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AISI 5140 steel was plasma nitrided at various gas mixtures of nitrogen, hydrogen, and argon. It was found that the growth of compound layer can be controlled and the diffusion improved when the gas mixture includes H 2 gas. The amount of Ar in dual gas mixture must be at 20% minimum to obtain distinctive surface hardness and compound layer thickness.
AISI 5140 steel was plasma nitrided at various gas mixtures of nitrogen, hydrogen, and argon. It was found that the growth of compound layer can be controlled and the diffusion improved when the gas mixture includes H 2 gas. The amount of Ar in dual gas mixture must be at 20% minimum to obtain distinctive surface hardness and compound layer thickness.
AISI 5140 steel was plasma nitrided at various gas mixtures of nitrogen, hydrogen, and argon. It was found that the growth of compound layer can be controlled and the diffusion improved when the gas mixture includes H 2 gas. The amount of Ar in dual gas mixture must be at 20% minimum to obtain distinctive surface hardness and compound layer thickness.
Effects of various gas mixtures on plasma nitriding
behavior of AISI 5140 steel
Mehmet Karakan * , Akgun Alsaran, Ayhan C elik Department of Mechanical Engineering, Ataturk University, 25240 Erzurum, Turkey Received 21 October 2002; accepted 9 January 2003 Abstract AISI 5140 steel was plasma nitrided at various gas mixtures of nitrogen, hydrogen, and argon to investigate the actions of hydrogen and argon on plasma nitriding. The structural and mechanical properties of ion-nitrided AISI 5140 steel have been assessed by evaluating composition of phases, surface hardness, compound layer thickness, and case depth by using X-ray diffraction (XRD), microhardness tests, and scanning electron microscopy (SEM). It was found that the growth of compound layer can be controlled and the diffusion improved when the gas mixture includes H 2 gas. Additionally, it was determined that the amount of Ar in dual gas mixture must be at 20% minimum to obtain distinctive surface hardness and compound layer thickness. D 2003 Elsevier Science Inc. All rights reserved. Keywords: Ion nitriding; Gas mixture 1. Introduction Plasma nitriding is one of the most effective meth- ods for increasing wear resistance, fatigue strength, surface hardness, and for protecting the surface of materials from corrosion. This method has been com- monly used in industry for the last two decades [13]. Hydrogen and nitrogen gas mixtures are widely used to enhance the rate of nitriding in the plasma nitriding process [47]. To investigate alternatives to these gas mixtures, several studies on mixtures such as nitrogen and argon [811] and nitrogen and neon [12] were performed. However, it remains uncertain as to the importance of any gas additions other than nitrogen to plasma nitriding. For example, hydrogen enhances case depth and surface hardness by remov- ing surface oxide. The presence of argon improves surface hardness and it may be beneficial either alone or in combination with hydrogen. This study primarily deals with the effect of various gas mixtures on plasma nitriding to improve surface hardness, composition and thickness of com- pound layer, and case depth. Therefore, AISI 5140 low-alloy steel was plasma nitrided under various gas mixtures such as nitrogen + argon, nitrogen + hydro- gen, and nitrogen + hydrogen +argon, for a constant time of 4 h and a temperature of 450 C at a working pressure of 5 mbar. The structural and mechanical properties of plasma nitrided AISI 5140 are inves- tigated using X-ray diffraction (XRD), scanning elec- tron microscopy (SEM), optical microscopy, and microhardness tests. 