used in this process.
PN 72.77 14.85 0.01 0.01 0.44 11.73 0.05
PNC 71.88 14.34 0.01 0.06 0.32 10.34 3.02

for the untreated along with the 350, 400, 450 and 500°C Effect of temperature on layer thickness
plasma nitrided and plasma nitrocarburised ferritic stainless Images of cross-sectioned plasma nitrided and plasma nitro-
steel specimens. carburised specimens treated at 400 and 500°C are shown in
As expected, the untreated AISI 430F stainless steel shows Figure 2.
the presence of only ferrite phase. On PN and nitrocarburising The microstructure of the layer significantly changed when
at 350 and 400°C the specimens revealed (110) peaks of α phase the treatment temperature was increased from 400 to 500°C.
but at lower 2 theta values. This phase is considered to be a That is, the plasma nitrided and nitrocarburised specimens
supersaturated solid solution of nitrogen in the ferritic phase treated at 400°C showed a layer which did not have significant
and is designated as αN (Figure 1(a)). Such an observation features mainly due to the presence of αN and αNC phases
was also reported by Gontijo et al. with regards to 350 and respectively (Figure 2(a) and (c)). Also, there was no differen-
400°C plasma nitrided AISI 409L ferritic stainless steel [11]. tiation between the treated layers and the substrate micro-
In the 350 and 400°C treated plasma nitrocarburised specimens structure in the specimens treated at 400°C. On the
(Figure 1(b)), αNC is found to be present instead of αN phase, contrary, there was a significant distinction between the trea-
because of the use of acetylene used as a carbon source during ted layers from the substrate microstructure, when the treat-
this process. The presence of carbon in the modified layer is ment temperature was raised to 500°C irrespective of the type
also revealed by WDS results shown in Table 2. of treatment. The modified layer formed at the higher temp-
Further, it is interesting to note the presence of ferrite erature also had a darker appearance indicating that it is
peaks in the XRD pattern of the specimen along with the highly etched (Figure 2(b) and (d)). This appearance is mainly
ones corresponding to αNC indicating that the modified layers due to the presence of chromium nitride precipitates [7,8].
formed by PNC could be thinner than those obtained with Figure 3 shows the variation in thicknesses of the plasma
PN treated specimens at that temperature. It seems that due nitrided and plasma nitrocarburised layers with temperature.
to the low solubility of nitrogen in BCC lattice, the Fe3N It is seen that the layer thicknesses increase with the
phase is also present along with αN and αNC phases, which treatment temperature. Another point worth noting is that
are solid solutions, in the 400°C treated specimens [13]. At the thickness of the plasma nitrided specimens was higher
450 and 500°C the peaks corresponding to αN disappear as compared to the plasma nitrocarburised specimens.
and additional peaks corresponding to CrN appear along The reason why plasma nitrided specimen exhibited higher
with those of Fe4N and Fe3N phases in plasma nitrided thickness than the plasma nitrocarburised layer at a given

Figure 2. Scanning electron microscope images of the cross-sectioned specimen obtained after PN at (a) 400°C and (b) 500°C and PNC at (c) 400°C and (d) 500°C.
54 J. ALPHONSA ET AL.

50 PN
PNC

Thickness of the layer (mm)

40

30

20

10

0
350 400 450 500
Temperature (ºC)

Figure 3. Measured thickness of plasma nitrided and nitrocarburised layers under different process temperatures.

temperature is due to faster diffusion of nitrogen than car- An increase in hardness with temperature was found on all
bon in ferrite, (BCC lattice) phase [14]. This is because of the treated specimens. The hardness values of the 500°C
the fact that the BCC structure is more open [15]. On the plasma nitrided and nitrocarburised surface were found to
contrary, during PNC, in presence of carbon, the thickness be highest among all the cases. They were found to be 1315
of the layer decreases. For this very reason, ferrite peaks HV0.05 and 1532 HV0.05 respectively; which are about 6 and
were visible in the XRD patterns of 350 and 400°C as 7 times as hard as the untreated material. This steep increase
shown in Figure 1(b). de Sousa et al. [16] also reported a in the surface hardness was due to the presence of chromium
similar observation and attributed this to the dissimilar nitride precipitates [17]. However, between the two treatments
nitrogen and carbon diffusion rates in ferrite matrix after PNC has yielded higher hardness values at all these tempera-
PNC process. tures. It is interesting to note that in spite of the thin modified
layer present in 350 and 400°C plasma nitrocarburised speci-
mens; there was an increase in the microhardness values in
Microhardness
comparison to the plasma nitrided specimens. This is attribu-
The microhardness of the untreated AISI 430F stainless ted to the presence of iron nitrides along with the carbon and
steel was measured to be 200 HV0.05. The microhardness nitrogen saturated expanded ferrite phases. Whereas, the
values of plasma nitrided and plasma nitrocarburised higher hardness of 450 and 500°C plasma nitrocarburised
specimens treated at different temperatures are shown in specimens is due to the presence of carbides and nitrides of
Figure 4. iron and chromium present in the modified layer [18].

