Combined effect of shot peening,subcritical austenitic nitriding,and cryo-treatment on surface modification of AISI 4140 steel

Shot peening is a simple but effective severe plastic deformation process to synthesize ultrafine grains in micro- to nanometer range on metallic surfaces. In this work, shot peening on AISI 4140 steel specimens was done in a novel centrifugal air blast shot peening reactor with shot velocity of 5.8?m/s for 3?h. Characterization of the shot peened surface (XRD, micro-hardness, SEM, and TEM) showed that surface undergoes significant plastic deformation with marked increase in microstrain of lattice, dislocation density, and surface hardness. XRD profiles and TEM analysis confirmed formation of ultrafine grain structure in the nanometer range. These specimens were then subjected to austenitic nitriding at 610°C for 4?h followed by cryo-treatment at???185°C for 32?h. Characterization of pre-shot peened nitrided and cryo-treated surfaces showed that there was marked improvement in surface hardness (from 695 to 797 HV_0.05) and effective case depth (from 19 to 54?µm) in comparison with un-shot peened nitrided and cryo-treated specimens. It was demonstrated that presence of ultrafine grain structure and austenitic phase during nitriding plays synergetic role to improve content and diffusion kinetics of nitrogen in AISI 4140 steel surface.     

The investigation of mechanical properties of ion-nitrided AISI 5140 low-alloy steel

The ion nitriding behavior of AISI 5140 low-alloy steel was investigated 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, and 3 N₂/H₂). The ion nitriding properties of AISI 5140 steel have been assessed by evaluating fatigue strength, hardness profile, compound layer thickness, and case depth by using a rotating bending fatigue machine, a microhardness tester, and scanning electron microscopy (SEM) with energy dispersive spectrometry (EDS). It was found that ion nitriding improves the fatigue strength, which depends on increasing the case depth, but the compound layer does not have a dominant effect on the fatigue strength. After the fatigue tests, sections of ion-nitrided specimens were observed to have failed by the fish eye phenomenon with the fatigue cracks originating from nonmetallic inclusions.     

Investigation of the formation of Al,Fe, N intermetallic phases during Al pack cementation followed by plasma nitriding on plain carbon steel

Plain carbon steels are not suitable for nitriding as they form an extremely brittle case that spalls off readily, and the hardness increment of the diffusion zone is small. In this research, the effect of plasma nitriding time and temperature variation on the microstructure of the pack cemented aluminized plain carbon steel is investigated. All samples were aluminized at 900 °C for 2 h; the aluminized samples were subsequently plasma nitrided at 500 °C, 550 °C and 600 °C for 2.5, 5, 7.5 and 10 h. The phases formed on the sample surface were detected by X-ray diffraction (XRD). The cross section and samples surface were investigated by optical and scanning electron microscopy (SEM). Microhardness test was conducted to determine hardness change from the surface to the sample core. Results showed that by aluminizing the steel, Fe₃Al phases as well as Fe–Al solid solution were formed on the surface and some aluminum rich precipitates were formed in solid solution grain boundaries. Plasma nitriding of the aluminized layer caused the formation of aluminum and iron nitride (AlN, Fe₄N) on the sample surface. Consequently, surface hardness was improved up to about eight times. By increasing the nitriding temperature and time, aluminum-rich precipitates dissociated. Moreover, due to the diffusion of nitrogen through aluminized region during ion nitriding, iron and aluminum nitrides were formed in aluminized grain boundaries. Increasing nitriding time and temperature lead to the growth of these nitrides in the grain boundaries of the substrate. This phenomenon results in the increment of sample hardness depth. Plasma nitriding of aluminized sample in low pressure chamber with nitrogen and hydrogen gas mixture reduced surface aluminum oxides which were formed in aluminizing stage.     

表面纳米化预处理对316L不锈钢渗氮层摩擦学性能的影响

为改善奥氏体不锈钢的表面硬度和耐磨性,采用超声滚压与离子渗氮复合工艺对316L不锈钢表面进行了表面强化处理。利用扫描电镜(SEM)、硬度计、X射线衍射仪(XRD)和能谱仪以及摩擦磨损试验机等测定了渗氮层的硬度、深度、含氮量和物相组成,研究了表面晶层组织结构对离子渗氮行为和渗氮层在润滑油条件下摩擦学性能的影响。结果表明:直接渗氮和超声滚压/渗氮试样表层组织均由S、γ'、ε和Cr N相组成,渗氮层厚度均为20μm,直接渗氮层以S相为主,超声滚压后渗氮层以ε和γ'相为主,组织结构较为致密;超声滚压/渗氮层的平均渗氮含量是直接渗氮层的2.88倍,摩擦系数降低了0.04,显微硬度和耐磨性是直接渗氮层的1.15倍和2.76倍;超声滚压处理诱使316L不锈钢表面形成的纳米晶层组织结构增强了渗氮试样表面的催渗效能和对渗氮层的支撑强度,超声滚压后渗氮试样的表面耐磨性能最好。     

