Surface and Coatings Technology 116–119 (1999) 205–211

www.elsevier.nl/locate/surfcoat

Plasma nitriding of stainless steels at low temperatures

B. Larisch *, U. Brusky, H.-J. Spies
TU Bergakademie Freiberg, Institute of Material Engineering, Gustav-Zeuner-Str. 5, 09596 Freiberg, Germany

Abstract

To avoid the drop in corrosion resistance of stainless steels in conventional nitriding (precipitation of CrN ), low-temperature
techniques like ion implantation, plasma immersion ion implantation (PIII, PI 3) and low-temperature plasma nitriding were
developed. In this investigation, four stainless-steel grades (ferritic: X6Cr17, austenitic–ferritic: X2CrNiMoN22.5.3, austenitic:
X8CrNiTi18.10 and X5CrNi18.10) were plasma-nitrided between 250 and 500°C. Nitrogen-enriched layers with a high nitrogen
content were produced, leading to a significant increase in surface hardness. X-ray diffraction indicated that CrN did not precipitate
if treatment temperatures did not exceed 400°C. ‘Expanded austenite’ formed in the austenitic and duplex steels and e-nitride
(Fe N ) in the ferritic steel. The optically visible structure of the nitrided cases is comparable with that of the PIII layers, with
2 1−x
higher charging densities being possible in the plasma nitriding. Also, in comparison to conventional ion implantation, large
charges and parts with complicated shapes can be treated. © 1999 Elsevier Science S.A. All rights reserved.

Keywords: Expanded austenite; Plasma nitriding; S-phase; Stainless steels

1. Introduction neous nitriding of all sides of the workpiece. In ion

Stainless steels have an excellent corrosion resistance
because of their native passive layer. However, their
load-bearing capacity is not very high. To increase the
surface hardness, conventional nitriding in gas and
plasma [1–4] was initially carried out leading to a drop
in corrosion resistance due to the formation of CrN
precipitates at temperatures above 400°C [3,5]. Plasma
nitriding was therefore carried out at lower temperatures
[3]. However, very long nitriding times were necessary
to obtain only relatively thin layers (AISI 316;
400°C/60 h: 20mm [3]). While activities in the field of
plasma nitriding had abated, techniques like ion implant-
ation [6 ] and plasma immersion ion implantation (PIII
or PI 3) [7–9] have been used more in recent times, with
the former technique being taken up again, now leading
to more optimal processes. Though all three techniques
are used in the case of austenitic steel nitriding, ferritic
and duplex [10] stainless steels have received less atten-
tion until now.
Implantation is restricted by its line-of-sight nature.
In contrast, PIII and plasma nitriding allow a simulta-
* Corresponding author. Tel.: +49-3731393102;
fax: +49-373393657.
E-mail address: larisch@ww.tu-freiberg.de (B. Larisch)
implantation and PIII, the temperature regime strongly
depends on the plasma parameters (i.e. ion energy, pulse
frequency, etc.). This effect is not as strong in plasma
nitriding due to lower ion energies.
Low-temperature plasma nitriding (LTPN; T<
500°C ) had been carried out using d.c., triode [23] and
r.f. systems as well as d.c. triode magnetron reactive
sputtering ( Table 1). LTPN can produce nitrogen-
enriched layers with structures comparable to those of
PIII layers [6 ]. These layers have a high hardness and
are not only wear-resistant but, above all, corrosion
resistant. In austenitic stainless steels and duplex steels,
a phase forms, called ‘expanded austenite’ [8] or
‘S-phase’ [7,12,13], whereby nitrogen remains in solid
solution in the f.c.c. lattice [6 ] (T≤450°C ). The real
nature of this metastable phase is a controversial theme
and is still an unknown territory [6,13–19].
Since the investigations mentioned above were con-
ducted with laboratory equipment, little can be said
about the possibility of producing such layers in devices
of industrial size. A French group [4,16,30], already
working for some time now in this field, as well as
Menthe/Rie [15] and Dearnley [13], presented some
screening results concerning layers produced in larger
furnaces. Furthermore, there is a wide range of investi-

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206 B. Larisch et al. / Surface and Coatings Technology 116–119 (1999) 205–211

