Plasma nitriding of AISI 52100 ball bearing steel and effect of heat treatment on nitrided layer

In this paper an effort has been made to plasma nitride the ball bearing steel AISI 52100. The difficulty with this specific steel is that its tempering temperature (~170–200°C) is much lower than the standard processing temperature (~460–580°C) needed for the plasma nitriding treatment. To understand the mechanism, effect of heat treatment on the nitrided layer steel is investigated. Experiments are performed on three different types of ball bearing races i.e. annealed, quenched and quench-tempered samples. Different gas compositions and process temperatures are maintained while nitriding these samples. In the quenched and quench-tempered samples, the surface hardness has decreased after plasma nitriding process. Plasma nitriding of annealed sample with argon and nitrogen gas mixture gives higher hardness in comparison to the hydrogen–nitrogen gas mixture. It is reported that the later heat treatment of the plasma nitrided annealed sample has shown improvement in the hardness of this steel. X-ray diffraction analysis shows that the dominant phases in the plasma nitrided annealed sample are ε (Fe_2 − 3N) and γ (Fe₄N), whereas in the plasma nitrided annealed sample with later heat treatment only α-Fe peak occurs.     

Structure and properties of gas-nitrided nanostructured FeAlMnC alloy

The as-quenched Fe–9Al–28Mn–1.8C (in wt.%) alloy was directly gas-nitrided at 500 °C for 8 h, resulting in a ∼30 μm-thick nitrided layer. The nitrided layer consists predominantly of nano-crystalline AlN with a small amount of Fe₄N. The nitrogen concentration at surface was extremely high up to ∼17 wt.% (∼41 at.%). Consequently, the surface microhardness (1700 Hv), substrate hardness (550 Hv), ductility (33.2%) and corrosion resistance in 3.5% NaCl solution of the present gas-nitrided alloy are far superior to those obtained previously for the optimally gas-nitrided or plasma-nitrided high-strength alloy steels, as well as martensitic and precipitation-hardening stainless steels. Moreover, it is very novel that the nitrided layer almost remained coherent and adhered well with the matrix after tensile test. Additionally, the present gas nitriding appeared to overcome the edge effects commonly encountered in plasma nitriding treatments for metals.     

Mössbauer spectroscopy study on the corrosion resistance of plasma nitrided ASTM F138 stainless steel in chloride solution

Plasma nitriding of ASTM F138 stainless steel samples has been carried out using dc glow discharge under 80% H₂–20% N₂ gas mixture, at 673 K, and 2, 4, and 7 h time intervals, in order to investigate the influence of treatment time on the microstructure and the corrosion resistance properties. The samples were characterized by scanning electron microscopy, glancing angle X-ray diffraction and conversion electron Mössbauer spectroscopy, besides electrochemical tests in NaCl aerated solution. A modified layer of about 6 μm was observed for all the nitrided samples, independent of nitriding time. The X-ray diffraction analysis shows broad γ_N phase peaks, signifying a great degree of nitrogen supersaturation. Besides γ_N, the Mössbauer spectroscopy results indicated the occurrence of γ′ and ε phases, as well as some other less important phases. Corrosion measurements demonstrate that the plasma nitriding time affects the corrosion resistance and the best performance is reached at 4 h treatment. It seems that the ε/γ′ fraction ratio plays an important role on the resistance corrosion. Additionally, the Mössbauer spectroscopy was decisive in this study, since it was able to identify and quantify the iron phases that influence the corrosion resistance of plasma nitrided ASTM F138 samples.     

Corrosion behavior of ion nitrided AISI 316L stainless steel

In the present work the corrosion susceptibility of ion nitrided AISI 316L stainless steel was investigated for two different nitriding times and compared with the corrosion susceptibility of the untreated material. Plasma nitriding for short times (30 min) produced the “S” phase or expanded austenite (γ_N), with a thickness of ∼ 5 μm and a micro-hardness of 1300-1400 HV_0.025 (6.5 times higher than the untreated material). Plasma nitriding for long times (6 h) resulted in the precipitation of iron and chromium nitrides.To evaluate the corrosion resistance of both untreated and nitrided samples, anodic potentiodynamic polarization curves and immersion tests were performed in 1 M NaCl at room temperature. It was found that the corrosion resistance depends on the nitriding time. Samples nitrided for half an hour developed a much better corrosion resistance - close to that observed in the untreated samples - than those nitrided for 6 h. Samples nitrided for half an hour showed high roughness probably due to the presence of sliding bands developed in the expanded austenite phase. These sliding bands provide appropriate sites for the developing of the corrosion process. This would explain the results obtained in the corrosion tests. Samples ion nitrided for 6 h showed a severe and massive surface damage due to corrosion.Ion nitriding of AISI 316L stainless steel for short periods of time (30 min in the present case) may be an interesting surface treatment process that efficiently improves the surface hardness of the steel with some reduction in its corrosion resistance.     

