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.     

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.     

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.     

A comparative study: The effect of surface treatments on the tribological properties of Ti-6Al-4V alloy

The effect of different surface treatments on the wear resistance of Ti-6Al-4V alloy has been investigated. For this purpose, plasma nitriding treatment was performed in a gas mixture 75% N₂-25% Ar, for 1 h treatment time and at 750 °C. The thin films were deposited using CFUMBS technique. The results showed that more surface roughness was obtained for nitrided specimens compared with thin film deposited specimens. It was also observed that both surface treatments improved the wear resistance of Ti-6Al-4V alloy. It was determined that plasma nitrided specimens exhibited excellent wear resistance compared with thin film deposited ones when applied load increased. Similar results were obtained from surface hardness measurements, and it was observed that load bearing capacity increased after plasma nitriding. The corrosion resistance of both surface treatments showed similar properties.     

Martensitic stainless steel modified by plasma nitrocarburizing at conventional temperature with and without rare earths addition

17-4PH Martensitic stainless steel was plasma nitrocarburized at conventional temperature (560 °C) with and without rare earths (RE) addition. The surface treated layers were characterized by optical microscope, scanning electron microscope equipped with an energy dispersive X-ray analyzer, X-ray diffraction and microhardness test. The wear and corrosion behavior of the modified specimens was studied respectively using pin-on-disc tribometer and anodic polarization tests. The results show that rare earths atoms can diffuse into the surface of the stainless steel. The microstructures of all modified layers are characterized by a compound layer containing three distinct zones but without an evident diffusion zone. The phases on all modified surface layers are mainly of θ-Fe₃C and CrN. It is exciting that the hardness profile of the modified layer is decreased gradually, which is rarely found in plasma nitriding of the stainless steel. The friction coefficient of a specimen can be dramatically decreased by plasma RE nitrocarburizing, whereas the corrosion resistance is deteriorated. In contrast, the corrosion resistance of a plasma nitrocarburized specimen is enhanced but the friction coefficient is not improved as much as that of a plasma RE nitrocarburized one.     

Corrosion properties of plasma nitrided AISI 410 martensitic stainless steel in 3.5% NaCl and 1% HCl aqueous solutions

Samples of an AISI 410 martensitic stainless steel were plasma nitrided at a temperature of 420 °C, 460 °C or 500 °C for 20 h. The composition, microstructure and hardness of the nitrided samples were characterised using a variety of analytical techniques. In particular, the corrosion properties of the untreated and plasma nitrided samples were evaluated using anodic polarisation tests in 3.5% NaCl solution and immersion tests in 1% HCl acidic water solution. The results showed that plasma nitriding produced a relatively thick nitrided case consisting of a compound layer and a nitrogen diffusion layer on the 410 stainless steel surface. Plasma nitriding not only increased the surface hardness but also improved the corrosion resistance of the martensitic stainless steel. In the immersion test, nitrided samples showed lower weight loss and lower corrosion rate than untreated one. In the electrochemical corrosion tests, the nitrided samples showed higher corrosion potentials, higher pitting potentials and greatly reduced current densities. The improved corrosion resistance was believed to be related to the iron nitride compound layer formed on the martensitic stainless steel surface during plasma nitriding, which protected the underlying metal from corrosive attack under the testing conditions.     

The wear and corrosion properties of stainless steel nitrided by low-pressure plasma-arc source ion nitriding at low temperatures

Low pressure plasma arc discharge-assisted nitriding of AISI 304 austenitic stainless steel is a process that produces surface layers with useful properties such as a high surface hardness of approximately 1500 Hv_0.1 and a high resistance to frictional wear and corrosion. The phase composition, the thickness, the microstructure and the surface topography of the nitrided layer, as well as its properties, depend essentially on the process parameters. Among them, the processing temperature is the most important factor for forming a hard layer with good wear and corrosion resistance. Nitriding austenitic stainless steel at approximately 420°C for 70 min can produce a thin layer of 7–8 μm with very high hardness and good corrosion resistance on the surface. The microstructure was studied by optical microscopy and both glancing angle and conventional Bragg–Brentano (θ–2θ) symmetric geometry X-ray diffraction (XRD). The formation of expanded austenite was observed. Measurements of the wear depths indicated that the wear resistance of austenitic stainless steel can be improved greatly by nitriding at approximately 420°C using low-pressure plasma-arc source ion nitriding.     