Table 1
Literature review of nitriding conditions for stainless steels

Reference PN Steels T (°C ) t (h) P (Pa) N :H (%) Electrical parameter

2 2
[20] AISI 304:X5CrNi18.10 400, 550 4 667 80:20
[21] 18-8 400+550/450/ 4; 40+4/2/4 667 80:20 300; 330; 395 V
550
21;25, 43 A m−2
[6 ] X5CrNi18 10 400 10 min, 30 min 1200 15:85 400 V
[22] X5CrNi18 10 400, 500 0.5; 1 332–465 25:75 1.6–3.2 mA cm−2
[24] r.f. AISI 316: X5CrNiMo17.12.2 400 100% N
2
[11] r.f. AISI 316:X5CrNiMo17.12.2 400 3 c. 50 V
[2] d.c. X3CrNi18 10 450, 500, 550 1; 5; 12; 30 400–670 25:75 400–450 V
70:30
[3] d.c. AISI 316: X5CrNiMo17.12.2 400 60 400–600 25:75
[4] d.c. X5CrNi18 10 500, 550, 600, A few (3–16) >133 NH , N 700 V
3 2
650
1 W cm−2
[13] d.c. AISI 316: X5CrNiMo17.12.2 450–950 300–400 NH ; 5N 600–800 V
3 2
+95H
2
20 kW
( Klöckner plant)
[25] d.c. 13Cr; 13Cr +2Ti/3V/3W/2Nb/ 500, 550, 600 1; 3; 6 800 50:50 c. 300–500 V
3Al/3Zr or 3Si
[26 ] d.c. triode AISI17/4PH; 420 30 1000 25:75 500 V
AISI 316: X5CrNiMo17.12.2
[27] Pulse d.c. AISI 304: X5CrNi1810 380, 460 20, 48 H,N 10 kW
2 2
(thyristor-controlled )
AISI 316: X5CrNiMo17.12.2
AISI 321: X6CrNiTi18.10
[15] Pulse d.c. AISI 304L:X3CrNi18.10 400–600 5 400 80:20 410 V
X20Cr13 PD: 50–200 ms
X4CrNiMoN27 5 2 PR: 50–1000 ms
Ni42
[10] Pulse d.c. X2CrNiMoN22 5 3 350 40 150 2N :1H 470–480 V
2 2
industrial plant
X2CrNiMo17 13 2 400 20
X1CrNiMoNb28 4 2
[16 ] d.c. sputtering AISI 310: X12CrNi25 20 300 0.4–4 Ar; N d.c. triode
2
magnetron sputtering