Surface characterization of multiple coated H11 hot work tool steel by plasma nitriding and hard chromium electroplating processes

Formation of multi-layer coating by plasma nitriding and hard chromium electroplating on the surface of H11 hot work tool steel was investigated. Specimens were coated via a triple process containing plasma nitriding, hard chromium electroplating and plasma nitriding. Surface composition has been studied by X-ray diffraction analysis. The surface morphology and elemental analysis was examined by using scanning electron microscopy. Wear tests were conducted by the use of pin-on-disk method, a cemented tungsten carbide pin and 1000 gF load. Polarization corrosion tests were carried out in distilled water solution containing 3% NaCl. The improvement in hardness distribution after third step is discussed in considering the forward and backward diffusion of nitrogen in the chromium interlayer. Also, the formed phases in the hybrid coating were determined to be CrN + Cr₂N + Cr + Fe_2-3N + Fe₄N. Wear results showed that although the multi-layer coated specimens have higher wear resistance in comparison with the reference specimen, their wear resistance is less than that of two and one layer coated specimens due to micro-ploughing and removal of hard surface nitrides from the surface. By increasing the third step time and temperature, the wear resistance of specimens increases due to higher diffusion of nitrogen in the chromium layer. But polarization results showed that triple coated specimens have the lowest corrosion rate.     

Effects of DC plasma nitriding parameters on microstructure and properties of 304L stainless steel

A wear-resistant nitrided layer was formed on a 304L austenitic stainless steel substrate by DC plasma nitriding. Effects of DC plasma nitriding parameters on the structural phases, micro-hardness and dry-sliding wear behavior of the nitrided layer were investigated by optical microscopy, X-ray diffraction, scanning electron microscopy, micro-hardness testing and ring-on-block wear testing. The results show that the highest surface hardness over a case depth of about 10 µm is obtained after nitriding at 460 °C. XRD indicated a single expanded austenite phase and a single CrN nitride phase were formed at 350 °C and 480 °C, respectively. In addition, the S-phase layers formed on the samples provided the best dry-sliding wear resistance under the ring-on-block contact configuration test.     

Sol-gel derived TiO2 coating on plasma nitrided 316L stainless steel

Titania film is coated on plasma nitrided 316L stainless steel by sol-gel method. Crystallization of titania as well as N loss and formation of Fe₂O₃ occurs during the annealing heat treatment. The titania film has short cracks within the grooves of plasma etched grain boundaries. With the increase of annealing temperature and duration, surface hardness of the samples is increased, but the toughness is decreased due to oxidization of the surface layer. The coating sample heat treated at 350 °C for 10 min and 450 °C for 10 min has better corrosion resistance than the nitrided stainless steel tested by the potentiodynamic polarization in 0.9% NaCl solution. Water contact angle of the titania film on the rough nitrided steel substrate decreases with UV irradiation treatment, reaching 17° after 3 h treatment.     

Effect of high temperature post-oxidizing on tribological and corrosion behavior of plasma nitrided AISI 316 austenitic stainless steel

In this research, the microstructure, tribological and corrosion properties of plasma nitrided-oxidized AISI 316 austenitic stainless steel at high oxidation temperature were studied and compared with conventional plasma nitride. The structural, tribological and corrosion properties were analyzed using XRD, SEM, microhardness testing, pin-on-disk tribotesting and electrochemical polarization. Plasma nitriding was conducted for 5 h at 450 °C with gas mixture of N₂/H₂ = 1/3 to produce the S-phase. The nitrided samples were post-oxidized at 500 °C with gas mixture of O₂/H₂ = 1/5 for 15, 30 and 60 min. X-ray diffraction confirmed the development of CrN, ? and γ′ nitride phases and magnetite (Fe₃O₄) oxide phase under plasma nitriding-oxidizing process. In addition, it was found that oxidation treatment after plasma nitriding provides an important improvement in the friction coefficient and the corrosion resistance. The optimized wear and corrosion resistance of post-oxidized samples were obtained after 15 min of oxidation.     

