Low Temperature Plasma Nitriding Research Articles

Verbesserte Tribokorrosionsbeständigkeit des martensitischen Stahls X54CrMoVN17-1 durch die Erzeugung von expanded martensite

Seal-free, media-lubricated rolling bearings have a high-energy efficiency as the absence of the seal minimizes frictional loss and increases the efficiency of the driven machine. In addition, the environment is protected by the absence of hazardous lubricants. However, media-lubrication increases tribocorrosive attack on the bearing surface. Therefore, the tribocorrosion resistance of the bearing surface can be increased by a thermal surface treatment called low-temperature plasma nitriding. The produced “expanded martensite” in martensitic steels features a high hardness with comparatively good corrosion resistance. Tribocorrosion tests in 0.9 % NaCl-solution show that the material loss could be reduced by 70 % due to expanded martensite compared to the initial state of the steel.

Formation and Properties of Nitrocarburizing S-Phase on AISI 316L Stainless Steel-Based WC Composite Layers by Low-Temperature Plasma Nitriding

Stainless steel-based WC composite layers fabricated by a laser cladding technique, have strong mechanical strength. However, the wear resistance of WC composite layers is not sufficient for use in severe friction and wear environments, and the corrosion resistance is significantly reduced by the formation of secondary carbides. Low-temperature plasma nitriding and carburizing of austenitic stainless steels, treated at temperatures of less than 450 °C, can produce a supersaturated solid solution of nitrogen or carbon, known as the S-phase. The combined treatment of nitriding and carburizing can form a nitrocarburizing S-phase, which is characterized by a thick layer and superior cross-sectional hardness distribution. During the laser cladding process, free carbon was produced by the decomposition of WC particles. To achieve excellent wear and corrosion resistance, we attempted to use this free carbon to form a nitrocarburizing S-phase on AISI 316 L stainless steel-based WC composite layers by plasma nitriding alone. As a result, the thick nitrocarburizing S-phase was formed. The Vickers hardness of the S-phase ranged from 1200 to 1400 HV, and the hardness depth distribution became smoother. The corrosion resistance was also improved through increasing the pitting resistance equivalent numbers due to the nitrogen that dissolved in the AISI 316 L steel matrix.

Low-Temperature Plasma Nitriding of 3Cr13 Steel Accelerated by Rare-Earth Block

The plasma nitriding of 3Cr13 steel occurred at 450 °C for 4, 8 and 12 h in NH3 with and without rare earth (RE). The nitrided layers were characterized using an OM, SEM, TEM, XRD, XPS, microhardness tester and electrochemical workstation. The modified layer, with and without La, are composed of a compound layer and diffusion layer from surface to core. After the addition of La during nitriding, the maximum increase of layer thickness, mass gain and average microhardness was 15.6%, 35.8% and 212.50HV0.05, respectively. With the increase of the proportion of ε-Fe2-3N, the passivation zone of the corrosion resistance curve increases from 2.436 to 3.969 V, the corrosion current density decreases, the corrosion potential and pitting potential both increase, and, consequently, the corrosion resistance is significantly improved. Most of the surface microstructures of the nitrided layer was refined by the addition of La. The presence of La reduces the N content in the modified layer, which accelerates the diffusion of N atoms and, thus, accelerates the nitriding process.

Effect of Deformation on the Microstructure of Cold-Rolled TA2 Alloy after Low-Temperature Nitriding

In order to improve the low hardness and poor wear resistance of TA2, this paper proposes a composite process of cold-rolling and low-temperature plasma nitriding with recrystallization. This composite modification process can effectively achieve the dual goals of modifying the matrix structure and surface of TA2 alloy simultaneously. The cold-rolling experimental results indicate that when the deformation rate increases, the small-sized grains in the sample increase significantly, and the grain orientation changes from TD (transverse direction) to RD (rolling direction) and then to TD. The nitriding experimental results indicate that the {0001} basal surface texture deflected from the TD direction to the RD direction, {10-10} cylindrical texture components gradually increased, and the special orientation phenomenon of cylindrical and conical texture disappeared, it can be seen that an increase in the deformation rate promotes recrystallization. The XRD test results indicate that after low-temperature nitriding, metastable nitriding phase TiN0.26 is formed on the surface of TA2. The SEM morphology of the cross-section shows that a relatively special nitrided zone is formed, and mechanical performance test results indicate the wear resistance and hardness of the alloy increased.

