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Department of Materials Science, Graduate School of Engineering, Osaka Prefecture University, 1-1 Gakuen-cho, Sakai-shi, 599-8531, Japan
b
Technology Research Institute of Osaka Prefecture, 7-1, Ayumino 2, Izumi-shi, Osaka 594-1157, Japan
c
Department of Materials Science and Engineering, Kanazawa University, Kakuma-machi, Kanazawa, 920-1192, Japan
Available online 28 October 2004
Abstract
Expanded austenite by low temperature plasma nitriding of austenitic stainless steels pushes carbon ahead of the nitrided layer.
Apparently, this phenomenon accompanies uphill carbon diffusion. Clarifying the mechanism of this carbon push-ahead effect is important
for controlling treated-layer microstructure. This investigation is intended to clear the push-ahead effect of specimens treated with a
combination of carburizing and nitriding. Plasma treatments were carried out for 18Cr8Ni steel in 667 Pa at 673 K. We used the
following gas-flow ratios: 80% N220% H2 for nitriding; Ar gas mixed with 5% CH4 for carburizing; and 80% N2 mixed with from 5%
CH4 and balancing H2 for simultaneous carburizing and nitriding. Glow-discharge optical emission spectroscopy (GDOES) indicated an
accumulated carbon layer beyond the nitrogen plateau on the nitrided specimen of pre-carburized sample. Such a carbon accumulation
profile also resulted from simultaneous treatment. Furthermore, carbon accumulated similarly in cases of carburizing after nitriding
treatment. Nitrided specimens of pre-carburized samples have a small carbon peak just under the surface on GDOES profile. This small
carbon peak weakened and disappeared with increasing nitriding time. X-ray diffraction analysis revealed formation of e (Fe23N) phase
just under the surface of the nitrided pre-carburized sample.
D 2004 Elsevier B.V. All rights reserved.
Keywords: Diffusion; Carburizing; Microstructure control; Austenitic stainless steel; Surface improvement
1. Introduction
Low temperature plasma nitriding hardens the surface
of austenitic stainless steel without deterioration of
corrosion resistance [15]. The distribution of dissolved
carbon in austenitic stainless steels changes by low
temperature nitriding. Expanded austenite by low temperature plasma nitriding of austenitic stainless steels pushes
carbon ahead of the nitrided layer. Thereby, the changed
carbon profile shows the carbon accumulation beyond the
front of the nitrided layer. This phenomenon has been
observed widely with a variety of profiling techniques
[58].
* Corresponding author. Tel.: +81 72 254 9317; fax: +81 72 254 9912.
E-mail address: masato@mtl.osakafu-u.ac.jp (M. Tsujikawa).
0257-8972/$ - see front matter D 2004 Elsevier B.V. All rights reserved.
doi:10.1016/j.surfcoat.2004.08.179
310
Table 1
Plasma treatment and specimen designation
Process
Nitriding
Carburizing
Simultaneous
process
Sequential
process
Symbol
First process
Second process
Temperature
(K)
N2
H2
Ar
8N
4C
8(C+N)
673
673
673
5
5
80
80
20
15
15
80
8
4
8
4C4N
8C4N
16C4N
24C4N
4C8N
4C16N
4C24N
4N4C
4N4C450
673
673
673
673
673
673
673
673
673
5
5
5
5
5
5
5
80
80
15
15
15
15
15
15
15
20
20
80
80
80
80
80
80
80
4
8
16
24
4
4
4
4
4
673
673
673
673
673
673
673
673
723
Process
time (h)
Temperature
(K)
Process
time (h)
Total
process
time (h)
N2
H2
Ar
8
4
8
5
5
80
80
80
80
80
80
80
20
20
20
20
20
20
20
15
15
80
80
4
4
4
4
8
16
24
4
4
8
12
20
28
12
20
28
8
8
2. Experimental procedures
The material used in this work is austenitic stainless,
which satisfies the grade of AISI 304. The chemical
composition of the specimen is Fe18.8 Cr8.3 Ni0.94
Mn0.21 Mo0.31 Cu0.4 Si0.037 P0.003 S0.06 C in
mass%. Roughly cut AISI 304 plates were solution treated
at 1303 K for 2.7 ks. Then they were dry ground slightly to
the specimen shape of 25 mm width, 50 mm length and 5
mm thickness. These preparations gave the specimens a
fully austenitic structure, which was confirmed by X-ray
diffraction analysis [13].
Plasma thermo-chemical treatment was performed with a
laboratory type apparatus with a d.c. power source. Each
specimen attached with a thermo couple was set in the furnace
as cathode. After evacuation up to 1.3310 1 Pa, the
pressure of the mixed gas for each specimen was adjusted
to 6.67102 Pa. All thermo-chemical treatment was performed in this study at 673 K, with the exception of the 4N
4C450 specimen. Its second process was treatment at 723 K.
Table 1 shows details of each plasma treatment with
specimen symbols. For example, the 8N specimen was
plasma treated at 673 K with a mixture of 80% nitrogen gas
and 20% hydrogen gas for 8 h. The 8(C+N) specimen was
treated by plasma carbo-nitriding process for 8 h at 673 K
with a mixture of nitrogen, methane, and hydrogen gases.
Similarly, the 4C4N specimen was first treated by plasma
carburizing for 4 h at 673 K, then followed by plasma
nitriding for 4 h at 673 K. In such sequential processes, gas
mixture changes were made at within 10 s without temperature change. After treatment, the specimens were allowed
to cool in the evacuated furnace.
X-ray diffraction analysis (XRD) using Cu-Ka (40 kV,
150 mA) radiation with a monochrometer, was undertaken
Fig. 1. GDS depth profiles of carburized specimen (a) and nitrided precarburized specimen (b).
311
312
(2)
(3)
(4)
Fig. 8. XRD patterns for nitrided pre-carburized specimens with various
nitriding times.
A series of nitriding and carburizing by plasma processing at relatively low temperature qualitatively clarified the
behavior of carbon in nitriding as followings:
(1)
References
[1]
[2]
[3]
[4]
[5]
[6]
[7]
[8]
[9]
4. Conclusions
313
[10]
[11]
[12]
[13]
[14]