Elevated temperature nitrogen plasma immersion ion implantation of AISI 302 austenitic stainless steel

AISI 302 steel was modified using elevated temperature nitrogen plasma immersion ion implantation. The thickness of the modified layers is improved significantly compared with that of the layer implanted at room temperature. The surface nanohardness of the treated sample is much higher. Both the friction coefficient and wear rate are dramatically reduced due to the formation of new phases such as (Cr, Fe)₂N_1−x, ε-(Fe, Cr, Ni)_2+xN, nitrogen expanded austenite (γ_N) or noncrystalline phase in the near surface.     

Corrosion behavior of AISI302 steel treated by elevated temperature nitrogen plasma immersion ion implantation

The corrosion behavior of AISI302 steel implanted with nitrogen at elevated temperature was investigated by electrochemical impedance spectroscopy. Equivalent circuits for explaining the impedance characteristics are proposed. The thick passive layer containing Cr₂O₃ and the expanded austenite layer in the sub-surface worked together, resulting in the high corrosion resistance.     

Parametric study of nitrided AISI 304 austenite stainless steel prepared by plasma immersion ion implantation

This paper investigates the characteristics of plasma immersion nitrogen-ion implanted AISI 304 austenite stainless steel against such processing parameters as bias voltage (5-20 kV), substrate temperature (300-500 °C), and implantation fluence (1.4 × 10¹⁸-4.2 × 10¹⁸ cm^− 2). Characteristics of the as-implanted specimens under investigation included elemental depth profile, hardness depth profile, crystallographic structure, and corrosion behavior and were determined using glow discharge spectrometry (GDS), the Vickers hardness tester, X-ray diffractometry (XRD), and the potentiodynamic polarization test, respectively. The results show that nitrogen depth profiles strongly depend on these processing parameters and closely relate to the corresponding chromium depth profiles. The hardness depth profiles increase and widen as substrate temperature, bias voltage, and implantation fluence increase. In particular, an improvement in hardness is accompanied by a reduction in corrosion resistance when substrate temperature reaches 500 °C. The corrosion-resistance degrader, CrN, precipitates as substrate temperature exceeds 450 °C, a phenomenon which is clearly evident in the chromium depth profiles as well as the XRD results.     

Hybrid elevated-temperature,low/high-voltage plasma immersion ion implantation of AISI304 stainless steel

Elevated-temperature plasma immersion ion implantation (PIII) is an effective non-line-of-sight technique to harden austenitic stainless steel by producing expanded austenitic phases in the near surface region. We report here a hybrid elevated-temperature, low/high voltage approach, which improves the efficiency while retaining the non-line-of-sight advantages of PIII. A low-voltage (4 kV), elevated-temperature (355°C) PIII process is first used to produce the modified layer, but the nitrogen concentration in this layer is typically relatively low and the thickness may not be adequate. This is followed by high-voltage (25 kV) PIII at a lower temperature to increase the nitrogen concentration and to achieve the desirable surface enhancement effects. To assess the efficacy of the technique, the samples are characterized using X-ray diffraction (XRD), nanohardness measurements, and secondary ion mass spectrometry (SIMS) depth profiling. The experimental results show that the nitrogen concentration increases by nearly 75% and the nitrogen penetration depth nearly doubles that of the low-voltage sample. The surface microhardness also improves by 150% and our data suggest that it is due to the formation of expanded austenites.     

Tribological behavior of AISI302 austenitic stainless steel modified by elevated temperature nitrogen plasma immersion ion implantation

AISI302 stainless steel samples were modified by elevated temperature nitrogen plasma immersion ion implantation at temperature ranging from 330 ℃ to 450 ℃. The tribological behaviors of the implanted layers of the samples were investigated. The samples were characterized by Auger electron spectroscopy (AES), glancing angle X-ray diffraction (GXRD), and nanoindentation. The results show that the implantation temperature plays an important rule on the microstructure and surface properties of the implanted layers. The thickness of the modified layer implanted at 390 ℃ is about 9 μm. It is improved about two orders compared with that of the implanted at room temperature. The surface nanohardness and the wear resistance of elevated temperature implanted layers increase significantly, and the friction coefficient decreases obviously in comparison with the unimplanted one. These data suggests that the improvement results from the formation of new phases such as ε-(Fe, Cr, Ni)2 xN, or noncrystal phase.     

Synchronous plasma enhancement in RF-driven plasma source for ion implantation

We report an original method to increase periodically the plasma density in RF-driven plasma source for surface treatment of materials by ion implantation. The method consists of supplementary injection of ions, electrons and metastable atoms into the processing RF plasma using very short high voltage pulsed discharges applied on a separate electrode at the same repetition rate as the negative accelerating pulses applied on the target. Thus plasma density is periodically increased by an order of magnitude so that the synchronized negative pulses applied on the target for ion implantation find a background plasma about 10 times denser. The advantages of this new method were revealed by nitrogen implanted tests on copper and brass samples.     