Characteristics of the nitrided layer formed on AISI 304 austenitic stainless steel by high temperature nitriding assisted hollow cathode discharge

A series of experiments have been conducted on AISI 304 stainless steel using a hollow cathode discharge assisted plasma nitriding apparatus. Specimens were nitrided at high temperatures (520–560 °C) in order to produce nitrogen expanded austenite phase within a short time. The nitrided specimen was characterized by scanning electron microscopy, X-ray diffraction, X-ray photoelectron spectroscopy, potentiodynamic polarization and microhardness tester. The corrosion properties of nitrided samples were evaluated using anodic polarization tests in 3.5% NaCl solution. The nitrided layer was shown to consist of nitrogen expanded austenite and possibly a small amount of CrN precipitates and iron nitrides. The results indicated that rapid nitriding assisted hollow cathode discharge not only increased the surface hardness but also improved the corrosion resistance of the untreated substrate.     

Effect of post-oxidizing temperature on tribological and corrosion behavior of plasma nitrided austenitic stainless steel

In this study, the effect of temperature of post-oxidation process on tribological and corrosion behavior of AISI 316 plasma nitrided stainless steel has been studied. Plasma nitriding was carried out at 450 °C for 5 h with gas mixture of N₂/H₂ = 1/3. The plasma nitrided samples were post-oxidized for 1 h with gas mixture of O₂/H₂ = 1/5 at different temperature of 400, 450 and 500 °C. The structural, tribological and corrosion properties were analyzed using XRD, SEM, microhardness testing, pin-on-disk tribotesting and electrochemical polarization. The results indicated that the nitride layer was composed of S-phase. The amount of S-phase decreased as the treatment temperature rose from 400 °C to 500 °C. In addition, it was found that oxidation treatment reduces wear resistance of plasma nitrided sample. It was demonstrated that the corrosion characteristics of the nitrided sample were further improved by post-oxidation treatment. The difference in corrosion resistance is mainly attributed to the thickness of the oxide top layer, which is governed by the post-oxidizing temperature.     

Comparison of ferritic and austenitic plasma nitriding and nitrocarburizing behavior of AISI 4140 low alloy steel

This paper compares the ferritic and austenitic plasma nitriding and nitrocarburizing behavior of AISI 4140 low alloy steel carried out to improve the surface corrosion resistance. The gas composition for plasma nitriding was 85% N₂–15% H₂ and that for plasma nitrocarburizing was 85% N₂–12% H₂–3% CO₂. Both treatments were performed for 5 h, for different process temperatures of 570 and 620 °C for ferritic and austenitic plasma treatment, respectively. Optical microscopy, X-ray diffraction and potentiodynamic polarization technique in 3.5% NaCl solution, were used to study the treated surfaces. The results of X-ray analysis revealed that with increasing the treatment temperature from 570 to 620 °C for both treatments, the amount of ε phase decreased and γ′ phase increased. Nitrocarburizing treatment resulted in formation of a more amount of ε phase with respect to nitriding treatment. However, the highest amount of ε phase was observed in the ferritic nitrocarburized sample at 570 °C. The sample nitrided at 620 °C exhibited the thickest layer. The potentiodynamic polarization results revealed that after plasma nitriding and nitrocarburizing at 570 °C, corrosion potential increased with respect to the untreated sample due to the noble nitride and carbonitride phases formed on the surface. After increasing the treatment temperature from 570 to 620 °C, corrosion potential decreased due to the less ε phase development in the compound layer and more porous compound layer formed at 620 °C with respect to the treated samples at 570 °C.     

Corrosion behavior of nitride layer obtained on AISI 316L stainless steel via simple direct nitridation route at low temperature