2. Experimental procedure A schematic diagram of the ion nitriding system is shown in Fig. 1. It consists of a glass bell jar in which 1044-5803/03/$ see front matter D 2003 Elsevier Science Inc. All rights reserved. doi:10.1016/S1044-5803(03)00010-X * Corresponding author. Tel.: +90442-231-4860; fax: +90442-236-0957. E-mail address: mkarakan@atauni.edu.tr (M. Karakan). Materials Characterization 49 (2003) 241246 an insulated central electrode is situated, which holds specimens. A cylindrical anode at earth potential surrounds it. The cathode has a nest on which the specimen is located. A thermocouple is connected to the specimen through the cathode and the nest to monitor the specimen temperature. A series of experiments has been carried out to investigate the ion-nitriding response of AISI 5140 low alloy. The chemical composition of AISI 5140 steel is listed in Table 1. The specimens were nor- malized at 850 C for 30 min, and then cooled in air. After cleaning in alcohol, the specimens were placed into the plasma-nitriding chamber and the chamber was evacuated to 2.5 10 2 mbar. Prior to ion nitriding, the specimens were subjected to cleaning by hydrogen sputtering for 15 min under a voltage of 500 V and a pressure of 5 mbar to remove surface contaminates. After ion nitriding, the specimens had a thin compound layer that was removed before they were polished through 0.05 mm alumina. This was fol- lowed by metallographic examination and hardness testing. The case depth and the surface hardness were measured by using a Buchler 16004980T at a load of 50 gf and a dwell time of 15 s. The maximum surface hardness at 25 mm depth was chosen for comparison so that any possible effects from a compound layer would be negligible. A Rigaku diffractometer was used for XRD analysis. The X- ray diffractomer was operated at 30 kV and 30 mA with CuK a radiation. The compound layer thickness was also investigated by using SEM. 3. Results and discussion Figs. 24 show XRD results for ion-nitrided AISI 5140 low-alloy steel as a function of various gas mixtures. As seen in the figures, polyphase (g and e) iron nitrides occur on the surface of low-alloy steel. Fig. 1. The schematic diagram of ion nitriding system. Table 1 Chemical composition of AISI 5140 low-alloy steel (%) Element (wt.%) C Mn Si Cr Ni Mo V S Cu P 0.426 0.77 0.287 0.845 0.134 0.054 0.0287 0.064 0.0154 0.019 M. Karakan et al. / Materials Characterization 49 (2003) 241246 242 Fig. 2 shows the XRD results of the ion-nitrided specimens at gas mixtures of 10% H 2 + 90% N 2 and 10% Ar + 90% N 2 . a-Fe phase was clearly observed with Ar N 2 mixtures, because the intensity of e phase was not high. A thin compound layer occurred at a gas mixture of 10% Ar + 90% N 2 . This is because the amount of Ar in the gas mixture was insufficient to create diffusion. The experiments showed that the amount of Ar in dual gas mixture should be a minimum of 20% to form a compound layer and to increase surface hardness. However, the compound layer was observed with a 10% H 2 gas mixture because the ionization energy of H 2 is lower than that of Ar. Fig. 3 illustrates the XRDresults of the ion-nitrided specimens for gas mixtures of 90% H 2 + 10% N 2 and 90% Ar + 10% N 2 . While the intensity of e decreased Fig. 2. XRD patterns of plasma nitrided AISI 5140 steel for gas mixtures of 10% H 2 +90% N 2 (a) and 10% Ar + 90% N 2 (b). Fig. 3. XRD patterns of plasma nitrided AISI 5140 steel for gas mixtures of 90% Ar + 10% N 2 (a) and 90% H 2 + 10% N 2 (b). M. Karakan et al. / Materials Characterization 49 (2003) 241246 243 for Ar N 2 mixtures, the intensity of g increased for H 2 N 2 mixtures. The 2q angles of phases were higher at large angles when the amount of N 2 in the tripartite gas mixture was high (Fig. 4). When Ar gas amount in the mixture was increased, the intensity of the phases occurring compound layer increased. The compound layer thickness, case depth, and surface hardness of the ion-nitrided AISI 5140 steel depending on the gas mixtures are given in Table 2. The minimum case depth, compound layer thickness, and surface hardness were obtained at the gas mix- tures of 10% Ar + 90% N 2 and at 450 C for 4 h. These results showed that ion nitriding did not completely occur. When these results are considered together with XRD results (Fig. 2), it can be con- cluded that the compound layer (Fe 23 N and Fe 4 N) was not observed. The compound layer provides materials with good physical properties against wear and