gated process parameters in d.c., triode, r.f. or pulse
plasma nitriding (Table 1) that do not allow a compari-
son of these processes in general.
Pulse plasma nitriding is a well-established process in
industry. The austenitic, duplex and ferritic stainless
steels were therefore treated in such an industrial nitrid-
ing equipment.
2. Experimental
Ferritic X6Cr17, austenitic steel grades X8CrNiTi18
10 and X5CrNi18 10 and duplex austenitic–ferritic steel
X2CrNiMoN22 5 3 samples were ground or polished
using 3-mm diamond paste and then degreased with
alcohol before being plasma-nitrided. A commercial
plasma-nitriding apparatus (pulsed d.c.) was used, with
an auxiliary heater being used for sample heating. In
contrast to other investigations ( Table 1), argon was
used in addition to nitrogen and hydrogen with relatively
long nitriding times. The nitriding experiments were
conducted in the temperature range of 250–500°C for
8–60 h at 300 Pa and 400–450 V. The pulse duration/
pulse repetition ratio was 50 ms/100 ms. Gas mixtures of
40–80% N , 10–30% H and 10–30% Ar were used.
2 2
After treatment, the samples were sectioned, nickel-
plated, ground and polished for optical microscopy and
etched in Beraha II solution. Glow discharge optical
spectroscopy (GDOS ) was conducted. The phases near
to the surface were identified using glancing-angle X-ray
diffraction ( Y- diffractometer method; radiation CuKa),
whereby different slits had to be used for technical
reasons. Furthermore, XRD measurements at incident
angles (a) of 2, 5 and 12° were carried out on selected
samples. The surface roughness was measured with a
laser optical system (auto focus principle). The micro-
hardness was estimated by load/displacement measure-
ments using a Vickers indenter and a maximum load of
1 N. Five indentations were made on each sample from
which average hardness values were calculated.
 B. Larisch et al. / Surface and Coatings Technology 116–119 (1999) 205–211
3. Results and discussion
3.1. Diffusion depths
Plasma nitriding in the temperature range 250–500°C
can produce nitrogen-enriched layers with high nitrogen
contents. The maximum concentrations of N mostly
ranged between c. 20 and 40 at.%. The layer thickness
and nitrogen concentration mainly depend on the tem-
perature, the nitriding time and the steel grade. The
higher concentration values and larger diffusion depths
correspond to higher temperatures (Fig. 1) and longer
nitriding times. As is known, the nitrogen diffusion is
faster in the ferrite ( X6Cr17) than in the austenite
( X5CrNi18 10). The duplex steel showed the lowest
case depths ( Fig. 2). The reason for the relatively low
case depths in Fig. 2 will be discussed in the next section.
To investigate the effect of gas composition, the ratio
of N :H :Ar (4:3:3; 6:3:1; 6:1:3; 8:1:1) was varied at a
2 2
constant total flux. In contrast to the literature [31], no
clear or significant influence of gas composition was
found from the nitrogen concentration profiles (Fig. 3,
Fig. 1. GDOS depth profiles of plasma nitrided X6Cr17.
Fig. 2. GDOS depth profiles of the plasma-nitrided samples (350°C;
26 h).
207
Table 2). However, from the way things stand at the
moment, it seems that a gas mixture of 80% N +10%
2
H +10% Ar leads to a weaker reproducibility. Often,
2
lower diffusion depths and nitrogen concentrations were
found when compared to the samples treated with the
other gas compositions (Fig. 3, Table 2).
This effect seems to be caused by the low proportions
of argon or hydrogen. In agreement with Wei [14], it is
assumed that the ion energy must be sufficiently high to
sputter-remove the native oxide layer. Furthermore, the
dissociative adsorption reaction of nitrogen could be
assisted by hydrogen (formation of N–H radicals,
according to the models of Szasz [14] and of gas
nitriding). It has been observed that the addition of
argon leads to a higher current density (higher effective
currents). This could result in a higher plasma density
that might lead to a more efficient dissociation or
activation of nitrogen molecules and/or an increase in
sputtering effects. Therefore, gas mixtures with higher
argon and/or hydrogen proportions are recommended.
If the surface barriers are overcome by sputtering, then
further layer growth is diffusion-controlled. Also, a
higher voltage leading to stronger bombardment of the
surfaces improves the results ( Fig. 3, Table 2). Further
experiments are necessary to investigate these effects in
more detail.
It seems that, especially for longer nitriding times,
the same ‘growth rates’ (W ) can be achieved as much
by plasma nitriding as by PIII or ion implantation
( Table 3). This supports the conclusion that the process
is diffusion-controlled, although a longer incubation
time cannot be excluded in plasma nitriding when com-
pared to ion implantation and PIII. However, there is
a wide scattering band for each technique, depending
on the process parameters. Normally, probably due to
the stronger heating effect of the ions with higher
energies, lower treatment times are chosen for ion
implantation and plasma immersion ion implantation
(mostly 120 min max.) compared to plasma nitriding.
In plasma nitriding and PIII, the temperature can be
regulated independently of the plasma parameters (pulse
frequency, power, etc.) due to the lower ion energies
and the possibility of cooling the workpieces by an
auxiliary cooling unit in the furnace wall during nitrid-
ing. This enables the production of thicker layers.
3.2. Micro-structure
The polished cross-sections were etched in Beraha II
solution. Micrographs of the structures of the nitrided
layers are presented in Fig. 4a–c.
The nitrided case in the X5CrNi18 10 ( Fig. 4a) is
relatively thin (2.5 mm) with a sharp boundary to the
core material. Due to better nitrogen diffusion in
the b.c.c. lattice, a thicker layer (14.6 mm) grows in the
X6Cr17 (Fig. 4b). The inner part of the nitrided, white
208 B. Larisch et al. / Surface and Coatings Technology 116–119 (1999) 205–211

Fig. 3. Influence of the gas composition on the nitrided case depth and the nitrogen content in the layer ( X5CrNi18.10; 350°C; 16 h; 400 V ).

