Improvement of corrosion and wear resistances of AISI 420 martensitic stainless steel using plasma nitriding at low temperature

The influence of low temperature plasma nitriding on the wear and corrosion resistance of AISI 420 martensitic stainless steel was investigated. Plasma nitriding experiments were carried out with DC-pulsed plasma in 25% N₂ + 75% H₂ atmosphere at 350 °C, 450 °C and 550 °C for 15 h. The composition, microstructure and hardness of the nitrided samples were examined. The wear resistances of plasma nitrided samples were determined with a ball-on-disc wear tester. The corrosion behaviors of plasma nitrided AISI420 stainless steel were evaluated using anodic polarization tests and salt fog spray tests in the simulated industrial environment.The results show that plasma nitriding produces a relatively thick nitrided layer consisting of a compound layer and an adjacent nitrogen diffusion layer on the AISI 420 stainless steel surface. Plasma nitriding not only increases the surface hardness but also improves the wear resistance of the martensitic stainless steel. Furthermore, the anti-wear property of the steel nitrided at 350 °C is much more excellent than that at 550 °C. In addition, the corrosion resistance of AISI420 martensitic stainless steel is considerably improved by 350 °C low temperature plasma nitriding. The improved corrosion resistance is considered to be related to the combined effect of the solid solution of Cr and the high chemical stable phases of ?-Fe₃N and α_N formed on the martensitic stainless steel surface during 350 °C low temperature plasma nitriding. However, plasma nitriding carried out at 450 °C or 550 °C reduces the corrosion resistance of samples, because of the formation of CrN and leading to the depletion of Cr in the solid solution phase of the nitrided layer.     

Corrosion properties of active screen plasma nitrided 316 austenitic stainless steel

AISI 316 austenitic stainless steel has been plasma nitrided using the active screen plasma nitriding (ASPN) technique. Corrosion properties of the untreated and AS plasma nitrided 316 steel have been evaluated using various techniques, including qualitative evaluation after etching in 50%HCl + 25%HNO₃ + 25%H₂O, weight loss measurement after immersion in 10% HCl, and anodic polarisation tests in 3.5% NaCl solution. The results showed that the untreated 316 stainless steel suffered severe localised pitting and crevice corrosion under the testing conditions. AS plasma nitriding at low temperature (420 °C) produced a single phase nitrided layer of nitrogen expanded austenite (S-phase), which considerably improved the corrosion properties of the 316 austenitic stainless steel. In contrast, AS plasma nitriding at a high temperature (500 °C) resulted in chromium nitride precipitation so that the bulk of the nitrided case had very poor corrosion resistance. However, a thin deposition layer on top of the nitrided case, which seems to be unique to AS plasma nitriding, could have alleviated the corrosion attack of the higher temperature nitrided 316 steel.     

Plasma nitriding of AISI 304 austenitic stainless steel with pre-shot peening

AISI 304 austenitic stainless steel was plasma nitrided at the temperature ranging from 410 to 520 °C with pre-shot peening. The structural phases, micro-hardness and electrochemical behavior of the nitrided layer were investigated by optical microscopy, X-ray diffraction, micro-hardness testing and anodic polarization testing. The effects of shot peening on the nitride formation, nitride layer growth and corrosion properties were discussed. The results showed that shot peening enhanced the nitrogen diffusion rate and led to a twice thicker nitrided layer than the un-shot peening samples under the same plasma nitriding conditions (410 °C, 4 h). The nitrided layer was composed of single nitrogen expanded austenite (S-phase) when nitriding below 480 °C, which had combined improvement in hardness and corrosion resistance.     

Corrosion resistance properties of glow-discharge nitrided AISI 316L austenitic stainless steel in NaCl solutions