Sequential low-temperature plasma-assisted thermochemical treatments of the AISI 420 martensitic stainless steel

The application of low-temperature plasma carburizing (C), nitriding (N) and nitrocarburizing (NC) treatments in sequential steps on AISI 420 martensitic stainless steel was investigated through nine different treatments. Experiments were performed at 400 °C, being divided in three (8 h)-single treatments, namely C, N and NC, and six distinct (4 h + 4 h)-sequential treatments, namely C + N, N + C, C + NC, N + NC, NC + N, and NC + C, using appropriate gas mixtures for each treatment step. Sequential treatments promoted the formation of treated layers constituted of iron carbides/nitrides, chromium nitrides, and nitrogen/carbon-expanded martensite phases. Interesting results were obtained for both C + N and C + NC sequential treatments, whose application results in greater hardening depths (~20% thicker) and leads to ~40% increase on the surface hardness, when compared to the obtained for the single C treatment keeping a smooth hardness profile. From the microstructural characterization, no significant sensitization was evidenced in the outer layers obtained for all treatments comprising the carburizing step, an indicative result that the interstitial carbon retards the chromium-rich particles precipitation kinetics. The combination of N + NC treatments produced thicker and harder treated cases compared to those produced by the respective single treatments. In brief, results showed that the appropriate selection of thermochemical treatments' sequence can promote increased treatments efficiency concerning the treated layers thickness or effective surface hardness. This work also contributes to the validation of the presented processing approach, proving its advantages over single thermochemical treatments.

Cyclic Fatigue of Dental NiTi Instruments after Plasma Nitriding.

This study investigated the possibility of nitride NiTi instruments using low-temperature plasma nitriding technology in a standard industrial device. Changes in the properties and fatigue life of used NiTi instruments before and after low-temperature nitriding application were investigated and compared. Nontreated and two series of plasma-nitrided NiTi instruments, designed by Mtwo company with tip sizes of 10/.04 taper, 15/.05 taper, and 20/.06 taper, were experimentally tested in this study. All these instruments were used and discarded from clinical use. The instruments were tested in an artificial canal made of stainless steel with an inner diameter of 1.5 mm, a 60° angle of curvature, and a radius of curvature of 3 mm. A low-temperature plasma nitriding process was used for the surface treatment of dental files using two different processes: 550 °C for 20 h, and 470 °C for 4 h. The results proved that it is possible to nitride dental instruments made of NiTi with a low-temperature plasma nitriding process. Promising results were achieved in trial testing by NiTi instruments nitrided at a higher temperature. Plasma-nitrided files were found to have, in some cases, significantly higher values than nontreated files in terms of fatigue life. The results showed that the nitriding process offers promising possibilities for suitably modified surface properties and quality of surface layer of NiTi instruments. Within the limitations of the present study, the cyclic fatigue life of plasma-nitrided NiTi dental files can be increased using this surface technology.

Comprehensive analysis of pulsed plasma nitriding preconditions on the fatigue behavior of AISI 304 austenitic stainless steel

This study aims to draw an exact boundary for microstructural and mechanical behaviors in terms of pulsed plasma nitriding conditions. The pulsed plasma nitriding treatment was applied to AISI 304 austenitic stainless steel at different temperatures and durations. Results reveal that nitriding depth increased as process temperature and duration increase. The nitriding depth remarkably increased at 475°C for 8 h and at 550°C for 4 h. An austenite structure was transformed into a metastable nitrogen-oversaturated body-centered tetragonal expanded austenite (S-phase) during low-temperature plasma nitriding. The S-phase was converted to CrN precipitation at 475°C for 8 h and at 550°C for 4 h. Surface hardness and fatigue limit increased through plasma nitriding regardless of process conditions. The best surface hardness and fatigue limit were obtained at 550°C for 4 h because of the occurrence of CrN precipitation.