Plasma nitriding behavior of Ti6Al4V orthopedic alloy

The influence of plasma nitriding on mechanical, corrosion and tribological properties of Ti6Al4V has been investigated using X-ray diffraction, microhardness tester, scanning electron microscopy, pin-on-disc tribotester, electrochemical polarization and impedance spectroscopy. Plasma nitriding treatment of Ti6Al4V has been performed in 25%Ar-75%N₂ gas mixture, for treatment times of 1-4 h at the temperatures of 650-750 °C. The corrosion tests were carried out in Ringer solution at 37 °C, and the wear tests were performed in dry sliding conditions. XRD analyses confirm the formation of δ-TiN and tetragonal ?-Ti₂N phases in the modified layer. It was observed that the surface hardness and wear resistance increase as the treatment time and temperature increase. The electrochemical impedance measurements indicate a decrease in double layer capacitance value and increase in charge transfer resistance for the nitrided specimens compared to the untreated ones.     

High temperature wear and friction properties of duplex surface treated bearing steels

Duplex treatments by thermo reactive diffusion (TRD) chromizing and puls plasma nitriding were carried out on AISI 52100 and 8620 bearing steels. Tribological behaviors of TRD chromized and duplex treated bearing steels were investigated against Al₂O₃ ball in ball-on-disc system at room temperature and 500 °C. The samples were pack chromized in a furnace at temperature of 1000 °C for 5 h. After chromizing, the samples were puls plasma nitrided for 5 h at 500 °C. The coated steels were characterized using scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDX), X-ray diffraction (XRD), scratch and microhardness testing. Plasma nitriding of chromized steels increased the total thickness of the compound layer. The subsequent plasma nitriding increased the surface hardness to 2135 HK_0.025 due to the formation of CrN and Cr₂N. The surface hardness and scratch resistance of coating can be increased with duplex treatment of chromizing followed by plasma nitriding, resulting in high wear resistance. Tribological tests indicated that puls plasma nitriding process decreased the coefficient of friction values and wear rate of the chromized steels at room temperature and 500 °C. Also, examination of the worn surface of the samples showed that particularly at high temperature, the oxidized compact layer occurs and tribo-oxidation played an important role in oxidation behaviour of the steels after the duplex treatment.     

Surface property enhancement of Ni-free medical grade austenitic stainless steel by low-temperature plasma carburising

Based on the success of the feasibility study reported, the surface properties of low-temperature plasma carburised P558 Ni-free medical grade (ASTM F2581) austenitic stainless steel have been fully evaluated in terms of electrochemical corrosion, dry- and corrosion-wear and fretting-wear in Ringer's solution. Anodic polarization tests demonstrated that the precipitate-free S-phase generated by low-temperature plasma carburising at 500 °C for 15 h can retain the good corrosion resistance of the untreated ASTM F2581 Ni-Free material in Ringer's solution. The wear resistance of the Ni-free austenitic stainless steel can be improved by 700% and 140% when reciprocating against a WC ball in air (dry-wear) and in Ringer's solution (corrosion-wear) respectively. In addition, the low-temperature plasma carburising treatment can considerably reduce the friction coefficient and improve the fretting-wear resistance of the Ni-free austenitic stainless steel in Ringer's solution.     

On the microstructure and phase identification of plasma nitrided 17-4PH precipitation hardening stainless steel

Systematic microstructure characterisation of plasma nitrided (350-500 °C for 10 to 30 h) 17-4PH alloy was carried out using SEM, XRD and TEM. Experimental results have shown that the microstructure and phase constituents of the plasma surface alloyed cases are highly treatment temperature dependent. When treated at low-temperatures (≤ 420 °C), the microstructure is dominated by nitrogen supersaturated martensite (α'_N-expanded martensite); Nitrogen S-phase grains can be formed from the pre-existent retained austenite by converting the retained austenite grains in 17-4PH but no continuous S-phase layer was found. When treated at high-temperatures (above 420 °C), a surface γ′-Fe₄N compound layer was formed, CrN precipitated and S-phase was decomposed.     

Microstructure and mechanical properties of 17-4PH steel plasma nitrocarburized with and without rare earths addition

17-4PH stainless steel was plasma nitrocarburized at 500 °C with and without rare earths (RE) addition. The nitrocarburized layers were characterized by optical microscope, scanning electron microscope equipped with an energy dispersive X-ray analyzer, X-ray diffraction, hardness tests and pin-on-disc tribometer. The results show that rare earths atoms can diffuse into 17-4PH steel surface and change the microstructure of the nitrocarburized layer. The incorporation of RE elements increases the layer thickness and the hardness of the nitrocarburized layer up to 29% and 70–120 HV, respectively. The friction coefficients and wear rates of the nitrocarburized specimens are apparently lower than that of un-nitrocarburized one. The wear mechanisms of steel specimen plasma nitrocarburized with and without RE addition are different mainly due to the differences in the microstructure, the phase proportion and the hardness of the modified layer.     

