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.     

Laser quenching of plasma nitrided 30CrMnSiA steel

30CrMnSiA steel has been commonly used in many industrial applications owing to its excellent mechanical properties. However, raw 30CrMnSiA steel cannot meet the requirements of practical application, such as high surface hardness and superior wear resistance. In practice, plasma nitriding (PN) is usually conducted to strengthen the surface properties of this steel. However conventional plasma nitriding (PN) technique is always hindered by diffusion kinetics. Alternatively, the process of laser quenching (LQ) has been utilized as a unique rapid method for tailoring the surface microstructure and chemical composition to improving the mechanical properties of steels. In the present study, a laser quenching technique (LQ) is utilized as subsequent procedure of typical plasma nitriding treatment process (PN) to improve the surface properties of 30CrMnSiA steel. The microstructure and properties of such layer are compared with those obtained by PN or LQ treatment. OM, XRD, SEM and EDS analysis are conducted for microstructure observation, phase identification, and estimating the nitrogen concentration, respectively. Microhardness tester and pin-on-disc tribometer are used to investigate the mechanical properties of the modified layers. Laser quenching of plasma nitrided (PN + LQ) 30CrMnSiA steel results in great increase in the thickness and hardness of the modified layer comparing with the PN and LQ treatment due to the reduction of eutectoid point caused by introduction of nitrogen. The mechanism is also discussed systematically based on the phase diagram in the paper. Moreover, the layer treated by PN + LQ process exhibits better wear resistance than the PN treated specimen. This is attributed to the formation of retained austenite and Fe₃O₄ according to the XRD analysis, which is beneficial to the improvement of impact toughness and the lubrication action during sliding.     

Characteristics of the nitrided layer formed on AISI 304 austenitic stainless steel by high temperature nitriding assisted hollow cathode discharge

A series of experiments have been conducted on AISI 304 stainless steel using a hollow cathode discharge assisted plasma nitriding apparatus. Specimens were nitrided at high temperatures (520–560 °C) in order to produce nitrogen expanded austenite phase within a short time. The nitrided specimen was characterized by scanning electron microscopy, X-ray diffraction, X-ray photoelectron spectroscopy, potentiodynamic polarization and microhardness tester. The corrosion properties of nitrided samples were evaluated using anodic polarization tests in 3.5% NaCl solution. The nitrided layer was shown to consist of nitrogen expanded austenite and possibly a small amount of CrN precipitates and iron nitrides. The results indicated that rapid nitriding assisted hollow cathode discharge not only increased the surface hardness but also improved the corrosion resistance of the untreated substrate.     

Microstructure and mechanical properties of the modified layer obtained by low temperature plasma nitriding of nanocrystallized 18Ni maraging steel

In the present study, low temperature plasma nitriding of nanocrystallized 18Ni maraging steel has been carried out at 360 °C from 1 to 24 h in a mixed gas of 25%N₂ + 75%H₂. The surface phase constitutions and microstructures of the nitrided layer have been investigated by X-ray diffraction analysis, transmission electron microscopy and optical microscopy. Nanoindentation and microhardness tests have been performed to determine the surface hardness and the hardness profile in the nitrided layer. The plasticity of the nitrided surface has been analyzed based on the nanoindentation results. The results show that at the initial stage of nitriding, the surface phase consists of a solid solution of nitrogen in α-Fe, and nanoscale nitrides and aging phase are formed with increasing of treatment time. The surfaces nitrided for 8 and 16 h possess the highest hardness. The plasticity factor calculations suggest that the nitrided surfaces have a good wear resistance and possess excellent plasticity.     

The study of tribological and corrosion behavior of plasma nitrided 34CrNiMo6 steel under hot and cold wall conditions

This paper reports on a comparative study of tribological and corrosion behavior of plasma nitrided 34CrNiMo6 low alloy steel under modern hot wall condition and conventional cold wall condition. Plasma nitriding was carried out at 500 °C and 550 °C with a 25% N₂ + 75% H₂ gas mixture for 8 h. The wall temperature of the chamber in hot wall condition was set to 400 °C. The treated specimens were characterized by using scanning electron microscopy (SEM), X-ray diffraction (XRD), microhardness and surface roughness techniques. The wear test was performed by pin-on-disc method. Potentiodynamic polarization and electrochemical impedance spectroscopy (EIS) tests were also used to evaluate the corrosion resistance of the samples. The results demonstrated that in both nitriding conditions, wear and corrosion resistance of the treated samples decrease with increasing temperature from 500 °C to 550 °C. Moreover, nitriding under hot wall condition at the same temperature provided slightly better tribological and corrosion behavior in comparison with cold wall condition. In consequence, the lowest friction coefficient, and highest wear and corrosion resistance were found on the sample treated under hot wall condition at 500 °C, which had the maximum surface hardness and ε-Fe_2–3N phase.     