Table 2 is also a transition zone to the core material. The

Influence of gas composition (and voltage) on ‘growth rate’ austenitic–ferritic steel (Fig. 4c) shows different layer
Nitriding conditions: ‘Growth rate’: thicknesses (average value 1.7 mm) in the two phases
350°C, 16 h, 400 V W=d/앀ta (mm h−0.5) due to the different diffusion velocities, as mentioned
above. In contrast to the pure ferritic steel, the boundary
N :H :Ar X5CrNi18 10 X6Cr17 line in the duplex steel is relatively sharp.
2 2
40:30:30 1.30 4.12 For higher nitriding temperatures, the nitrided layers
40:30:30 (450 V ) 2.20 >5.95b have a darker appearance, indicating less corrosion
60:10:30 1.18 3.85 resistance. The layer thickness (Fig. 4) corresponds well
60:30:10 1.31 3.30 with the nitrogen diffusion depths ( Fig. 2) estimated
80:10:10 (450 V ) 0.50 3.05
by GDOS.
a d: case depth; t: time.
b The layer was thicker than the depth measurable by GDOS.
3.3. Phase analysis by X-ray diffraction
Table 3
Comparison of the ‘growth rate’of the layers obtained by plasma Diffraction patterns of the austenitic steel X8Cr-
immersion ion implantation (PIII ), ion implantation (II ), plasma nit- NiTi18 10 are shown in Fig. 5. Up to temperatures of
riding (PN ) and gas nitriding (GN ) at 400°C ( X5CrNi18 10; AISI304, 400°C, a set of broad peaks are observable together
AISI 304L)
with the substrate austenite peaks.
X5CrNi18 10 W=d/앀t (mm h−0.5) With increasing temperature and time, the substrate
austenite peaks disappear due to increasing layer thick-
Technique 400°C Reference ness. The broad peaks have been associated with a
PIII/25–45 keV 1.24–2.56 [22] metastable phase called ’’expanded austenite‘‘ or
I /0.7 keV–60 keV 1.24–4.42 [14,22,28,29] ‘S-phase’. The lines of the austenite are shifted towards
PN 0.46–2.50 [14,15,20,22] smaller angles, and the peaks become broader, indicating
GN 0.39–1.01 [22] an expansion of the lattice due to nitrogen in the
Puls — PN/300°C 0.36–0.39 IWT Freiberg
interstitial solution. Analogous patterns were found on
Puls — PN/350°C 0.50–0.67 This investigation
Puls — PN/400°C 1.36–3.20 80N :10H :10Ar (%) ion-implanted samples, as shown in Fig. 5. As observed
2 2 for austenitic steels nitrided by ion implantation, nitro-
GN/400°C 0.60–0.95 IWT Freiberg
gen remains in solid solution in the fcc lattice if the
temperature is less than 400°C [7]. At 450°C, depending
layer is not as white as the outer region (7 mm), and on the nitriding time, CrN begins to precipitate, and
needle-like structures can be seen, which are interpreted c∞-Fe N forms simultaneously.
4
as deformation bands. This deformation seems to occur For duplex steel plasma-nitrided below 350°C, a
as a result of the high internal stresses in the case. There transformation of ferrite into expanded austenite was
 B. Larisch et al. / Surface and Coatings Technology 116–119 (1999) 205–211
Fig. 4. Microstructures of the nitrided samples (350°C; 26 h).
observed (Fig. 6). This has been attributed here to the
reduction of ferrite content in the XRD patterns, especi-
ally compared to the untreated steel. The ferritic steel
X6Cr17 and the ferritic phase in the duplex steel
X2CrNiMoN22.5.3 behave differently. This can be
209
Fig. 5. XRD patterns obtained from ion-nitrided and ion-implanted
X8CrNiTi18 10.
Fig. 6. XRD patterns of the X2CrNiMoN22 5 3, nitrided: 300°C/60 h.
Fig. 7. XRD patterns of the X6Cr17, nitrided: 350°C/26 h.
ascribed to the fact that the ferritic phase in the duplex
steel contains c. 4 wt% nickel, assisting the transforma-
tion into austenite.
210 B. Larisch et al. / Surface and Coatings Technology 116–119 (1999) 205–211

Table 4
Results of the XRD-phase analysis after plasma nitriding at different temperatures and times

Steel grade 300°C/60 h 350°C/26 h 350°C/40 h 450°C/26 h 500°C/20 h

X6Cr17 (ferritic) Ferrite Fe N Ferrite Fe N Ferrite Fe N Ferrite Fe N Fe N Fe N CrN

2 1−x 2 1−x 2 1−x 2 1−x 2 1−x 4
Fe N ? CrN ? Fe N CrN
4 4
X8CrNiTi18 10 (austenitic) Austenite exp. aust. Austenite exp. aust. Austenite exp. aust. Exp. aust. Fe N CrN Fe N CrN
4 4
X2CrNiMoN22 5 3 Ferrite austenite Ferrite austenite Austenite ( Exp. aust.)
(ferritic–austenitic) exp. aust. exp. aust. exp. aust. CrN ferrite Fe N
4