Glow-discharge nitriding treatments can modify the hardness and the corrosion resistance properties of austenitic stainless steels. The modified layer characteristics mainly depend on the treatment temperature. In the present paper the results relative to glow-discharge nitriding treatments carried out on AISI 316L austenitic stainless steel samples at temperatures ranging from 673 to 773 K are reported. Treated and untreated samples were characterized by means of microstructural and morphological analysis, surface microhardness measurements and corrosion tests in NaCl solutions. The electrochemical characterization was carried out by means of linear polarizations, free corrosion potential-time curves and prolonged crevice corrosion tests. Nitriding treatments performed at higher temperatures (>723 K) can largely increase the surface hardness of AISI 316L stainless steel samples, but decrease the corrosion resistance properties due to the CrN precipitation. Nevertheless nitriding treatments performed at lower temperatures (?723 K) avoid a large CrN precipitation and allow to produce modified layers essentially composed by a nitrogen super-saturated austenitic metastable phase (S-phase) that shows high hardness and very high pitting and crevice corrosion resistance; at the same polarization potentials the anodic current density values are reduced up to three orders of magnitude in comparison with untreated samples and no crevice corrosion event can be detected after 60 days of immersion in 10% NaCl solution at 328 K.     

Plasma nitriding of plastic mold steel to increase wear- and corrosion properties

In this study, the wear- and corrosion resistance of the layers formed on the surface of a precipitation hardenable plastic mold steel (NAK55) by plasma nitriding were investigated. Plasma nitriding experiments were carried out at an industrial nitriding facility in an atmosphere of 25% N₂ + 75% H₂ at 475 °C, 500 °C, and 525 °C for 10 h. The microstructures of the nitrided layers were examined, and various phases present were determined by X-ray diffraction. Wear tests were carried out on a block-on-ring wear tester under unlubricated conditions. The corrosion behaviors were evaluated using anodic polarization tests in 3.5% NaCl solution.The findings had shown that plasma nitriding does not cause the core to soften by overaging. Nitriding and aging could be achieved simultaneously in the same treatment cycle. Plasma nitriding of NAK55 mold steel produced a nitrided layer consisted of a compound layer rich in ε-nitride and an adjacent nitrogen diffusion layer on the steel surface. Increasing the nitriding temperature could bring about increase in the thickness of the nitrided layer and the nitride volume fraction. Plasma nitriding improved not only surface hardness but also wear resistance. The anti-wear property of the steel was found to relate to the increase in the thickness of the diffusion layer. Corrosion study revealed that plasma nitriding significantly improved corrosion resistance in terms of corrosion potential and corrosion rate. Improvement in corrosion resistance was found to be directly related to the increase in the nitride volume fraction at the steel surface.     

The corrosion and corrosion-wear behaviour of plasma nitrided 17-4PH precipitation hardening stainless steel

Plasma surface nitriding of 17-4 PH martensitic precipitation hardening stainless steels was conducted at 350 °C, 420 °C and 500 °C for 10 h using a DC plasma nitriding unit, and the surface properties of the plasma surface engineered samples were systematically evaluated. Experimental results have shown that the surface properties of the plasma nitrided layers in terms of hardness, wear resistance, corrosion behaviour and corrosion-wear resistance are highly process condition dependent, and it is feasible to provide considerable improvement in wear, corrosion and corrosion-wear resistance of 17-4PH steel using optimised plasma treatment conditions. All three treatments can effectively improve the surface hardness and the sliding wear resistance under unlubricated conditions; high temperature (420 °C and 500 °C) treated materials revealed improved corrosion and corrosion-wear properties due to the formation of surface compound layers.     

Plasma nitriding of 90CrMoV8 tool steel for the enhancement of hardness and corrosion resistance

The aim of the study is to apply a plasma nitriding process to the 90CrMoV8 steel commonly employed in wood machining, and to determine its efficiency to improve both mechanical and electrochemical properties of the surface. Treatments were performed at a constant N₂:H₂ gas mixture and by varying the temperature and process duration. The structural and morphological properties of nitrided layers were characterized by X-ray diffraction (XRD) and scanning electron microscopy (SEM) coupled with EDS microanalyses. Surface hardening and hardness profiles were evaluated by micro hardness measurements. To simulate the wood machining conditions, electrochemical tests were carried out with an oak wood electrolyte with the purpose of understanding the effects of the nitriding treatment on the corrosion resistance of the tool in operation.X-ray diffraction analyses revealed the presence of both γ′ (Fe₄N) and ε (Fe_2-3N) nitrides with a predominance of the ε phase. Moreover, α-Fe (110), γ′ and ε diffraction peaks were shifted to lower angles suggesting the development of compressive stresses in the post nitrided steel. As a result, it was shown that nitriding allowed a significant hardening of steel with hardness values higher than 1200 HV. The diffusion layers were always composed of an outer compound layer and a hardened bulk layer which thickness was half of the total diffusion layer one. No white layer was observed. Similarly, no traces of chromium nitrides were detected. The temperature seemed to be a parameter more influent than the process duration on the morphological properties of the nitrided layer, while it had no real influence on their crystallinity. Finally, the optimal nitriding conditions to obtain a thick and hard diffusion layer are 500 °C for 10 h.On the other hand, to verify the effect of these parameters on the corrosion resistance, potentiodynamic polarization tests were carried out in an original “wood juice” electrolyte. After corrosion, surface was then observed at the SEM scale. Electrochemical study indicated that the untreated steel behaved as a passive material. Although the very noble character of steel was somewhat mitigated and the corrosion propensity increased for nitrided steels, the passive-like nature of the modified surface was preserved. For the same optimized parameters as those deduced from the mechanical characterization (500 °C, 10 h), surface presented, in addition to a huge surface hardening, a high corrosion resistance.     