Application of Active-Screen Plasma Nitriding to an Austenitic Stainless Steel Small-Diameter Thin Pipe

Low-temperature active-screen plasma nitriding (ASPN) was applied in this study to improve the bending rigidity and corrosion resistance of a small-diameter thin pipe composed of austenitic stainless steel (SUS 304). The inner and outer diameters of the pipe were ϕ0.3 and ϕ0.4 mm, respectively, and the pipe length was 50 mm. The jig temperature was measured using a thermocouple and was adopted as the nitriding temperature because measuring the temperature of a small-diameter pipe is difficult. The nitriding temperature was varied from 578 to 638 K to investigate the effect of temperature on the nitriding layer and mechanical property. The nitriding layer thickness increased with an increase in nitriding temperature, reaching 15 μm at 638 K. The existence of expanded austenite (S phase) in this nitriding layer was revealed using the X-ray diffraction pattern. Moreover, the surface hardness increased with the nitriding temperature and took a maximum value of 1100 HV above 598 K. The bending load increased with an increase in the nitriding temperature in relation to the thicker nitriding layer and increased surface hardness. The nitrided samples did not corrode near the center, and corrosion was noted only near the tip at high nitriding temperatures of 618 and 638 K in a salt spray test. These results indicated that the bending rigidity of the small-diameter thin pipe composed of austenitic stainless steel was successfully improved using low-temperature ASPN while ensuring corrosion resistance.

Corrosion Resistance of Ferritic Stainless Steel X12Cr13 After Application of Low-Temperature and High-Temperature Plasma Nitriding

The impact of plasma nitriding process on corrosion resistance of ferritic stainless steel (FSS) was evaluated in this study. The FSS X12Cr13 (AISI 410) was subjected to low-temperature plasma nitriding (LTPN) treatment at a temperature of 400°C in 3H2:1N2 (l/h) and in 1H2:3N2 (l/h) reverse working atmosphere (LTPN-R) and to high-temperature plasma nitriding (HTPN) treatment at 550 °C for 15 h. The microstructure and microhardness of the untreated and nitrided stainless steel were evaluated. The corrosion properties of the untreated and plasma nitrided steel samples were evaluated using the anodic potentiodynamic polarization tests in neutral 2.5% NaCl deaerated solution. The phase analysis showed that LTPN and LTPN-R treatment on the AISI 410 steel led to the formation of N layer (nitrogen expanded ferrite) accompanied by Fe3C and Fe4N iron nitrides and CrN. The HTPN technique led additionally to the formation of an increased volume of Cr4N4 chromium nitrides and Cr15Fe7C6 chromium iron carbide. The plasma nitriding process significantly increased the microhardness of the ferritic stainless steel. The pitting was evaluated, and the pitting coefficient was calculated. The electrochemical corrosion tests showed the best corrosion resistance of the untreated X12Cr13 stainless steel, only slightly increased corrosion rates of LTPN and LTPN-R techniques, and extreme corrosion rates after application of the HTPN technique, causing Cr depletion and thereby suppressing the ability to passivation.

Shaping the structure and properties of titanium and Ti6Al7Nb titanium alloy in low-temperature plasma nitriding processes