At 350°C, the ferrite peaks disappear due to the
transformation of ferrite into expanded austenite. At
higher nitriding temperatures, the austenite (substrate)
transforms into ferrite and CrN. As a result CrN, ferrite
and c∞-Fe N can be seen in the XRD patterns
4
(500°C/20 h). No substrate austenite peak is observed
because the layer is relatively thick.
The XRD patterns of the ferritic steel show peaks of
ferrite and e-Fe N (i.e. Fe N ) after plasma nitriding
2 1−x 3
for 26 h at 350°C (Fig. 7).
With longer treatment times (40 h), the amount of
e-Fe N increases. The formation of CrN and
2 1−x
c∞-Fe N cannot be excluded, although the XRD patterns
4
show no clear evidence of these phases. After treatment
at higher temperatures (450°C, 26 h) e-Fe N , c∞-
2 1−x
Fe N and CrN were detected by XRD.
4
The results of the X-ray measurements are summa-
rized in Table 4.
X-ray measurements (sin2 Y method ) in the expanded
austenite [(311) interference] showed evidence of high
internal stresses. In the X8CrNiTi18 10, maximum
values were measured in samples nitrided within the
temperature range of 300°C (−3,3 GPa) to 350°C
(−3.6 GPa).
3.4. Surface roughness
Surface roughness increases with temperature and
time ( Table 5). Plasma nitriding at low temperatures
(<400°C ) and shorter nitriding times leads to a relatively
low increase in surface roughness. For the industrial
application of these layers, a further surface finish seems
unnecessary.
3.5. Micro-hardness measurements
The micro-hardness values are influenced by the core
material and the thickness and structure of the layer.
Because of the thin, modified near-surface regions, it is
impossible to measure the hardness of the layer alone.
Due to the surface roughness, higher loads (>1000 mN )
must be used. The hardness values increase with temper-
ature and nitriding time ( Table 6) due to an increasing
layer thickness (d : at 1 wt% nitrogen; GDOS
N
measurements).
4. Summary and conclusions
These screening experiments show that nitrogen-
enriched layers of sufficient thickness can be produced
in stainless steels in an industrial plant at temperatures
at and below 400°C. The micro-structure of these layers
is identical to that produced by ion implantation. In the
austenitic and duplex steels, expanded austenite was
observed with high concentrations of nitrogen in the
solid solution. The XRD patterns of the ferritic steel
show peaks of ferrite and Fe N (i.e. Fe N ) after
2 1−x 3
plasma nitriding at temperatures below 400°C. The
micro-hardness of the steels increased with temperature
and time, i.e. the nitrided layer thickness. To ensure a
high process certainty, minimum hydrogen and argon
percentages seem to be necessary. The optimum nitriding
parameters have not yet been determined. In screening
tests, no significant decrease in the corrosion resistance
has been observed for samples nitrided at and below
350°C. These results will be presented elsewhere.
The ‘growth rates’ in plasma nitriding are comparable

Table 5
Roughness values R (mm) before and after plasma nitriding of the Table 6
a
steels Hardness values, HV, of plasma-nitrided X8CrNiTi18 10 samples

Nitriding X6Cr17 X8CrNiTi18 X5CrNi18 10 Nitriding: Max. N d (mm) HV (N mm−2)

N
T (°C )/t (h) 10 (ground ) T (°C )/t (h) (wt%) F=1000 mN

– 0.012 0.17 0.02 – – – 2350

300/60 0.18 0.23 0.06 300°C/60 h 7.9 2.0 3305
350/26 0.23 0.21 0.11 350°C/40 h 7.4 6.4 4285
350/40 0.40 0.20 0.16 400°C/26 h 8.9 10 6399
500/20 0.64 0.87 0.61 450°C/26 h 12.5 32.6 8292
 B. Larisch et al. / Surface and Coatings Technology 116–119 (1999) 205–211
to those of PIII or ion implantation, although longer
incubation times cannot be excluded.
In comparison to PIII [7,9] or ion implantation [14]
in pulsed d.c. plasma nitriding, the temperature regu-
lation is more independent of plasma parameters.
Therfore, longer nitriding times are possible, and thicker
layers can be produced. In comparison to the conven-
tional ion implantation, large charges and parts with
complicated shapes can be treated. Compared to PIII,
higher charging densities are possible in plasma nitrid-
ing. Stainless steels can be treated in available com-
mercial plasma-nitriding units, thus avoiding higher
investments.
Acknowledgements
This investigations were supported financially by the
Sächsisches Ministerium für Wissenschaft und Kunst
(SMWK; 4-7531.50-03-FZR/603)
Dr E. Richter and S. Parascandola (Institute of Ion
Beam Physics and Materials Research, Forschungs-
zentrum Rossendorf ) put the ion-implanted sample
(Fig. 5) at our disposal.
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