Influence of initial heat treatment of 17-4 PH stainless steel on gas nitriding kinetics

Results of the investigation of nitrided layers on 17-4 PH type precipitation hardening stainless steel are presented in this paper. The layers have been produced in the process of gas nitriding in a partly dissociated ammonia at temperatures between 410 and 570 °C. Hydrogen chloride admixture to active atmosphere was used as a surface activator. Structure of the nitrided layers were examined using scanning and transmission electron microscopy, X-ray microanalysis (EDX and WDX), and X-ray diffraction. The influence of the initial steel heat treatment on the nitriding kinetics has been considered. 17-4 PH stainless steel was nitrided at various heat treatment conditions, i.e. after solution treatment or ageing at different temperatures. The influence of precipitation processes taking place during the heat treatment before nitriding on the diffusive process kinetics was proven. It was found that, that increasing of steel ageing temperature up to 600 °C before nitriding effects on an increasing of the nitriding kinetics.     

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.     

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.     

304 不锈钢低温离子渗氮及氮碳共渗处理

目的研究304不锈钢离子渗氮层和氮碳共渗层的组织、硬度及耐磨、耐蚀性能,并考察渗层的磨损机理。方法利用离子渗氮及氮碳共渗工艺在304不锈钢表面获得硬化层,利用XRD,OM及共聚焦显微镜、显微硬度仪、电化学测试仪,分析处理前后渗层的组织、相结构及渗层的硬度及耐磨耐蚀性能。结果 304不锈钢氮碳共渗和渗氮层主要为S相层,在相同工艺条件下,氮碳共渗工艺获得的渗层为γN+γC的复合渗层,且厚度大于单一渗氮层。渗氮层和氮碳共渗层硬度约为基体硬度的3.5倍。在干滑动摩擦条件下,氮碳共渗层比渗氮层具有更好的耐磨性能;渗氮层的磨损机理为磨粒磨损的犁沟效应和断裂,氮碳共渗层的磨损机理为磨粒磨损的犁沟和微切削。电化学测试表明,渗氮层和氮碳共渗层的耐蚀性能均优于基体。结论 304不锈钢在420℃进行离子渗氮和氮碳共渗处理后,硬度和耐磨性能可大幅提高,且氮碳共渗处理效果更佳。     

Structure of duplex CrN/NbN coatings and their performance against corrosion and wear

In tribological applications the coating-substrate combination can be considered as a system, since both greatly influence the properties of that affect the tribological performance. Further, it is often desirable that both high wear resistance and corrosion resistance can be achieved even when low cost and easily machineable substrate materials are considered. Duplex surface treatment combining pulse plasma nitriding and PVD coating can provide solution for excellent wear and corrosion resistance for low alloy and constructional steels.In this work three different pulse plasma nitriding processes were carried out prior to the CrN/NbN PVD coating to attain high surface hardness and enhanced load bearing behaviour for S154 high strength construction steel. The phase composition of the compound layer, formed in the nitriding process, was found to greatly affect the tribological properties of the duplex system. The compound layer with high amount of ?-phase contributed to superior corrosion and wear resistance, whereas the ductile γ'-phase compound layer provided better impact resistance and enhanced. The best duplex treated S154 samples had wear resistance comparable to that of similarly coated HSS. The corrosion resistance was also improved by duplex process. If anodic current at + 500 mV vs. SCE is considered as criteria, the best system has almost 3 orders of magnitude lower corrosion current than with the PVD coating alone.     

Tribology and cyclic oxidation behavior of plasma nitrided valve steel

In this study, the tribology and cyclic oxidation behavior of plasma nitrided DIN 1.4871 austenitic valve steel were investigated. For this purpose plasma nitriding treatments were carried out in nitrogen and hydrogen with ratio N₂/H₂: 1/3 at 10 Torr pressure. Nitriding cycles of 400, 450, 500 and 550 °C for 7 h were selected. To remove oxide layer and to enhance diffusion, an effective sputter cleaning procedure was applied in argon and hydrogen gases. The pin-on-disc sliding wear experiments were performed at a load of 6 N and sliding velocity of 0.1 m/s in normal atmosphere under dry condition. Cyclic oxidation tests used to evaluate the oxidation characteristics of the samples consisted of 50 cycles each 30 min at 750 °C. The structure and properties of the samples were examined by optical and scanning electron microscopy (SEM), microhardness measurements and X-ray diffraction. The results indicated plasma nitriding at all temperatures increased the wear resistance of valve steel when sliding against bearing steel. The 550 °C nitrided layer, with CrN, Fe₄N and Fe_2-3N on the surface, was most effective in improving wear resistance. In the case of cyclic oxidation, the results showed that oxidation resistance depends strongly on nitriding temperature. Nitriding at 450 °C produced a layer of predominantly “S” phase which was more effective in improving the oxidation resistance of valve steel.     

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.     

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。