Plasma nitriding of titanium Grade 2 and Ti6Al7Nb titanium alloy at 730 °C was used to produce nitrided surface layers with an outer zone consisting of nanocrystalline titanium nitride - TiN, and a Ti2N zone right above the αTi(N) diffusion area. The paper presents a comparison of structure (TEM, SEM), phase composition (XRD, SAED) surface topography (AFM, optical profilometer), corrosion (potentiodynamic method), tribological properties (‘ball-on-disc’), and adhesion (scratch-test) of TiN + Ti2N + αTi(N) type nitrided surface layers produced on Grade 2 titanium and Ti6Al7Nb titanium alloy using conventional glow-discharge nitriding (so called glow discharge nitriding at the cathode potential) and with the use of an ‘active screen’ (glow discharge nitriding at plasma potential). A reduction of cathodic sputtering in the plasma potential process made it possible to produce surface layers maintaining a high smoothness of the titanium surfaces. Due to the low surface roughness and the high compressive residual stress of the sample after nitriding at plasma potential, ‘ball-on-disc’ test results showed the lowest coefficient of friction and the lowest penetration depth for this layer and very good adhesion of the layer to the substrate – i.e. Ti6Al7Nb titanium alloy. Nitriding of titanium alloy at cathode potential increased the corrosion potential value and slightly decreased corrosion current density. The corrosion current density of the sample nitrided at plasma potential was similar to initial state Ti6Al7Nb titanium alloy. The nitriding process type (cathode potential or plasma potential) used to produce TiN + Ti2N + αTi(N) surface layers on Ti6Al7Nb titanium alloy has an influence on the microstructure of the layer, its residual stress, in particular its TiN outer titanium nitride zone, its thickness, and on its properties such as wear and corrosion resistance.

Evaluation of the sliding wear and corrosion performance of triode-plasma nitrided Fe-17Cr-20Mn-0.5N high-manganese and Fe-19Cr-35Ni-1.2Si high-nickel austenitic stainless steels

Low-temperature plasma nitriding has been widely studied and applied, in enhancing the wear performance of austenitic stainless steels (ASSs) without losing corrosion resistance. In this work the wear and corrosion behaviours of two specialty ASSs, i.e. Staballoy® AG17 (Fe-17Cr-20Mn-0.5N, in wt%) and RA330® (Fe-19Cr-35Ni-1.2Si, in wt%), were evaluated – and compared to AISI 304 – before and after low-temperature triode plasma nitriding (TPN) at 400 °C and 450 °C. A nitrogen interstitially-supersaturated expanded austenite layer (γN) was developed for all three ASSs after TPN treatment at 400 °C, which led to a) an approximately 4-fold increase in surface hardness, b) a reduction in specific wear rate of at least 2 orders of magnitude in unlubricated dry-sliding, and c) an improved resistance to pitting in 3.5 wt% NaCl aqueous solution. Large numbers of ‘linear defects’ (identified in TEM studies as strips of HCP-εN) were seen in the γN-AG17 layer, that could be correlated to comparatively higher surface hardness and better wear resistance. Several slip/shear bands were also seen in the γN-330 layer, where short-range Cr-segregation could occur, leading to localised corrosion. More importantly, after TPN treatment at 450 °C, alloys AISI 304 and AG17 presented a deterioration in corrosion performance, whereas good corrosion performance was maintained for alloy RA330. Redistribution of Si (in preference to Cr) was revealed in γN-330 after TPN treatment at 450 °C, whereby Si-alloying at a significantly higher level than in the other two alloys investigated appears (in addition to the high Ni content in alloy 330) to be beneficial in delaying CrN precipitation, and thus in maintaining the good corrosion performance of γN after nitriding at low-to-intermediate temperatures.

Enhancement of hardness of low alloy steel after low temperature plasma nitriding

The present work is focused on the plasma assisted nitriding of martensitic stainless steel at low temperature. Sample coupons of dimensions 8 × 8 × 6 mm3 were cut from the hardened and tempered steel sheet. Following grinding and mirror polishing samples were placed inside the chamber. At a low temperature of 460 °C (±10) nitriding was performed in the plasma generated by nitrogen and hydrogen gas mixture, Nitrided samples were then subjected to hardness measurements. The structural characterization was followed by X-ray diffraction (XRD) studies for the phase analysis. It was shown that even at a low temperature the surface modifies to high hardness for the improved tribological properties.