Corrosion and mechanical properties of duplex-treated 301 stainless steel

Plasma nitriding is a widely used technique for increasing the surface hardness of stainless steels, and consequently, for improving their tribological properties. It is also used to create an interface between soft stainless steel substrates and hard coatings to improve adhesion. This paper reports on the mechanical and corrosion properties of AISI301 stainless steel (SS) after a duplex treatment consisting of plasma nitriding followed by deposition of Cr bond coat and CrSiN top layer by magnetron sputtering. Mechanical properties of the deposited films, such as hardness (H) and reduced Young's modulus (E_r), were measured using depth-sensing indentation. Potentiodynamic polarization and electrochemical impedance spectroscopy (EIS) were carried out to evaluate resistance to localized and to general corrosion, respectively. The corrosion behavior has been correlated with the microstructure and composition of the surface layers, determined by complementary characterization techniques, including XRD, SEM, and EDS. The CrSiN layers exhibited an H value of 24 GPa, whereas the nitrided layer was shown to present a gradual increase of H from 5 GPa (in the nitrogen-free SS matrix) to almost 14 GPa at the surface. The electrochemical measurements showed that the nitriding temperature is a critical parameter for defining the corrosion properties of the duplex-treated SS. At a relatively high temperature (723 K), the nitrided layer exhibited poor corrosion resistance due to the precipitation of chromium nitride compounds and the depletion of Cr in the iron matrix. This, in turn, leads to poor corrosion performance of the duplex-treated SS since pores and defects in the CrSiN film were potential sites for pitting. At relatively low nitriding temperature (573 K), the nitrided interface exhibited excellent corrosion resistance due to the formation of a compound-free diffusion layer. This is found to favor passivation of the material at the electrode/electrolyte interface of the duplex-treated SS.     

17-4PH不锈钢激光气体渗氮层显微组织与摩擦学性能

目的 提高17-4PH马氏体沉淀硬化不锈钢的表面硬度及耐磨性。方法 采用光纤激光器对17-4PH不锈钢进行激光气体氮化,采用不同激光功率在其表面制备渗氮层。利用光学显微镜(OM)、电子扫描显微镜(SEM)和X射线衍射仪(XRD)等设备分析渗氮层的显微组织和相组成;借助显微硬度仪测试渗氮层截面深度方向的硬度;采用多功能摩擦磨损试验机测试基体、渗氮层的摩擦学性能,并通过SEM分析磨痕形貌,揭示基体与渗氮层的磨损机制。结果 在渗氮前样品组织为回火马氏体,经激光渗氮后样品表面形成了由板条马氏体组成的熔化区和回火马氏体组成的热影响区构成的渗氮层。经渗氮后,样品的硬度均得到提高。在激光功率3 000 W下,渗氮层的表面硬度最高,达到了415HV0.2,约是基体硬度的1.2倍,渗氮层的硬度随着深度的增加呈下降趋势,在深度为2.6 mm处其硬度与基体一致。在回火马氏体向板条马氏体转变的相变强化,以及氮原子(以固溶方式进入基体)的固溶强化作用下,提高了渗氮层的硬度。经渗氮后,样品的摩擦因数均高于基体,但渗氮后其磨损量相较于基体有所减少,在激光功率3 000 W下,其磨损体积最小,相较于基体减少了62%。在激光功率2 500 W下马氏体转变不完全,在激光功率3 500 W下渗氮层出现了裂纹,都降低了渗氮层的硬度,其耐磨性也随之减小,且都略低于在3 000 W下。磨损机制由渗氮前的以黏着磨损为主,转变为渗氮后的以磨粒磨损为主。结论 在17-4PH马氏体沉淀硬化不锈钢表面进行激光渗氮后,其表面硬度和耐磨性均得到提高,在激光功率3 000 W下制备的渗氮层具有较高的表面硬度和优异的耐磨性。     