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

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

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

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

Einfluss unterschiedlicher Oberflächenzustände vor dem Plasmanitrieren auf Eigenschaften und Zerspanungsverhalten des Schnellarbeitsstahls S 6‐5‐2

Surface states and wear behavior of drills of ground, sandblasted and plasmanitrided samples and drills made of AISI M2 high speed steel In the present work the effect of different surface conditions on plasma nitriding response of AISI M2 high speed steel was investigated. The plasma nitriding of ground and sandblasted samples and drills was performed at temperatures of 400°C and 500°C for two gas mixtures: 5 vol.% N₂ and 76 vol.% N₂ in hydrogen. Surface layers were characterized before and after plasma nitriding concerning the microstructure, roughness, microhardness, chemical composition, phase composition and residual stress states. Machining tests were carried out with drills during which drilling forces and flank wear have been measured. A significant effect of the surface state prior to nitriding on residual stress states and the properties of the nitrided layer and untreated core has been observed. Thinner nitrided layers on ground and sandblasted samples were attributed to high compressive residual stress states and a stress affected diffusion of nitrogen and carbon. In the machining tests, sandblasted drills exhibited the best performance. Lower nitrogen concentrations in the gas atmosphere without the formation of a compound layer gave the lowest drill flank wear for sandblasted surfaces while higher nitrogen concentrations led to a reduction of drilling forces and torque.     

Influence of nitriding on corrosion resistance of martensitic X17CrNi16‐2 stainless steel

Nitriding increases surface hardness and improves wear resistance of stainless steels. However, nitriding can sometimes reduce their corrosion resistance. In this paper, the influence of nitriding on the corrosion resistance of martensitic stainless steel was investigated. Plasma nitriding at 440 °C and 525 °C and salt bath nitrocarburizing were carried out on X17CrNi16‐2 stainless steel. Microhardness profiles of the obtained nitrided layers were examined. Phase composition analysis and quantitative depth profile analysis of the nitrided layers were preformed by X‐ray diffraction (XRD) and glow‐discharge optical emission spectrometry (GD‐OES), respectively. Corrosion behaviour was evaluated by immersion test in 1% HCl, salt spray test in 5% NaCl and electrochemical corrosion tests in 3.5% NaCl aqueous solution. Results show that salt bath nitrocarburizing, as well as plasma nitriding at low temperature, increased microhardness without significantly reducing corrosion resistance. Plasma nitriding at a higher temperature increased the corrosion tendency of the X17CrNi16‐2 steel.     

Influence of the microstructure on the corrosion resistance of plasma‐nitrided austenitic stainless steel 304L and 316L

Austenitic stainless steels are widely used in medical and food industries because of their excellent corrosion resistance. However, they suffer from weak wear resistance due to their low hardness. To improve this, plasma nitriding processes have been successfully applied to austenitic stainless steels, thereby forming a thin and very hard diffusion layer, the so‐called S‐phase. In the present study, the austenitic stainless steels AISI 304L and AISI 316L with different microstructures and surface modifications were used to examine the influence of the steel microstructure on the plasma nitriding behavior and corrosion properties. In a first step, solution annealed steel plates were cold‐rolled with 38% deformation degree. Then, the samples were prepared with three kinds of mechanical surface treatments. The specimens were plasma nitrided for 360 min in a H₂–N₂ atmosphere at 420 °C. X‐ray diffraction measurements confirmed the presence of the S‐phase at the sample surface, austenite and body centered cubic (bcc)‐iron. The specimens were comprehensively characterized by means of optical microscopy, scanning electron microscopy, glow discharge optical emission spectroscopy, X‐ray diffraction, surface roughness and nano‐indentation measurements to provide the formulation of dependencies between microstructure and nitriding behavior. The corrosion behavior was examined by potentio‐dynamic polarization measurements in 0.05 M and 0.5 M sulfuric acid and by salt spray testing.     