Mössbauer spectroscopy study on the corrosion resistance of plasma nitrided ASTM F138 stainless steel in chloride solution

Plasma nitriding of ASTM F138 stainless steel samples has been carried out using dc glow discharge under 80% H₂–20% N₂ gas mixture, at 673 K, and 2, 4, and 7 h time intervals, in order to investigate the influence of treatment time on the microstructure and the corrosion resistance properties. The samples were characterized by scanning electron microscopy, glancing angle X-ray diffraction and conversion electron Mössbauer spectroscopy, besides electrochemical tests in NaCl aerated solution. A modified layer of about 6 μm was observed for all the nitrided samples, independent of nitriding time. The X-ray diffraction analysis shows broad γ_N phase peaks, signifying a great degree of nitrogen supersaturation. Besides γ_N, the Mössbauer spectroscopy results indicated the occurrence of γ′ and ε phases, as well as some other less important phases. Corrosion measurements demonstrate that the plasma nitriding time affects the corrosion resistance and the best performance is reached at 4 h treatment. It seems that the ε/γ′ fraction ratio plays an important role on the resistance corrosion. Additionally, the Mössbauer spectroscopy was decisive in this study, since it was able to identify and quantify the iron phases that influence the corrosion resistance of plasma nitrided ASTM F138 samples.     

Rotating bending fatigue properties of two case hardening steels after nitriding treatment

Fatigue properties of two Al-containing steels have been investigated by rotating bending fatigue tests. Results show that the fatigue limits (the fatigue strength at 10⁷ cycles) were improved remarkably by plasma nitriding due to the high hardness of 1000 Hv and compressive stress of 400 MPa in the nitrided layer. Scanning electron microscopic observations show that after nitriding the fatigue crack initiation sites moved from the surface flaws or near-surface matrix into the AlN inclusions at around the case-core interface. Degassing treatment can increase the fatigue limit because it prevented fatigue crack initiation at AlN inclusions due to the reduced [N] contents and refined inclusion size.     

Comparison of high temperature wear behaviour of plasma sprayed WC–Co coated and hard chromium plated AISI 304 austenitic stainless steel

The wear behaviour of plasma sprayed coating and hard chrome plating on AISI 304 austenitic stainless steel substrate is experimentally investigated in unlubricated conditions. Experiments were conducted at different temperatures (room temp, 100 °C, 200 °C and 300 °C) with 50 N load and 1 m/s sliding velocity. Wear tests were carried out by dry sliding contact of EN-24 medium carbon steel pin as counterpart on a pin-on-disc wear testing machine. In both coatings, specimens were characterised by hardness, microstructure, coating density and sliding wear resistance. Wear studies showed that the hard chromium coating exhibited improved tribological performance than that of the plasma sprayed WC–Co coating. X-ray diffraction analysis (XRD) of the coatings showed that the better wear resistance at high temperature has been attributed to the formation of a protective oxide layer at the surface during sliding. The wear mechanisms were investigated through scanning electron microscopy (SEM) and XRD. It was observed that the chromium coating provided higher hardness, good adhesion with the substrate and nearly five times the wear resistance than that obtained by uncoated AISI 304 austenitic stainless steel.     

Wear assessment of plasma nitrided AISI H11 steel

Plasma nitriding is one of the effective methods for improvement of the hardness, wear and corrosion resistance of steels. In this research AISI H11 hot working tool steel was plasma nitrided in various gas mixtures for different times and temperatures. The morphology, size and composition of nitride nanoparticles formed on the surface of the specimens were investigated using scanning electron microscopy (SEM), atomic force microscopy (AFM), X-ray diffraction (XRD). The wear behavior of plasma nitrided samples was studied by means of unlubricated pin-on-disc method under constant load of 80 N, sliding speed of 1 m/s, sliding distance of 2000 m at room temperature. The results showed plasma nitriding process improved the wear behavior of H11 steel. The increase in time and temperature of plasma nitriding decreased the hardness and increased the wear weigh loss of the specimens.     