Anticorrosion Properties of the Low-Temperature Glow Plasma Nitriding Layer on AISI 904L Austenitic Stainless Steel in Hydrofluoric Acid Obtained at Various NH3 Pressures

A low-temperature (400 °C) glow plasma nitriding layer on AISI 904L austenitic stainless steel was obtained at various NH3 pressures and studied using electrochemical method, X-ray diffraction, and scanning Kelvin probe. The pressure of NH3 dominated the microstructure of the nitriding layer. The saturation degree of γN controlled corrosion performance and microhardness. Insufficient NH3 pressure (<100 Pa) resulted in discontinuous nitride caking coverage, whereas excessive NH3 pressure (>100 Pa) facilitated the transformation of the nitriding layer to harmful nitrides (CrN) due to a localized overheating effect caused by the over-sputtering current.

Corrosion Resistance of Plasma Nitrided Austenitic Stainless Steel AISI 304 (X5CrNi18-10)

In this paper, austenitic stainless steel AISI 304 (X5CrNi 18-10) has been subjected to low-temperature plasma nitriding (LTPN) at 400°C (673 K) in 24H2:8N2 (l/h), and in 8H2:24N2 (l/h) marked as LTPN-R, and to high-temperature plasma nitriding (HTPN) at 550°C (823 K) in 24H2:8N2 (l/h) working atmosphere, for 15h. The microstructure, microhardness, and phase evaluation of the nitrided steel were studied. The PN led to significant microhardness increase from 206 ± 3 HV0.05 to 842 ± 27 HV0.05 (LTPN), 821 ± 18 HV0.05 (LTPN-R), resp. to 1246 ± 27 HV0.05 (HTPN). The corrosion properties were evaluated using the anodic potentiodynamic polarization tests in neutral 2.5% NaCl deaerated solution. The corrosion rate CR (mm.a-1) increased only slightly for LTPN procedures. But using the HTPN increased 43-times to untreated steel, due to reduced passivation ability by chromium depletion by formed CrN. Additionally, the pitting was evaluated, and the pitting coefficient was calculated.

Micro-/Nano-Texturing of Aluminum by Precise Coining for Functional Surface Decoration

The AISI316 austenitic stainless steel die was prepared and nitrided at 673 K for 14.4 ks. Through this low temperature plasma nitriding, the AISI316 die was homogeneously hardened up to 1400 HV within its surface layer of 50 μm. This nitrided AISI316 die was utilized to print the tailored micropattern with nanotextures onto its surface by the femtosecond laser processing. Each micropattern consisted of the tailored segments to have unidirectional nanotextures with different orientations. Each segment was recognized by its intrinsic surface plasmonic brilliance to tailored nanotextures. The CNC (Computer Numerical Control) stamping system was used to coin these micropatterns with nanotextures onto the AA1060 aluminum plates with the thickness of 1 mm. SEM (Scanning Electron Microscopy) and optical microscopy were employed to characterize the original micro-/nano-textures on the AISI316 die as well as the coined nanotextured patterns on the AA1060 plate surfaces.

Low-Temperature Plasma Nitriding of Low- and High-Chromium Steels

The possibility of plasma nitriding without altering the surface morphology of structural steels 30Ni2CrMoV (30ХН2МФА) and 30CrMnSi (30ХГСА) with low chromium contents and steels 03Cr11Ni10Mo2Ti (03Х11Н10М2Т-ВД) and Cr12Mo (X12M) with high chromium contents is studied at temperatures of 400–450°C. Compound layers do not form in 30Ni2CrMoV and 30CrMnSi steels upon nitriding at low nitrogen concentrations in mixtures of N2+H2, and their surface morphologies remain the same. Nitriding can be done for steels 03Cr11Ni10Mo2Ti and Cr12Mo without forming compound layers, but the surface roughness increases at both low and high concentrations of nitrogen in the working gas.