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

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

Mechanical and structural properties of AISI 1015 carbon steel nitrided after warm rolling

Nitriding is usually applied to alloyed steels with the scope of increasing their surface hardness and wear resistance. Warm working has been found to produce a fine-grained microstructure, which makes possible further treatment of low carbon steels. In combination with a low temperature thermochemical treatment, such as nitriding, warm working can be used to produce machine parts with a though core and with a hard, wear resistant surface layer. This paper presents a study of mechanical and structural properties of AISI 1015 carbon steel nitrided after warm rolling. The rolling was performed in the following conditions: temperature 670–550°C, rolling speed 1.39 s^-1 and deformation ratio 36.4%. After rolling, the samples were reheated to 550°C for a duration varying from a few minutes to 10 hours. The microstructural changes were assessed by light microscopy and quantitative microscopy analysis. Warm rolled samples were ion nitrided at 510–520°C in dissociated ammonia. The microstructure was analyzed by scanning electron microscopy and the mechanical properties were evaluated by tensile testing, surface hardness and friction coefficient measurements. Prior application of warm rolling makes possible (in the sense that is a viable solution) the ion nitriding of low carbon steels in order to produce machine parts with improved mechanical properties in the core (due to warm rolling) and longer service life (due to ion nitriding).     

Nitriding of AISI M2 tool steel in an inductive r.f. plasma

The nitriding of AISI M2 tool steel in an inductive r.f. plasma was investigated. The plasma was sustained with a 27.12 MHz generator in gas mixtures of N₂ and H₂ at a pressure of 10 mbar. The ion nitriding was performed at a net r.f. power of 400 W at substrate temperatures of 450–500 °C. X-ray diffraction studies of the treated samples revealed that the most efficient formation of nitride phases was observed in samples nitrided in a pure N₂ plasma. As a result of the ion nitriding the surface hardness was substantially increased from a Vickers hardness VHN of 290 kgf mm^-2 for untreated samples to a maximum VHN of 1200 kgf mm^-2 for samples treated in a plasma sustained in a gas mixture with N₂:H₂ = 1:1.     

Formation of carbide layers on AISI H13 and D2 steels by treatment in molten borax containing dissolved both Fe–Nb and Fe–Ti powders

In this work, AISI H13 and D2 tool steels were treated in molten borax, containing dissolved ferro-niobium, ferro-titanium and aluminum, at 1020 °C for 4 h. Samples were characterized by scanning electron microscopy (SEM), energy dispersive X-ray spectrometry (EDS), X-ray diffraction (XRD) and Vickers microhardness. Well defined layers were obtained with excellent thickness regularity. For the AISI H13 steel the layer measured 9 μm and for the AISI D2 steel the layer thickness was 18 μm. Their microhardness values were at about 2600 HV_0.050. The layers consisted of niobium carbide according to XRD analysis. EDS results showed the predominance of niobium and absence of iron in the layers on both steels. The presence of titanium was detected, just in small amounts, in the region of the layer next to substrate.     

Duplex surface treatment of AISI 1045 steel via plasma nitriding of chromized layer

In this work AISI 1045 steel were duplex treated via plasma nitriding of chromized layer. Samples were pack chromized by using a powder mixture consisting of ferrochromium, ammonium chloride and alumina at 1273 K for 5 h. The samples were then plasma-nitrided for 5 h at 803 K and 823 K, in a gas mixture of 75%N₂ + 25%H₂. The treated specimens were characterized by scanning electron microscopy (SEM), X-ray diffraction (XRD) analysis and Vickers micro-hardness test. The thickness of chromized layer before nitriding was about 8 μm and it was increased after plasma nitriding. According to XRD analysis, the chromized layer was composed of chromium and iron carbides. Plasma nitriding of chromized layer resulted in the formation of chromium and iron nitrides and carbides. The hardness of the duplex layers was significantly higher than the hardness of the base material or chromized layer. The main cause of the large improvement in surface hardness was due to the formation of Cr_xN and Fe_xN phases in the duplex treated layers. Increasing of nitriding temperature from 803 to 823 K enhanced the formation of CrN in the duplex treated layer and increased the thickness of the nitrided layer.     

Nitriding of stainless steel in plasma of a pulse electron beam

The formation of a hardened layer with low-temperature (400°C)nitriding of grade 12Kh18N10T stainless steel in plasma of a pulse electron beam which is generated under continuous and pulse conditions at equal average current (2.6 A) and electron energy (200 eV) is studied. In spite of intense ion sputtering of the surface during the pulse, both nitriding conditions yielded equal quantities of thickness and hardness of the layer, which indicated that neutral atomic nitrogen plays a main role during nitriding.     

