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Low temperature ion nitriding of Ti-6Al-4V alloy

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2017 J. Phys.: Conf. Ser. 830 012066

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International Conference
5th International CongressononRecent
EnergyTrends inand
Fluxes Physics 2016 (ICRTP2016)
Radiation Effects 2016 IOP Publishing
Journal of Physics:
IOP Conf. Conference
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Series011001
830 (2017) 012066
1234567890 doi:10.1088/1742-6596/755/1/011001
doi :10.1088/1742-6596/830/1/012066

Low temperature ion nitriding of Ti-6Al-4V alloy

R D Agzamov, K N Ramazanov, A F Tagirov, E L Vardanyan

Ufa State Aviation Technical University, Department of Mechanical Engineering, ul.
Karla Marksa 12, Ufa, Russia

E-mail: vipt127@yandex.ru

Abstract. The paper presents the results of nitriding the titanium alloy VT6 (Ti-6Al-4V) in a
non-self-maintained high-current discharge and in a glow discharge in different regimes.
Nitriding was conducted in pure nitrogen and in the mixture of nitrogen and argon. It is shown
that microhardness of the samples increased; however, the efficiency of surface modification
depends on the modification conditions.

1. Introduction
Currently, titanium alloys play an important role in aviation and space industry due to heat resistance,
high specific strength, high corrosion resistance, low density and non-magnetization.
However, along with the positive characteristics such alloys also demonstrate disadvantageous
properties: low surface hardness and poor tribological characteristics [1, 2].
Surface modification can improve physical and mechanical properties of titanium alloys. The use
of traditional gas nitriding in this case is impossible because this type of treatment requires
temperatures in the range of 800-900 °C. Ion nitriding is one of the most efficient methods of surface
treatment that increase hardness, wear resistance, and corrosion resistance. The temperature of
nitriding of titanium alloys can be reduced in glow discharge and non-self-maintained arc discharge
plasmas. Low temperature nitriding can preserve high quality of surface and exclude deformation of
final products [3,4,5].
The aim of this work is to study the impact of low temperature ion nitriding on the microhardness
and depth of the hardened Ti-6Al-4V layer.

2. Experimental approach
The Ti-6Al-4V alloy with chemical composition presented in Table 1 was used as the initial material
for the investigations.

Table 1. Chemical composition of steel [wt%]

Fe C Si V N Ti Al Zr O H
0.3 0.1 0.15 3.5–5.3 0.05 86.485–91.2 5.3–6.8 0.3 0.2 0.015

Literature analysis has shown that gas composition influences the hardness of a surface [5].
Nitriding of the titanium alloy was carried out in the mixture of argon and nitrogen of different
concentrations. It is also known [1-5] that the depth of a nitrided layer is substantially impacted by
temperature and time of exposure.

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5th International Congress on Energy Fluxes and Radiation Effects 2016 IOP Publishing
IOP Conf. Series: Journal of Physics: Conf. Series 1234567890
830 (2017) 012066 doi:10.1088/1742-6596/830/1/012066

In the study, several samples of VT6 titanium alloy (Ti-6Al-4V) were subjected to nitriding in a
non-self-maintained high-current arc discharge using PINK plasma source [6] with an incandescent
cathode installed in NNV-6.6-I1 installation [6] under the following conditions (Table 2):

Table 2. The treatment regimes on installation NNV-6.6-I1

Sample No. Temperature of
treatment [°C]
1 550
2 500
3 400
4 500
5 400
Treatment time [h] Composition of the
working fluid
3 60% Ar, 40% N2
1 20%Ar, 80%N2
1 20%Ar, 80%N2
3 100%N2
1 100%N2

The other samples were subjected to nitriding in a glow discharge on modernized ELU-5M
installation under the following conditions (Table 3):

Table 3. The treatment regimes on installation ELU-5M

Sample No. Temperature of
treatment [°C]
1 500
2 500
3 500
4 450
Treatment time [h] Composition of the
working fluid
3 85%Ar, 15%N2
3 85%Ar, 10%N2, 5%H2
1 85%Ar, 10%N2, 5%H2
1 85%Ar, 15%N2

The initial microhardness of the VT6 specimen surface subjected to quenching and aging was
330 kgf/mm2. The uniformity of microhardness distribution over the surface was determined by
measuring the microhardness diagonally at regular intervals with PMT-3M microhardness tester. The
depth of the modified layers was measured in cross sections at angle   6. A visual analysis of the
samples was used to investigate color uniformity against the initial state in order to identify possible
surface defects.

3. Results and discussion

The visual analysis showed that after ion nitriding in a non-self-maintained high-current arc discharge,
the samples appeared dull with a barely noticeable golden hue (Figure 1a). The samples treated in a
glow discharge acquired a golden hue with slight color heterogeneity (Figure 1b).
Surface microhardness tests showed that the hardness increased in all samples in the range of 348-
672 kgf/mm2. Surface microhardness for the samples treated with non-self-maintained arc discharge
and glow discharge is shown in Tables 4 and 5, respectively.