1600
PN
PNC
1400

1200
Microhardness HV0.05

1000

800

600

400

200

0
350 400 450 500
Temperature (ºC)

Figure 4. Microhardness values obtained on plasma nitrided and plasma nitrocarburised specimens treated at different temperatures.
 CORROSION ENGINEERING, SCIENCE AND TECHNOLOGY 55

1.0

UNT
350PN
0.5 400PN
450PN
500PN

E (V vs. SCE) 0.0

-0.5

-1.0

10-8 10-7 10-6 10-5 10-4 10-3 10-2 10-1

2
i (A/cm )

Figure 5. Potentiodynamic curves of the untreated and plasma nitrided AISI 430F ferritic stainless steels treated at different temperatures in 3.5 wt-% NaCl solution.

Electrochemical corrosion studies in 3.5 wt-% NaCl stainless steel. As brought out earlier, the treatment has
caused an increase in the nitrogen content in the ferritic stain-
Cathodic and anodic polarisation curves of the untreated and
less steel treated at 350 and 400°C without the formation of
treated specimens obtained from 3.5 wt-% NaCl are shown in
any detrimental phases like chromium nitrides while at 450
Figure 5. Table 3 summarises the electrochemical corrosion
and 500°C the alloy forms these phases. Formation of these
parameters such as corrosion potentials (Ecorr) and corrosion
phases (CrN)) leads to chromium depletion in the matrix.
current densities (icorr). The obtained data are within an error
It is well known that nitrogen addition in stainless steels
of 10%.
can significantly increase their corrosion resistance provided
As seen from Figure 5, the anodic polarisation curve of the
it does not lead to chromium depletion [20–22]. Thus, it is
untreated AISI 430F stainless steel obtained from 3.5 wt-%
expected that 350 and 400°C treated specimens shall exhibit
NaCl solution did not show any passive region and very
higher corrosion resistance than the untreated specimen. As
low corrosion potential (−518 mV vs SCE). The reason for
opposed to these specimens, 450 and 500°C treated speci-
the poor corrosion resistance of AISI 430F can be suggested
mens show the presence of CrN phases and consequent chro-
to be due to the presence of MnS inclusions. It is reported
mium depletion in the matrix.
that MnS inclusion promotes localised corrosion in steel as
It was observed from Figure 6 and Table 3 that 350 and
they are known to be the initiation sites of pitting corrosion
400°C plasma nitrocarburised AISI 430F ferritic stainless
[19]. After PN of AISI 430F, it is seen from Figure 5 and
steel behaves similarly to that of plasma nitrided ones at simi-
Table 3 that the Ecorr of 350, and 400°C, 4 h treated specimens
lar temperatures with respect to the untreated specimens.
showed a higher value than that of the untreated specimen.
Thus, the Ecorr values shifts to a higher value on PNC in
However, it decreased on further increasing the treatment
relation to the untreated specimen. Moreover, as compared
temperature to 500°C. It was observed that the corrosion cur-
to the plasma nitrided specimens the Ecorr were found to be
rent densities for the specimens treated at 350 and 400°C were
lower for plasma nitrocarburised specimens. However, the
lower than the untreated specimens. Such observations were
high corrosion current densities compared to that of the
also found in 350 and 400°C plasma nitrided AISI 409 speci-
plasma nitrided specimens indicates an increase in anodic
mens [11].
kinetics during PNC. This is due to the presence of a large
The above results with respect to Ecorr and icorr values can
amount of iron nitrides along with nitrogen and carbon
be explained based on the variation in the anodic and catho-
supersaturated in the ferrite phase. This could be due to the
dic kinetics of untreated and plasmanitrided AISI 430F
lower corrosion resistance of iron nitrides than nitrogen
supersaturated ferrite phases as nitrogen is present as nitrides.
However, when the treatment temperature was further
Table 3. Electrochemical kinetic parameters of plasma nitrided and increased to 450 and 500°C, the Ecorr values significantly
nitrocarburised specimens treated for 4 h obtained in 3.5 wt-% NaCl solution.
reduced. Both 450 and 500°C treated specimen exhibited
Process Treatment temperature °C Ecorr (mV vs SCE) Icorr (µA cm−2)
poor corrosion resistance. This can be attributed to the for-
Untreated – −518 3.80
PN 350 −182 2.50
mation of chromium nitrides and carbides as a consequence
400 −309 3.00 of which chromium depletion occurred at the matrix.
450 −542 3.80 Typical SEM images of the specimens of (a) untreated (b)
500 −729 5.80
PNC 350 −406 5.5
plasma nitrided at 400°C and (c) plasma nitrocarburised at
400 −521 4.30 400°C (d) plasma nitrided at 500°C (e) plasma nitrocar-
450 −623 5.00 burised at 500°C after subjecting them to polarisation tests
500 −742 8.00
are shown in Figure 7. The micrographs of the untreated
56 J. ALPHONSA ET AL.