Plasma nitriding of 42CrMo low alloy steels at anodic or cathodic potentials

The nitriding of low alloy steel has been carried out at anodic potential in a space enclosed by an active screen that consists of two cylinders with different diameter. These two cylinders made up a hollow cathode in a discharge system. The difference in diameter of the two cylinders is about 8-10 mm to maintain strong discharge between them. They can also be heated rapidly to the required temperature for treatment. The sample to be nitrided was held at the same potential as that of the anode used in the discharge and heated through heat radiation from the hot cylinders and by electron bombardment. Electrons bombarded the surface of the sample even though the intensity of bombardment was low because of the anodic sheath. To illustrate the effect of the anodic potential on the nitriding a comparison was made between nitriding at anodic and cathodic potential (general plasma nitriding). The phase composition, the compound layer thickness and the surface topography of the nitrided layer, as well as its properties, were investigated using X-ray diffraction, scanning electron microscopy and microhardness tester. In particular, the corrosion properties of the untreated and plasma nitrided samples were evaluated using anodic polarization tests in 3.5% NaCl solution. The results showed that anodic plasma nitriding not only increased the surface hardness but also improved the corrosion resistance of the low alloy steel.     

Effect of the initial microstructure on the plasma nitriding behavior of AISI M2 high speed steel

The nitriding behavior of AISI M2 steel was studied on samples previously submitted to two different heat treatments in order to investigate the effects of the initial microstructure on the thickness and hardness of nitrided layer. Prior to nitriding, one group of samples was fully annealed while the other group was quenched and tempered, thus acquiring the lowest and highest hardness respectively. Plasma nitriding was performed at 450 °C for 8 h with a mixture of N₂ and H₂ in a plasma reactor working under floating potential. Structural and mechanical properties of nitrided layers were characterized using X-ray diffraction (XRD), optical microscopy and microhardness testing. Variations in surface roughness were obtained by 3D surface profilometry analysis. The thicker nitrided layer was obtained for the fully annealed samples, in which the nitrided layer is composed of γ′-Fe₄N and ε-Fe_2-3N phases plus a diffusion zone. For the hardened-tempered samples, the nitrided region mainly consisted of a diffusion zone. Plasma nitriding increased the surface hardness of the fully annealed samples by 330% and that of the quenched-tempered samples by 50%. The nitrided depth was also estimated using cross-sectional microhardness profiles; giving about 140 µm and ∼ 70 µm for the fully annealed and quenched-tempered samples, respectively. Due to the grain to grain nitrogen diffusion, plasma nitriding also increased the surface roughness. The largest roughness was obtained for the fully annealed samples, in accordance with the largest nitrided depth. The difference in the nitriding behavior was explained on the basis of the microstructural aspects of the substrates such as the concentration of the freely dispersed alloying elements and the level of compressive residual stresses.     

Advance Complex Liquid Nitriding of Stainless Steel AISI 321 Surface at 430 °C

Liquid nitriding of type 321 austenite stainless steel was conducted at low temperature at 430 °C, using a type of a complex chemical heat-treatment; and the properties of the nitrided surface were evaluated. Experimental results revealed that a modified layer was formed on the surface with the thickness ranging from 2 to 30 μm varying with changing treatment time. When the stainless steel subjected to the advanced liquid nitriding less than 8 h at 430 °C, the main phase of the nitrided coating layer was the S phase generally. When the treatment time prolonged up to 16 h, S phase formed and partially transformed to CrN subsequently; and then the fine secondary CrN phase precipitated. All treatments performed in the current study can effectively improve the surface hardness. The nitrided layer thickness changed intensively with the increasing nitrided time. The growth of the nitride layer took place mainly by nitrogen diffusion according to the expected parabolic rate law. The highest hardness value obtained in this experiment was about 1400 Hv_0.25. Low-temperature nitriding can improve the corrosion resistance of the 321 stainless steel against diluted vitriolic acid. The immerse test results revealed that the sample nitrided for 16 h had the best corrosion resistance than the others. SEM examinations indicated that after nitriding, the corrosion mechanisms of the steel had changed from serious general corrosion of untreated sample to selectivity corrosion of nitrided samples in the diluted vitriolic acid.     