Table 4. Surface microhardness of the samples before and after ion nitriding
Microhardness before nitriding Microhardness after nitriding
Regime Hardening [%]
[kgf/mm2] [kgf/mm2]
Sample 1 672 104
Sample 2 528 60
Sample 3 330 373 13
Sample 4 493 49
Sample 5 348 6

2
5th International Congress on Energy Fluxes and Radiation Effects 2016 IOP Publishing
IOP Conf. Series: Journal of Physics: Conf. Series 1234567890
830 (2017) 012066 doi:10.1088/1742-6596/830/1/012066

Figure 1. General view of the samples before and after ion nitriding: а) samples treated in non-self-
maintained high-current discharge; b) samples treated in glow discharge.

Table 5. Surface microhardness of the samples before and after ion nitriding
Microhardness before nitriding Microhardness after nitriding
Regime Hardening [%]
[kgf/mm2] [kgf/mm2]
Sample 1 353 7
Sample 2 389 17.8
Sample 3 390 18
330
Sample 4 389 17.9
Sample 5 393 19
Sample 6 395 20

The increase of the microhardness for the samples treated in glow discharge is less significant as
compared to those treated in non-self-maintained arc discharge.
Changes in the profile along the microhardness depth of the samples processed in non-self-
maintained arc discharge are shown in Figure 2. The maximum surface microhardness of nitrided
samples of 672 kgf/mm2 was found in Sample 1. The minimum surface microhardness of nitrided
samples of 348 kgf/mm2 was found in Sample 5. Microhardness in Samples 2, 3 and 4 was 528, 373
and 493 kgf/mm2, respectively. Thus, the surface hardness and growth kinetics of the nitrided layers
were influenced by nitriding temperature at the greatest [7, 8]. The proportions of gas composition do
not have any significant impact on hardness and depth of the nitrided layers.
Hardness-depth changes of the samples after nitriding in a glow discharge are shown in Figure 3.
The hardness on the surfaces of all samples that were ion nitrided in glow discharge was about
390 kgf/mm2. The maximum depth of the hardened layer was found in Sample 2 and reached 17 μm.
The dependencies in Figure 3 show that the temperature change of 50 °C had no significant effect on
the surface hardness. Addition of hydrogen increases the depth of the modified layer. This is probably
due to the fact that hydrogen reacts with oxygen, which results in reduced oxygen concentration in the
surface layer and increased nitrogen adsorption sites on the surface. This in turn enhances nitrogen in
the sample volume and increases the hardness of the surface layer [6, 9].

3
5th International Congress on Energy Fluxes and Radiation Effects 2016 IOP Publishing
IOP Conf. Series: Journal of Physics: Conf. Series 1234567890
830 (2017) 012066 doi:10.1088/1742-6596/830/1/012066

Figure 2. Hardness-depth changes of samples after nitriding in a non-self-maintained arc discharge.

Figure 3. Hardness-depth changes of samples after nitriding in glow discharge.

4. Conclusion
Samples that were subjected to ion nitriding demonstrate sufficiently even microhardness distribution
on the surface and in the volume of the material without sharp transitions to the core.
The study showed that ion nitriding can be efficient in improving microhardness. The
microhardness and depth of a surface layer are greatly influenced by temperature.
Visual study showed that non-self-maintained high-current discharge nitriding leads to only slight
change of sample color. The samples processed in a glow discharge acquired a golden color due to the
appearance of titanium nitride on their surfaces.

4
5th International Congress on Energy Fluxes and Radiation Effects 2016 IOP Publishing
IOP Conf. Series: Journal of Physics: Conf. Series 1234567890
830 (2017) 012066 doi:10.1088/1742-6596/830/1/012066

References
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[2] Budilov V, Agzamov R and Ramazanov K 2007 Ion nitriding in a hollow cathode glow discharge
Metal Science and Heat Treatment 7 25
[3] Arzamasov B, Bratukhin A, Yeliseev Yu and Panajoti T 1999 Ion thermochemical treatment of
alloys (Moscow: Publishing House of Bauman Moscow State Technical University) p 400
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Interaction of Radiation with Solids 32
[6] Berlin Ye, Koval N and Seidman L 2012 Plasma thermochemical treatment of steel products
(Moscow: Tehnosfera) p 464
[7] Malinov L, Zecheva A and Sha V 2004 Dependence of microstructure and properties of
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Treatment 7 21
[8] Pogreluk I Nitriding of titanium alloys 2000 International conference 4 182
[9] Smoljakova M and Vershinin D 2011 Influence of gas mixture composition on titanium
structure and properties in low temperature nitriding Perspektivnye materialy 478