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

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

The effect of temperature on plasma nitriding behaviour of DIN 1.6959 low alloy steel

A series of experiments have been conducted on DIN 1.6959 low-alloy steel using a 5 kVA DC plasma nitriding apparatus with the aim of elucidating the role of treatment temperature in plasma nitriding process. Treatments were carried out in 75%N₂-25%H₂ atmosphere of 4 mbar for 5 h at temperatures ranging from 350 to 550 °C. Optical microscopy, scanning electron microscopy, X-ray diffraction, along with surface roughness and microhardness measurements were utilized to characterize the treated samples. The depth, microstructure, hardness profile and phase constituents of the nitrided layers as well as the surface roughness of the samples were assessed as a function of treatment temperature. The results suggested that the compound layers were mostly dual phase consisting of gamma prime and epsilon iron nitride phases. Increasing treatment temperature increases compound layer and diffusion layer thicknesses. However, maximum surface hardness and roughness were found on the samples treated at 500 and 550 °C, respectively.     

Stress induced and concentration dependent diffusion of nitrogen in plasma nitrided austenitic stainless steel

The nitrogen transport mechanism in austenitic stainless steel during plasma nitriding at moderate temperatures (around 400 °C) is considered by stress induced diffusion model. The model involves diffusion of nitrogen in presence of internal stresses gradient induced by penetrating nitrogen as the next driving force of diffusion after concentration gradient. Furthermore, in the present work it was found that nitrogen diffusion coefficient vary with nitrogen concentration according to well-known Einstein-Smoluchowski relation D(C_N) = f(1/C_N). Nitrogen depth profiles in nitided AISI 316L steel at T = 400 °C for 1, 3 and 8 h calculated on the basis of this model are in good agreement with experimental nitrogen profiles. The dependencies of nitrogen flux and nitriding time on nitrogen concentration, nitrogen surface concentration and penetration depth are analyzed by proposed model. It is shown that, with the increase of nitriding time the compositionally-induced stresses and thickness of stressed steel layer increases.     

Microstructure and mechanical properties of copper–titanium–nitrogen multiphase layers produced by a duplex treatment on C17200 copper–beryllium alloy

In this study, a copper–titanium–nitrogen multiphase coating was fabricated on the surface of C17200 copper–beryllium alloy by deposition and plasma nitriding in order to improve the surface mechanical properties. The phase composition, microstructure and microhardness profiles of the as-obtained multiphase coating were characterized by X-ray diffractometer (XRD), scanning electron microscopy (SEM) and Vickers microhardness measurements, respectively. Pin-on-disk tribometer and SEM equipped with energy dispersive spectrometer (EDS) were applied to measure tribological properties and analyze wear mechanisms involved. The XRD results show that the phase composition changes with nitriding temperature. The Ti₂N layer is replaced by a Cu–Ti intermetallic layer when the nitriding temperature is higher than 700 °C. The Cu/Ti ratio in the multiphase coatings remains at a constant value of 2:1 due to the incorporation of nitrogen atoms. The surface hardness achieves a maximum value of 983 HV at 650 °C, and decreases as the nitriding temperature increases. The increased hardness corresponds to the improved wear resistance and decreased frictional coefficient and the surface hardness is proportional to the wear rates. The wear mechanism depends on the phase composition of the multiphase coatings. With the nitriding temperature increasing, the oxidative wear mechanism changes to adhesive and abrasive mode.     

Verschleißschutz und Korrosionsbeständigkeit von austenitischem Stahl durch Plasmadiffusions behandlung

In this paper, we report on a series of experiments designed to study the influence of plasma nitriding on the mechanical properties and the corrosion resistance of austenitic stainless steel. Plasma nitriding experiments were conducted on AISI 304L steel in a temperature range of 375‐475°C using pulsed‐DC plasma with different N ₂‐H ₂ gas mixtures and treatment times. First of all, the formation and the microstructure of the modified layer will be highlighted followed by the results of hardness measurement, adhesion testing, wear resistance and fatigue life tests. In addition the corrosion resistance of the modified layer is described. The microhardness after plasma nitriding is increased by a factor of five compared to the untreated material. The adhesion is examined by Rockwell indentation and scratch test. No delamination of the treated layer could be observed. The wear rate after plasma nitriding is significantly reduced compared to the untreated material. Plasma nitriding produces compressive stress within the modified layer. This treatment improves the fatigue life which can be raised by a factor of ten at a low stress level. The results show that plasma nitriding of austenitic stainless steel is a suitable process for improving the mechanical and the technological properties without significantly effecting the excellent corrosion resistance of this material.