Significant acceleration of nitriding kinetics in pure iron by pressurized gas treatment

The effect of nitriding pressure on the formation of nitrides and the nitriding kinetics in pure iron were investigated by applying pressurized gas nitriding at 500 °C for 5 h. Increasing the nitriding pressure from 1 atm (conventional nitriding condition) to 5 atm significantly increased the nitrided layer thickness from about 210 μm to 1100 μm. Furthermore, it was found that the constituents of the compound layer can be controlled by changing the nitriding pressure. These improvements are related to the fast reaction rates and high inward diffusive flux of nitrogen during the pressurized gas nitriding.     

Surface hardness improvement of plasma-sprayed AISI 316L stainless steel coating by low-temperature plasma carburizing

Low-temperature carburizing below 773 K of austenite stainless steel can produce expanded austenite, known as S-phase, where surface hardness is improved while corrosion resistance is retained. Plasma-sprayed austenitic AISI 316L stainless steel coatings were carburized at low temperatures to enhance wear resistance. Because the sprayed AISI 316L coatings include oxide layers synthesized in the air during the plasma spraying process, the oxide layers may restrict carbon diffusion. We found that the carbon content of the sprayed AISI 316L coatings by low-temperature carburizing was less than that of the AISI 316L steel plates; however, there was little difference in the thickness of the carburized layers. The Vickers hardness of the carburized AISI 316L spray coating was above 1000 HV and the amount of specific wear by dry sliding wear was improved by two orders of magnitude. We conclude that low-temperature plasma carburizing enabling the sprayed coatings to enhance the wear resistance to the level of carburized AISI 316L stainless steel plates. As for corrosion resistance in a 3.5 mass% NaCl solution, the carburized AISI 316L spray coating was slightly inferior to the as-sprayed AISI 316L coating.     

Structure and wear resistance of the composite layers produced by glow discharge nitriding and PLD method on AISI 316L austenitic stainless steel

The rapid technical development enhances the demands on constructional materials in terms of their resistance to frictional wear, resistance to corrosion and erosion, high hardness, high tensile and fatigue strength. These demands can be satisfied by e.g. applying various surface engineering techniques that permit to modify the microstructure, phase and chemical composition of the surface layers of the treated parts. A prospective line of the development of surface engineering is the production of composite layers by combining various surface engineering methods. The paper presents the results of examinations of the phase composition and frictional wear resistance of the layers produced by hybrid processes, i.e. such that combined glow discharge assisted nitriding performed at 450 °C and 550 °C with a pulsed laser deposition of boron nitride coatings (PLD method). It has been shown that the boron nitride coatings formed on nitrided AISI 316L steel increase its frictional wear resistance.     

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.     

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.     

Microstructural characteristics and evolution of Ti2AlN/TiAl composites with a network reinforcement architecture during reaction hot pressing process

The microstructural evolution of TiAl matrix composites with a novel network distribution of Ti₂AlN particle reinforcement was studied. The composites were synthesized by reaction hot pressing method using pure Al and nitrided Ti powders as initial materials. Pure Ti powders nitrided at 600 °C for a certain time in an atmosphere of flowing nitrogen turned into new compound Ti(N) powders, which have a shell of titanium nitrides (such as TiN, Ti₂N and TiN_0.3) and a core of Ti–N solid solution. Within the composites synthesized, Ti₂AlN particles, produced by in situ reaction, exhibit a network distribution. The special shell/core structure of the compound Ti(N) powders contributes to this architecture. Nitriding time of the Ti powders greatly affects the microstructure of the composites. Increasing the nitriding time is beneficial to the distribution of Ti₂AlN particles in a continuous network form. However, too long nitriding time can result in the aggregation of Ti₂AlN particles and thus destroy the uniformity of the network structure. The in-situ synthesized Ti₂AlN/TiAl composites with uniform network structure have a superior mechanical property, and their compressive strengths at 800 °C and 1000 °C are 1112 MPa and 687 MPa, respectively.     