Newly developed low-temperature nitride synthesis route was used to introduce interstitial nitrogen into the passive layer of as-received and as-polished 316L stainless steel. The new thermochemical route is based on treating the stainless steel samples in potassium nitrate melt in an ultra pure nitrogen atmosphere at 450 °C. Electrochemical impedance spectroscopy (EIS) and dc polarization measurements have been used to evaluate the nitride layer performance in 3.5% NaCl solution. Results showed a marked increase in the corrosion resistance of nitrided stainless steel even after maintaining two weeks in NaCl solution. The effect of the treatment temperature was also studied. Data showed that the as-polished samples nitrided at 450 °C have the highest corrosion resistance. The polarization resistance (R_p) for the as-polished and as-received blank stainless steel samples was estimated by EIS were approximately 4.0 × 10⁴ Ω cm² and 2.0 × 10⁴ Ω cm², respectively. The R_p increased by a factor of 2.5–5 for the nitrided samples. Increasing the nitriding temperature from 450 to 600 °C affects negatively the corrosion resistance of stainless steel in NaCl solution. The R_p of the samples nitrided at 600 °C decreased sharply being almost 1/30 of the R_p of the samples nitrided at 450 °C. Linear polarization measurements showed that the lowest corrosion rates and highest polarization resistances obtained from the as-polished nitrided samples at 450 °C. It has been found from the potentiodynamic measurements that the E_corr of the as-polished nitrided samples at 450 °C is nobler than that measured from the other groups. The surface morphology was analysed by optical microscope and SEM-EDS under different nitriding conditions.     

Research on new rapid and deep plasma nitriding techniques of AISI 420 martensitic stainless steel

Cyclic plasma oxynitriding and cyclic plasma nitriding catalyzed by rare earth La of AISI 420 martensitic stainless steel were performed and compared with conventional plasma nitriding. The nitrided layers were investigated by means of an optical microscope, microhardness tester, Auger electron spectroscopy (AES), X-ray diffraction (XRD), wear machine, scanning electron microscope (SEM) and energy dispersive spectroscopy (EDS). The results show that the wear resistance of AISI 420 martensitic stainless steel is improved significantly by the two new rapid and deep plasma nitriding techniques. The new techniques increase the surface hardness of the nitrided layers and make the microhardness profiles gentler, which are consistent with the nitrogen concentration depth profiles. Meanwhile, the nitrided effect improves with increasing cycles. It was also found that the optimum phase compositions of nitrided layers with more γ′ phases and less ? phases for long-term service conditions can be obtained by the two new techniques, which is in agreement with the microstructure. In addition, traces of Fe₃O₄ were found in the cyclic plasma oxynitrided sample. Combining the SEM and EDS analysis indicated the existence of La in the nitrided layer of the sample under cyclic plasma nitriding catalyzed by rare earth La.     

Kinetics and wear behaviour of M50NiL steel plasma nitrided at low temperature

The quenched M50NiL steel was plasma nitrided at 460°C for different time to investigate the effects of the duration time on the microstructure, microhardness and wear resistance of the nitrided layers. The results show that the plasma nitrided layer depth increases with increasing nitriding time. The plasma nitrided layer includes only the diffusion layer without compound layer. The main phases in the nitrided surface layer are nitrogen expended α′-Fe and γ′-Fe₄N. The microstructure of the nitrided layer is refined. The wear resistance of the nitrided samples can be improved significantly by plasma nitriding. The sample nitrided for 4?h possesses the highest wear resistance, due to its relatively smooth surface and ultra-fine grains in the nitrided layer.     

Struktur und Eigenschaften nichtrostender Stähle nach einer Plasmaimmersionsionenimplantation und einer Plasmanitrierung

Structure and properties of stainless steels after plasma immersion ion implantation and plasma nitriding Stainless steels can be nitrided at temperatures ≤ 400 °C to increase their hardness and wear resistance without a decreasing of their excellent corrosion resistance. Structure and properties of the surface layers produced by plasma nitriding and plasma immersion ion implantation in this temperature range were tested. There are negligible differences in the structure of the produced surface layers in spite of different interaction principles of the used technologies. However there are clear differences between the case of different steels. The case of ferritic chromium steels mainly consists of ε-nitride. Whereas the cases of austenitic and ferritic austenitic steels are characterized by expanded austenite. The corrosion resistance of the steels is reduced by nitriding only, if evident CrN-formation occurs.     

Effect of annealing on corrosion behaviour of nitrogen S phase in austenitic stainless steel

Abstract

The corrosion behaviour of both as nitrided and nitrided then annealed 316 austenitic stainless steel has been investigated. Results show that low temperature plasma nitriding can, to some extent, enhance the corrosion resistance of 316 steel, and this can be attributed to the high nitrogen content in the nitrogen S phase layer. However, when annealed at certain conditions, the corrosion resistance of the S phase layer would be impaired. This is mainly because thermodynamically the S phase is a metastable phase, which will decompose into stable chromium nitride and the alpha phase if the kinetic conditions (temperature and time) are favourable. Clearly, the improved corrosion resistance conferred by low temperature plasma nitriding can be retained provided the S phase layer remains untransformed under service conditions.     