Low-temperature plasma nitriding of martensitic stainless steel

This study presents the plasma nitriding of Cr–Mo–V tool steel to protect it from environmental degradation. The steel samples after metallographic polishing were nitrided in the glow discharge plasma of N2 and H2 gas mixture (80:20). Nitriding was performed at two different temperatures, a lower temperature of 450 °C and the higher temperature of 500 °C. The potentiodynamic polarization tests in 3.5% NaCl electrolyte had shown the enhancement of corrosion resistance of steels after nitriding. X-ray diffraction (XRD) studies and scanning electron microscopic analysis coupled with energy dispersive spectroscopic analysis (SEM/EDS) was performed to understand the modification of surface microstructure. XRD analysis of the nitrided steels revealed the presence of γ′- and e-nitrides of iron, which were responsible for the improvement of corrosion resistance.

Effects of low and high temperature plasma nitriding on electrochemical corrosion of steel

Abstract This study concerns plasma nitriding of tool steel at different temperatures and its effects on corrosion resistance. Inside the nitriding reactor steel samples were placed on the sample holder after metallographic polishing and then the vacuum chamber was evacuated to a pressure of ∼0.5 Pa. At a lower temperature of 450 °C and the higher temperature of 550 °C nitriding was performed for a fixed duration of 10 h. All the nitrided and the bare steel samples studied under X-ray diffraction (XRD) and scanning electron microscopic analysis/energy dispersive X-ray spectroscopy (EDS). Iron nitride (FexN, x = 2–3, 4) peaks were revealed in the nitrided steels after XRD analyses. EDS revealed the increased amount of nitrogen in the nitrided sample treated at 550 °C. For the assessment of corrosion resistance of these steel samples potentiodynamic polarization tests were performed in 3.5% NaCl. On comparison, it was found that the steel nitrided at higher temperature is more effective in enhancing the corrosion resistance.

Low-Temperature Plasma Nitriding for Austenitic Stainless Steel Layers with Various Nickel Contents Fabricated via Direct Laser Metal Deposition

In this study, low-temperature plasma nitriding is applied to austenitic stainless steels at temperatures below 450 °C. This enhances the wear resistance of the steels with maintaining corrosion resistance, by producing expanded austenite (known as the S-phase), which dissolves excessive nitrogen. Austenitic stainless steels contain nickel, which has the potential to play an important role in the formation and properties of the S-phase. In this experiment, austenitic stainless steel layers with different nickel contents were processed using direct laser metal deposition, and subsequently treated using low-temperature plasma nitriding. As a result, the stainless steel layers with high nickel contents formed the S-phase, similar to the AISI 316L stainless steel. The thickness and Vickers hardness of the S-phase layers varied with respect to the nickel contents. Due to lesser chromium atoms binding to nitrogen, the chromium content relatively decreased. Moreover, there was no evident change in the wear and corrosion resistances due to the nickel contents.

Effect of Low-Temperature Plasma Nitriding on Corrosion and Surface Properties of Duplex Stainless Steel UNS S32205

The duplex stainless steel UNS S32205 was plasma nitrided at 380 °C for 10 h using a gas mixture of 25% N2-75% H2. The thickness of the nitrided layer was 4.5 ± 0.5 μm, composed mainly of nitrogen-expanded austenite and iron nitrides precipitates. There was an increase in surface hardness around 2.6 and 3.8 times in the nitrided layer formed on the austenite and the ferrite phases, respectively, in relation to the untreated samples. The surface texture parameters skewness (Ssk), maximum peak height (Sp) and texture aspect ratio (Str) were the most appropriate parameters for studying the topography changes after treatment. An improvement in the localized corrosion properties after the nitriding treatment was revealed by the cyclic polarization curves. The nitrided samples showed higher pitting corrosion and repassivation potentials compared to the untreated material. The ferritic phases and grain boundaries were more susceptible to corrosion in the nitrided samples. The potentiodynamic curves of the nitrided samples exhibited a hillside on the passive-to-transpassive transition. This feature was already observed by other researchers, but it has not been well investigated. Potentiostatic studies demonstrated that metastable pitting took place on this transition.