Evaluation of the effects of plasma nitriding temperature and time on the characterisation of Ti 6Al 4V alloy

The effects of plasma nitriding (PN) temperature and time on the structural and tribological characterisation of Ti 6Al 4V alloy were investigated. PN processes under gas mixture of N₂/H₂ = 4 were performed at temperatures of 700, 750, 800 and 850 °C for duration of 2, 5 and 10 h. Cross section and surface characterisation were evaluated by means of SEM, AFM, XRD and microhardness test techniques. Dry wear tests were performed using a pin on disc machine. Mass loss and coefficient of friction were measured during the wear tests. Three distinguished structures including of a compound layer (constituted of δ-TiN and ɛ-Ti₂N), an aluminium-rich region and a diffusion zone (interstitial solid solution of nitrogen in titanium) were detected at the surface of plasma nitrided Ti 6Al 4V alloy. These structures increased surface hardness of Ti 6Al 4V alloy significantly and gradually distributed the hardness from the surface to the substrate. The "surface hardness", "surface roughness", "wear resistance" and "coefficient of friction" of the alloy were increased due to plasma nitriding process. Moreover, rising both process temperature and time led to increasing of "layers thicknesses", "surface hardness", "surface roughness", "dynamic load-ability" and "wear resistance" of Ti 6Al 4V alloy.     

Effect of phase transformation and intermetallic compounds on the microstructure and tensile strength properties of diffusion-bonded joints between Ti–6Al–4V and AISI 304L

The occurrence of a phase transformation and the effect of intermetallic compounds on the microstructure and tensile strength properties of diffusion-bonded (DB) joints between Ti–6Al–4V and AISI 304L were studied in the temperature range of 875–950 °C with an interval of 25 °C, a bonding time of 60 min and pressures of 4 MPa and 8 MPa. A maximum tensile strength of 242.6 MPa, was observed for diffusion-bonded joints that were processed at a temperature of 900 °C, bonded for 60 min at a pressure of 4 MPa and annealed for 2 h at 750 °C. Optical microscopy and scanning electron microscopy (SEM) were used to examine the grain growth and the fine details of the interface structure. Energy dispersive X-ray analysis (EDAX) and X-ray diffraction analysis (XRD) revealed the existence of intermetallic compounds and corroborated the phase transformation.     

Cracking in a multiple gas-nitrided H13 aluminum extrusion mandrel

A failure analysis was carried out to investigate the root cause of cracking in a mandrel used in a local aluminum extrusion plant. The tool was made of AISI H13 and received multiple gas-nitriding case hardening during its service life. The scraped mandrel showed several microcracks in the filleted bridges. Izod impact tests were conducted over a range of temperatures (23–550 °C) for un-nitrided and single nitrided H13 specimens to examine the possible susceptibility of the tool steel to temper embrittlement. The effect of single and multiple nitriding cycles on the surface fracture resistance of H13 specimens was characterized using Vickers indentation test. The impact test results showed a low impact-energy regime at temperatures at or below 350 °C and a high impact-energy regime at higher temperatures. Temper embrittlement was ruled out as a likely cause of cracking since the extrusion temperature of 425 °C is within the high impact-energy regime. Vickers indentations typically showed sharp cracks initiated from the corners of the indentation for a sample taken from the mandrel. No cracks emanated from indentations applied on un-nitrided and single-nitrided specimens. Crack initiation in the mandrel is primarily attributed to multiple gas-nitriding and the subsequent thickening of the brittle nitrided layer which promoted brittle crack initiation in the mandrel bridges under the applied extrusion pressure.     

An investigation of nitrided layer prepared by direct current nitrogen arc discharge

A simple direct current (DC) nitrogen arc discharge method is presented, which allows for in situ nitriding of titanium at atmospheric pressure. The microstructure and microhardness of the nitrided layer and effects of the arc discharge current were investigated. The nitrided layer was mainly composed of TiN dendrites and small amounts of TiN_0.3. The density and size of the TiN dendrites gradually decreased from the surface towards the titanium substrate. The layer had a good adhesion with titanium. With an increase of the arc discharge current from 40 to 80 A, the TiN dendrites coarsened, the layer thickness and amount of TiN increased and the layer hardness enhanced. The nitrided layer with the highest hardness value of 1600 HV and thickness of 1800 μm was obtained for an arc discharge current of 80 A.