Improving the surface properties of A286 precipitation-hardening stainless steel by low-temperature plasma nitriding

Plasma nitriding over a wide range of treatment temperatures between 350 and 500 °C and time from 5 to 30 h on A286 austenitic precipitation-hardening stainless steels has been investigated. Systematic materials characterisation of the plasma surface alloyed A286 alloy was carried out in terms of microstructure observations, phase identification, chemical composition depth profiling, surface and cross-section microhardness measurements, electrochemical corrosion tests, dry sliding wear tests and corrosion-wear tests. Experimental results have shown that plasma nitriding can significantly improve the hardness and wear resistance of A286 stainless steels owing to the formation of nitrogen supersaturated S-phase; the surface layer characteristics (e.g. microstructure, case depth and hardness) of the plasma surface alloyed cases are highly process condition dependent and there are possibilities to provide considerable improvement in wear, corrosion and corrosion-wear resistance of A286 steel.     

The microstructure and properties of 17-4PH martensitic precipitation hardening stainless steel modified by plasma nitrocarburizing

17-4PH martensitic precipitation hardening stainless steel was plasma nitrocarburized at 430 °C and 460 °C for 8 h. The nitrocarburized layers were characterized by optical microscope, scanning electron microscope, X-ray diffractometer, microhardness tests, pin-on-disc tribometer and the anodic polarization method in a 3.5% NaCl solution. The results show that the microstructure of plasma nitrocarburized layer is characterized by a compound layer with no evident diffusion zone. The phases in the 430 °C treated layer are mainly of γ′-Fe₄N, nitrogen and carbon expanded martensite (α′_N), and some incipient CrN phases. When the temperature increases up to 460 °C, there is no evidence of α′_N phase. The processes of bulk precipitation hardening and surface treatment by plasma nitrocarburizing can be successfully combined in a single-step process on this steel. The hardness of modified layer can reach up to 1186HV, which is 3 times higher than that of untreated steel. The wear and corrosion resistance of the specimens can be apparently improved by plasma nitrocarburizing. The 460 °C/8 h treated specimen has the best wear and corrosion resistance in the present test conditions.     

Influence of time on the microstructure of AISI 321 austenitic stainless steel in salt bath nitriding

Influence of nitriding time on the microstructure and microhardness of AISI 321 austenite stainless steel was investigated, using a complex salt bath heat-treatment at low temperature, 430 °C. Experimental results revealed that after salt bath nitriding, a modified layer was formed on the surface of substrate with the thickness ranging from 2 μm to 30 μm with changing treating time. The nitrided layer depth thickened extensively with increasing nitriding time. The growth of the nitrided layer takes place mainly by nitrogen diffusion according to the expected parabolic rate law. Scanning electron microscopy and X-ray diffraction showed that in 321 stainless steel subjected to complex salt bathing nitrided at such temperature for less than 8 hours, the main phase of the nitrided layer was expanded austenite (S phase) by large. When the treatment time is prolonged up to 8 hours and more, S phase is formed and subsequently transforms partially into CrN, and then the secondary CrN phase precipitated. With treating time prolonged, more CrN precipitates formed along the grain boundaries in the outer part. In the inside part between the some CrN and the substrate, there is still a broad single S phase layer. All treatments can effectively improve the surface hardness.     

Surface modification of austenitic stainless steel with plasma nitriding for biomedical applications

In the present study, plasma nitriding of AISI type 303 austenitic stainless steel (SS) specimens was performed using a microwave system. The nitrided layers were characterized by performing scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD), and a Vickers microhardness test. The antibacterial activities of the nitrided layers were evaluated. XRD and TEM showed that a single γ_N phase was formed by plasma nitriding at the plasma power of 700 W and 450 °C. The analytical results demonstrated that the hardness of type 303 specimens could be enhanced by plasma nitriding because of the formation of the γ_N phase. A bacterial test also demonstrated that the nitrided layer exhibited excellent antibacterial properties.     