Fluorine and carbon ion implantation and deposition on metals by plasma source ion implantation

Deposition of fluorine containing diamond-like carbon films is an effective solution for the improvement of machine parts in an aggressive aqueous environment when the combination of a hydrophobic surface with good corrosion protection and low friction coefficients is required. Stainless steel and silicon were treated by plasma source ion implantation using the gases CF₄, C₆F₆ and C₆H₅F, in the latter case with previous methane implantation. Depending on the plasma gas there are differences in the fluorine content, depth distribution, film thickness, water contact angle and friction coefficient.     

Reduction in surface resistivity of polymers by plasma source ion implantation

The surface resistivity of several polymers such as poly(styrene/butadiene copolymer), modified poly(phenyleneoxide), poly(ethylene terephthalate), and polyimide was improved by the argon gas plasma source ion implantation (Ar-PSII) technique equipped with a mesh-type conducting grid. With the grid, the surface resistivities of the modified polymers decreased up to 11 orders of magnitudes at a high ion dose, and remained nearly at the same values after 3 months. The PSII treated polymer sample with the grid provided more uniformly modified surface and lower surface resistivity than that treated without the grid. The extent of the decrease in surface resistivity depended on the polymer structures and physical properties. However, the surface resistivity was independent of the sample thickness, the grid size, and the grid height. Surface analyses using scanning electron microscopy, time-of-flight secondary ion mass spectrometry, and Raman spectroscopy provided the useful information on modified surfaces.     

Nitrogen diffusion in medical CoCrNiW alloys after plasma immersion ion implantation

CoCr alloys are widely used for medical applications, e.g. total hip replacements or coronary stents. Nevertheless, an increase in the surface hardness and a reduction of the wear rate is still desirable to improve the biocompatibility. Plasma immersion ion implantation (PIII) at different temperatures, acceleration voltages and working pressures is used to determine the nitrogen diffusivity in the CoCr alloys SY21med, L605 and HS188. Depending on the temperature, two different treatment regimes can be distinguished, independent of the ion energy. At low temperatures, a diffusion process with an activation energy of 1.0-1.1 eV is present, indicative of interstitial nitrogen diffusion. Beyond 350 °C, a reduced activation energy of 0.5-0.7 eV is observed. Additionally, a strong dependency of the layer thickness on the working pressure in the range 0.3-0.8 Pa was observed for the temperature dependent diffusion regime, which suggests a synergistic interplay of adsorption and implantation during PIII. Below 500 °C, an increase of the diffusion coefficient by three orders of magnitude was observed for PIII, compared with pure plasma nitriding.     

Delayed cracking in plasma nitriding of AISI 420 stainless steel

The phenomenon of delayed cracking in nitrided layers after DC-plasma nitriding of AISI 420 steel has been observed by optical microscopy. Prior to the plasma treatment, the samples were austenitized at 1303 K for 30 min and then oil quenched. Two tempering conditions were assessed: one group was tempered at 673 K, while another group was tempered at 943 K.All samples were subjected to sputtering, in the plasma chamber, to remove the passive oxide layer, under a 1:1 Ar/H₂ atmosphere. Finally, specimens were plasma nitrided at 673 K for 20 h, with a 1/3: N₂/H₂ relation, at a pressure of 6.5 hPa and 700 V bias in the nitriding chamber.The nitrided layers were analyzed initially by X-ray diffraction (XRD). Detailed observations were conducted at frequent and regular intervals under optical microscopy (OM) and scanning electron microscopy (SEM) with secondary and back-scattered electrons detectors. The results revealed that after an incubation time, even without any external disturbance, cracks are formed and propagate in the nitrided layers. Both groups of samples were equally affected. The presence of precipitated particles and local residual stresses are possible causes of such a phenomenon.     

Pulse current plasma assisted electrolytic cleaning of AISI 4340 steel

An electrolytic plasma process (EPP) for cleaning AISI 4340 steel was performed in a 10% solution of sodium bicarbonate operated at 70 °C. The effects of the pulse frequency (f) and duty cycle (δ) on the surface morphology, microstructure, mechanical and corrosion properties were investigated. Compared to the conventional DC process, the pulsed EPP cleaning resulted in reduced surface roughness and compressive residual stress at the surface. Minimal reduction in hardness and no reduction in toughness due to hydrogen embrittlement (ASTM F519) were found. At the same time, rotating bending beam fatigue tests indicated a noticeable reduction in fatigue life, which could be offset by a shot peening treatment prior to EPP cleaning at 10 kHz and δ = 0.8. Glow discharge optical emission spectroscopy indicated minimal changes in the surface composition and potentiodynamic corrosion studies revealed a slight ennoblement of the surface attributable to an increased rate of cathodic processes. Optimal process parameters were identified for δ = 0.8 and f = 100–10,000 Hz.     

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.     