Duplex treatment of 304 AISI stainless steel using rf plasma nitriding and carbonitriding

Surface of 304 AISI austenitic stainless steel has been modified using duplex treatment technique of nitriding and carbonitriding. A thick modified nitrided layer, of approximately 20 µm, has been achieved when rf inductively coupled plasma was adjusted at 450 W for processing time of only 10 min. After performing the nitrided layer, the nitrided samples were carbonitrided using the same technique at different acetylene partial pressure ratios ranges from 10% to 70%, the balance was pure nitrogen. Different amount of nitrogen and carbon species are diffused underneath the surface through the nitrided layer during carbonitriding process and are found to be gas composition dependent. The treated samples were characterized by glow discharge optical spectroscopy, X-ray diffractometry, scanning electron microscopy and Vickers microhardness tester. The microstructure of the duplex treated layer indicates the formation of γ?-Fe₄N, Fe₃C, CrN and nitrogen-expanded austenite (γ_N). The thickness of the duplex treated layer increases with increasing the acetylene partial pressure ratio. The surface microhardness of duplex treated samples has been found to be gas composition dependent and increased by 1.29 fold in comparison to the nitrided sample.     

The study of tribological and corrosion behavior of plasma nitrided 34CrNiMo6 steel under hot and cold wall conditions

This paper reports on a comparative study of tribological and corrosion behavior of plasma nitrided 34CrNiMo6 low alloy steel under modern hot wall condition and conventional cold wall condition. Plasma nitriding was carried out at 500 °C and 550 °C with a 25% N₂ + 75% H₂ gas mixture for 8 h. The wall temperature of the chamber in hot wall condition was set to 400 °C. The treated specimens were characterized by using scanning electron microscopy (SEM), X-ray diffraction (XRD), microhardness and surface roughness techniques. The wear test was performed by pin-on-disc method. Potentiodynamic polarization and electrochemical impedance spectroscopy (EIS) tests were also used to evaluate the corrosion resistance of the samples. The results demonstrated that in both nitriding conditions, wear and corrosion resistance of the treated samples decrease with increasing temperature from 500 °C to 550 °C. Moreover, nitriding under hot wall condition at the same temperature provided slightly better tribological and corrosion behavior in comparison with cold wall condition. In consequence, the lowest friction coefficient, and highest wear and corrosion resistance were found on the sample treated under hot wall condition at 500 °C, which had the maximum surface hardness and ε-Fe_2–3N phase.     

Microstructure and mechanical properties of the modified layer obtained by low temperature plasma nitriding of nanocrystallized 18Ni maraging steel

In the present study, low temperature plasma nitriding of nanocrystallized 18Ni maraging steel has been carried out at 360 °C from 1 to 24 h in a mixed gas of 25%N₂ + 75%H₂. The surface phase constitutions and microstructures of the nitrided layer have been investigated by X-ray diffraction analysis, transmission electron microscopy and optical microscopy. Nanoindentation and microhardness tests have been performed to determine the surface hardness and the hardness profile in the nitrided layer. The plasticity of the nitrided surface has been analyzed based on the nanoindentation results. The results show that at the initial stage of nitriding, the surface phase consists of a solid solution of nitrogen in α-Fe, and nanoscale nitrides and aging phase are formed with increasing of treatment time. The surfaces nitrided for 8 and 16 h possess the highest hardness. The plasticity factor calculations suggest that the nitrided surfaces have a good wear resistance and possess excellent plasticity.     

Liquid metal induced embrittlement of a nitrided clutch shell of a motorbike

The failure mechanism of a clutch shell made from SPCC nitrided steel was analyzed. The component sustained multiple brittle fractures during assembly. Under SEM examination, the fracture surface was found to have facet and cleavage grain appearance. It was predicted that the cleavage fractures started from sites of intergranular fractures. XRD results showed that the nitriding layer contained Fe₃N (60 wt.%) and Fe₄N (40 wt.%). It is noted that Fe₃N is more brittle than Fe₄N. An impact test was carried out to compare the impact resistance of the failed and normal components. EDS analysis was also carried out, and it was found that the fracture surface contained zinc, which was not an element specified for the SPCC steel or the nitriding salt. As the salt bath nitriding process operated at a temperature higher than the melting point of zinc, failure was most likely due to liquid metal zinc induced embrittlement, as a result of localized salt bath material contamination with zinc.