corrosion. However, the case is very hard and brittle, and for an application subjected to stresses, the compound layer should be thin or absent. Addi- tion of H 2 gas into the gas mixture prevented from undesirable effects by stopping the rapid growth of compound layer. The surface hardness of ion-nitrided AISI 5140 increased up to two to three times for gas mixtures including H 2 . Furthermore, the maximum case depth was also observed for the 10% N 2 +90% H 2 gas mixture. The hardness profiles and SEM photograph of microhardness indentations of the ion-nitrided specimens are given in Fig. 5. The increase in indent dimension is a sign of decreasing hardness. In addi- tion, the hardness decreases from surface to core because the concentration of metal nitrides decreased toward the core. Fig. 4. XRD patterns of plasma nitrided AISI 5140 steel for gas mixtures of 10% Ar +10% H 2 + 80% N 2 (a), 80% Ar + 10% H 2 +10% N 2 (b), and 10% Ar + 80% H 2 +10% N 2 (c). Table 2 The change of the compound layer thickness, the case depth, and surface hardness with the gas mixtures Plasma nitriding parameters Compound Case depth Surface Time (h) Temperature (C) Gas mixture layer (mm) (mm) hardness (HV) 4 450 90% N 2 + 10% H 2 45 160190 540550 4 450 10% N 2 + 90% H 2 22.5 210240 760770 4 450 90% N 2 + 10% Ar 3565 290300 4 450 10% N 2 + 90% Ar 810 6090 470480 4 450 80% N 2 + 10% H 2 + 10% Ar 56 110140 470480 4 450 10% N 2 + 10% H 2 + 80% Ar 5.56.5 90120 500510 4 450 10% N 2 + 80% H 2 + 10% Ar 23 185215 700710 M. Karakan et al. / Materials Characterization 49 (2003) 241246 244 Fig. 6 shows SEM micrographs of ion-nitrided AISI 5140 at different gas mixtures. The thickness of the compound layer is 22.5 mm at 90% H 2 (Fig. 6a) and 9 mm at 90% Ar (Fig. 6b). A lot of voids were observed in the compound layer, as seen in Fig. 6b. The porous shows one of the undesirable features of the compound layer. 4. Conclusions The following main conclusions can be derived from the above results and discussions:
The hardness profiles of the ion-nitrided speci-
mens exhibited maximum hardness in the range of 760770 HV 0.05 for the 10% N 2 + 90% H 2 gas mixture. It was observed that the compound layer thickness and case depth can be controlled and the good surface hardness can be obtained with an increase in the amount of H 2 gas in the gas mixture.
The compound layer of the ion-nitrided speci-
mens consists of e phase and g phase. The intensity of e phase is not high for the 10% N 2 + 90% Ar gas mixtures. Ar in the gas mixture causes the rapid growth of compound layer but the case depth is not as deep with Ar in the gas mixtures.
The amount of Ar in dual gas mixture must be a
minimum of 20% to obtain distinctive surface hardness and compound layer thickness. Fig. 5. (a) The hardness profiles of ion-nitrided specimens as gas mixtures, (b) SEM micrograph of specimen ion nitrided at gas mixtures of 80% N 2 + 10% H 2 + 10% Ar. Fig. 6. SEM micrographs of plasma nitrided AISI 5140 for 90% H 2 + 10% N 2 (a) and 90% Ar + 10% N 2 (b). M. Karakan et al. / Materials Characterization 49 (2003) 241246 245 References [1] Inal OT, Robino CV. Structural characterization of some ion-nitrided steels. Thin Solid Film 1982;95: 195207. [2] Karamis B. An investigation of the properties and wear behavior of plasma nitrided hot-working steel (H13). Wear 1991;150:33142. [3] Alsaran A, Celik A. The structural characterization of ion nitrided AISI 5140 low alloy steel. Mater Charact 2001;47(34):20713. [4] Edenhofer B. Physical and metallurgical aspect of ion- itriding. Heat Treat Met 1974;2:5967. [5] Sun Y, Bell T. Plasma surface engineering of low alloy steel. Mater Sci Eng, A 1991;140:41934. [6] Alsaran A, Karakan M, C elik A. The investigation of mechanical properties of ion-nitrided AISI 5140 low alloy steel. Mater Charact 2002;48(4):3237. [7] Alsaran A, C elik A, C elik C. Determination of opti- mum conditions for ion nitriding of AISI 5140 steel. Surf Coat Technol 2002;160(23):21926. [8] Hudis M. Study of ion-nitriding. J Appl Phys 1973; 44(A):148996. [9] Inal OT, O
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