Electrochemical studies of stainless steel implanted with nitrogen and oxygen by plasma immersion ion implantation

Plasma Immersion Ion Implantation (PIII) of stainless steel with nitrogen at temperatures lower than 400 °C has been reported to increase the hardness of the material by several times. However, expectations that the corrosion resistance will remain unaffected after implantation were not found to be so. In the present study the influence of post-oxygen implantation on the corrosion resistance of nitrogen implanted stainless steel is presented. Stainless steel samples were subjected to oxygen, nitrogen and post-oxygen ion implantation at different temperatures. GIXRD and microRaman studies of the implanted samples showed that oxygen implantation leads to the formation of an oxide layer consisting of corundum and spinel structures. The corrosion properties of the implanted samples were studied by potentiodynamic polarization and electrochemical impedance techniques in 3.5% NaCl solution. After nitrogen implantation the corrosion current increased and the corrosion potential shifted to the less noble side to − 0.486 V as compared to − 0.284 V for the substrate. Oxygen implantation at 400 °C shifted the corrosion potential to the nobler side to − 0.2 V with decrease of corrosion current. For post-oxygen ion implantation at temperatures lower than 400 °C, the corrosion current was higher than the substrate and the corrosion potential was also on the less noble side. However, post-oxygen ion implantation at 400 °C after nitrogen ion implantation resulted in improved corrosion resistance as the corrosion potential shifted to nobler side and the corrosion current was lower than that of substrate.     

Selective laser melting of Fe-Ni-Cr layer on AISI H 13 tool steel

An attempt to fabricate Fe-Ni-Cr coating on AISI H13 tool steel was performed with selective laser melting. Fe-Ni-Cr coating was produced by experimental facilities consisting of a 200 W fiber laser which can be focused to 80 μm and atmospheric chamber which can control atmospheric pressure with N₂ or Ar. Coating layer was fabricated with various process parameters such as laser power, scan rate and fill spacing. Surface quality and coating thickness were measured and analyzed. Three different surface patterns, such as type I, type II and type III, are shown with various test conditions and smooth regular pattern is obtained under the conditions as 10 μm of fill spacing, 50–350 mm/s of scan rate and 40 μm of fill spacing, 10–150 mm/s of scan rate. The maximum coating thickness is increased with power elevation or scan rate drop, and average thickness of 10 μm fill spacing is lower than that of 40 μm fill spacing.     

Investigation of compound layer formed during ion nitriding of AISI 4140 steel

Low alloy AISI 4140 steel was ion nitrided at temperatures of 500, 550 and 600 °C for various times in a 50%N₂---50%H₂ gas mixture. The nature of the compound layer formed was studied by X-ray diffraction and optical metallography. The X-ray analysis shows the existence of a γ-Fe₄N compound zone on the surface at all three temperatures. The thickness of the compound layer increases with increasing time at 500 and 550 °C; however, it begins to decrease with increasing time at 600 °C.     

Determination of the optimum conditions for ion nitriding of AISI 5140 steel

AISI 5140 low alloy steel was ion nitrided under different process parameters including time (1, 4, 8 and 12 h), temperature (400, 450, 500 and 550 °C) and gas mixture ratio (0.05, 0.33, 1 and 3 N₂/H₂). By determining the fatigue strength, surface hardness, compound layer thickness and case depth, the optimum working conditions were determined by using a Taguchi design of experiment. After ion nitriding process, it is aimed to maximize fatigue strength, surface hardness and case depth as well as to minimize compound layer thickness. While the optimum conditions were determined, due to the goals (above aims) more than one being, the trade-off among goals was considered. First of all, each goal was optimised, separately. Then, all the goals were optimised together, considering the priority of the goals, and the optimum results were obtained at 0.05 N₂/H₂ gas mixture ratio, at the temperature of 450 °C and for 12 h process time.     

温度对AISI304奥氏体不锈钢离子渗氮的影响

对AISI304奥氏体不锈钢进行脉冲电流辉光离子渗氮处理,在不同处理温度(480 ℃、520 ℃、580 ℃)下渗氮8 h后,获得了一定厚度的渗氮层.通过对渗层进行金相分析和硬度测试表明,随着渗氮温度升高,渗层厚度增大,显微硬度先增大后减小.综合温度对渗层厚度与显微硬度的影响,AISI304奥氏体不锈钢卡套辉光离子渗氮温度可采用520 ℃,渗氮后渗层厚度为90 μm,显微硬度为1317 HV0.1.     

Diamond-like carbon films synthesized on bearing steel surface by plasma immersion ion implantation and deposition

Diamond-like carbon (DLC) films were synthesized by plasma immersion ion implantation and deposition (PIIID) on 9Cr18 bearing steel surface. Influences of working gas pressure and pulse width of the bias voltage on properties of the thin film were investigated. The chemical compositions of the as-deposited films were characterized by Raman spectroscopy. The micro-hardness, friction and wear behavior, corrosion resistance of the samples were evaluated, respectively. Compared with uncoated substrates, micro-hardness results reveal that the maximum is increased by 88.7%. In addition, the friction coefficient decreases to about 0.1, and the corrosion resistance of treated coupons surface are improved significantly.