1.5

UNT
1.0 350PNC
400PNC
450PNC
0.5 500PNC
E(Vvs. SCE)
0.0

-0.5

-1.0

-1.5
10-8 10-7 10-6 10-5 10-4 10-3 10-2 10-1
i (A/cm2)

Figure 6. Potentiodynamic curves in 3.5 wt-% NaCl solution of the untreated and plasma nitrocarburised AISI 430F ferritic stainless steel at different temperatures.

Figure 7. SEM images of specimens obtained after the polarisation tests for (a) untreated (b) plasma nitrided at 400°C (c) plasma nitrocarburised at 400°C (d) plasma
nitrided at 500°C (e) plasma nitrocarburised at 500°C conditions.
 CORROSION ENGINEERING, SCIENCE AND TECHNOLOGY 57

specimen, after polarisation test, show a large number of deep causing this problem. However, among the plasma
pits (about 25 µm) supporting the potentiodynamic data nitrided and nitrocarburised specimens treated at 400°
(Figure 7(a)). Compared to the untreated specimens, 400°C C, the corrosion resistance was better compared to the
treated specimens had only a fewer pits of small sizes untreated specimens mainly due to the presence of
(about 5 µm) indicating improvement in pitting resistance nitrogen in solid solution as revealed by few pits of
(Figure 7(b) and (c)). This is mainly due to the presence of smaller sizes. At 450 and 500°C, plasma nitrided and
nitrogen in solid solution as revealed by WDS analysis nitrocarburised specimens treated for 4 h lost the pas-
shown in Table 2. The EDS analysis at a location near the sivity and this was mainly due to the chromium
pit of 400°C treated specimen showed chromium and iron depletion in the alloy matrix.
contents to be Fe: 72.77 and Cr: 14.85 wt-% respectively for (v) 400°C, 4 h treatment gave optimised hardness and cor-
PN case and Fe: 71.88 and Cr: 14.85 wt-% respectively for rosion resistance in both the treatments.
PNC case indicating that there was only a slight decrease
compared to the untreated specimen (Fe: 79.96 wt-% and
Cr: 15.67 wt-%). At 500°C, the entire surface of the specimen Acknowledgements
was found to have suffered severe corrosion. The extensive
The authors acknowledge Dr S.L. Kamath of IIT Bombay (IIT B) and
uniform corrosion seen in Figure 7(d) and (e) could be attrib-
Mrs Purvi Dave (FCIPT) for carrying out SEM and EDS analysis. One
uted to the extensive loss of Cr in the matrix as observed from of the authors J. Alphonsa expresses her gratitude to Mr G. Jhala for
the EDS analysis (Cr: 13.35; and Fe: 67.53; in wt-%) in plasma his assistance in conducting the experiments. The National Facility
nitrided and (Cr: 12.85; and Fe: 63.55 in wt-%) in plasma (OIM and Texture Lab), Department of Metallurgical Engineering and
nitrocarburised specimens due to the formation of a large Materials Science, IITB extended its facility to carry out GIXRD studies.
The authors would like to acknowledge Sophisticated Analytical Instru-
amount of iron and chromium nitrides in the former and
ment Facility, IITB for WDS studies.
their nitrides/carbides in the later as has been revealed by
XRD patterns (Figure 1(a) and (b)).
From these results, it is found that 400°C plasma nitrided Disclosure statement
and nitrocarburised specimens treated for 4 h exhibited
No potential conflict of interest was reported by the authors.
higher surface hardness and better corrosion resistance
among all the treated specimens. Hence, plasma nitrided
and nitrocarburised specimens treated at 400°C for 4 h can References
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