Investigation of the effects of time and temperature of oxidation on corrosion behavior of plasma nitrided AISI 4140 steel

In this paper, the effect of the time and temperature of the post oxidation process on corrosion behavior of AISI 4140 plasma nitrided steel has been studied. Plasma nitriding was carried out at 550 °C for 5 h with a gas mixture of N2/H2:3/1. The plasma nitrided samples were post oxidized for 30 and 60 min with a gas mixture of O2/H2: 1/5 at temperatures of 400 and 450 °C. The treated samples were characterized by optical microscopy, SEM, XRD, roughness testing, electrochemical polarization and salt spray testing. The X-ray analysis revealed the formation of the iron-nitride phases ε and γ′ during plasma nitriding and the iron oxide phases of magnetite and hematite through the post-oxidizing treatment. It was also demonstrated that the corrosion characteristics of the nitrided compound layer were further improved by post-oxidation treatment and that the least corrosion rate and optimum condition relative to pitting corrosion belongs to the oxidized sample at 450 °C for 30 min.     

Microstructure and corrosion behaviour of pulsed plasma-nitrided AISI H13 tool steel

The effect of pulsed plasma nitriding temperature and time on the pitting corrosion behaviour of AISI H13 tool steel in 0.9% NaCl solutions was investigated by cyclic polarization. The pitting potential (E_pit) was found to be dependent on the composition, microstructure and morphology of the surface layers, whose properties were determined by X-ray diffraction and scanning electron microscopy techniques. The best corrosion protection was observed for samples nitrided at 480 °C and 520 °C. Under such experimental conditions the E_pit-values shifted up to 1.25 V in the positive direction.     

High frequency and low voltage plasma immersion ion implantation of nitrogen on industrial pure iron at different Rf power

Traditional plasma ion immersion implantation (PIII) can effectively improve material mechanical property and corrosion resistance. But the modified layer by PIII is too thin for many industrial applications. High frequency and low voltage plasma immersion ion implantation (HLPIII) has advantages of PIII and nitriding. Comparing with traditional ion nitriding, HLPIII can obtain higher implantation energy and create a thick modified surface layer. In the present paper nitriding layers were synthesized on industrial pure iron using high frequency and low voltage plasma immersion ion implantation with different RF power (400 W, 600 W, and 800 W). The microstructure of the nitriding layers was characterized by X-ray diffraction (XRD) and scanning electron microscopy (SEM). The mechanical properties such as microhardness and wear resistance were analyzed using HXD1000 microhardness and CSEM pin-on-disk wear testing machine. The anodic polarization characteristics were measured in a 0.9% NaCl solution at room temperature to examine the corrosion resistance of the nitriding layer. The results reveal that Fe₂N, Fe₃N and Fe₄N coexist in the nitriding layer. The nitriding layer is a corrosion protective coating on industrial pure iron in 0.9% NaCl solution. The hardness, wear resistance and corrosion resistance of the nitrided layers on industrial pure iron increase with RF power.     

马氏体不锈钢不同渗氮方法对比试验

采用离子渗氮、液体渗氮及气体渗氮对耐蚀耐热马氏体型热稳定不锈钢1Cr12Ni2WMoVNb进行表面改性,研究了不同渗氮方法下不锈钢的硬度、组织形貌、物相变化及脆性,并对3种渗氮方法下不锈钢的耐蚀性及耐高温磨损性能进行了比较。结果表明:3种渗氮方法均可大幅度提高不锈钢的表面硬度,且不同渗氮处理后不锈钢的渗层组织结构大致相同,但表面物相有所差异,离子渗氮后的表面物相主要为Fe₄N及少量CrN相,液体渗氮后为Fe₃O₄及ε相,气体渗氮后为Fe₃O₄、Fe₄N及少量ε相;3种渗氮方法均可提高不锈钢的耐磨损性能,特别是在500~600 ℃下的高温耐磨性得到了大幅提升,但不锈钢渗氮后的耐蚀性均有所降低。