Plasma nitriding of sintered AISI 316L at several temperatures

Samples of sintered AISI 316L stainless steel were plasma nitrided in a mixture of H-2-20% N-2, for 3 or 4 h. The treatment temperature was selected in 400-550 degreesC interval, in steps of 50 degreesC. X-ray diffraction (glancing angle geometry-GAXRD), conversion electron Mossbauer spectroscopy (CEMS), optical microscopy and Vickers microhardness were used as analytical techniques. For T greater than or equal to 500 degreesC and t = 4 h, a 40-mum layer is formed. The GAXRD results showed a transformation of the austenite gamma phase to the martensite in the sinterization process and showed as well, that the gamma' (Fe4N) phase is the predominant nitride besides small amounts of epsilon-Fe2N, gamma(N) CrN, Cr2O3 and the fcc nitrogen supersatured solid phase gamma(N). The CrN phase seems to decrease with temperature while the gamma(N) phase fraction is almost less than or equal to10%, independently on the temperature. The CEMS results indicated that while the gamma(N) fraction decreases with temperature of plasma nitriding, the gamma' fraction increases proportionally. (C) 2003 Elsevier B.V. All rights reserved.

Microstructural characterization of layers produced by plasma nitriding on austenitic and superaustenitic stainless steel grades

High chromium content is responsible for the formation of a protective passive surface layer on austenitic stainless steels (ASS). Due to their larger amounts of chromium, superaustenitic stainless steels (SASS) can be chosen for applications with higher corrosion resistance requirements. However, both of them present low hardness and wear resistance that has limited their use for mechanical parts fabrication. Plasma nitriding is a very effective surface treatment for producing harder and wear resistant surface layers on these steel grades, without harming their corrosion resistance if low processing temperatures are employed. In this work UNS S31600 and UNS S31254 SASS samples were plasma nitrided in temperatures from 400 °C to 500 °C for 5 h with 80% H 2-20% N2 atmosphere at 600Pa. Nitrided layers were analyzed by optical (OM) and transmission electron microscopy (TEM), x-ray diffraction (XRD), and Vickers microhardness testing. Observations made by optical microscopy showed that N-rich layers were uniform but their thicknesses increased with higher nitriding temperatures. XRD analyses showed that lower temperature layers are mainly composed by expanded austenite, a metastable nitrogen supersaturated phase with excellent corrosion and tribological properties. Samples nitrided at 400 °C produced a 5 μm thick expanded austenite layer. The nitrided layer reached 25 lm in specimens treated at 500 °C. There are indications that other phases are formed during higher temperature nitriding but XRD analysis was not able to determine that phases are iron and/or chromium nitrides, which are responsible for increasing hardness from 850 up to 1100 HV. In fact, observations made by TEM have indicated that formation of fine nitrides, virtually not identified by XRD technique, can begin at lower temperatures and their growth is affected by both thermodynamical and kinetics reasons. Copyright © 2012 by ASTM International.

Plasma nitriding and nitrocarburising of a supermartensitic stainless steel

Supermartensitic stainless steels (SMSSs) are a new generation of the classic 13%Cr martensitic steels, lower in carbon and with additional alloying of nickel and molybdenum offering better weldabilty and low temperature toughness. Several works have shown that plasma nitriding and nitrocarburising of stainless steels at low temperatures produces a hard surface layer which results in increased wear resistance. In this work, SMSS samples were plasma nitrided and nitrocarburised at 400, 450 and 500 °C. The plasma treated SMSS samples were characterised by means of optical microscopy, microhardness, X-ray diffraction and dry wear tests. The thickness of the layers produced increases as temperature is raised, for both plasma nitriding and nitrocarburising. X-ray diffraction demonstrates that the chromium nitride content grows with temperature for nitriding and nitrocarburising, which also showed increasing content of iron and chromium carbides with temperature. After plasma treating, it was found that the wear volume decreases for all temperatures and the wear resistance increased as the treatment temperature was raised. The main wear mechanism observed for both treated and untreated samples was grooving abrasion. © 2012 IHTSE Partnership Published by Maney on behalf of the Partnership.

Nanosized precipitates in H13 tool steel low temperature plasma nitriding

A comprehensive study of pulsed nitriding in AISI H13 tool steel at low temperature (400 degrees C) is reported for several durations. X-ray diffraction results reveal that a nitrogen enriched compound (epsilon-Fe2-3N, iron nitride) builds up on the surface within the first process hour despite the low process temperature. Beneath the surface, X-ray Wavelength Dispersive Spectroscopy (WDS) in a Scanning Electron Microscope (SEM) indicates relatively higher nitrogen concentrations (up to 12 at.%) within the diffusion layer while microscopic nitrides are not formed and existing carbides are not dissolved. Moreover, in the diffusion layer, nitrogen is found to be dispersed in the matrix and forming nanosized precipitates. The small coherent precipitates are observed by High-Resolution Transmission Electron Microscopy (HR-TEM) while the presence of nitrogen is confirmed by electron energy loss spectroscopy (EELS). Hardness tests show that the material hardness increases linearly with the nitrogen concentration, reaching up to 14.5 GPa in the surface while the Young Modulus remains essentially unaffected. Indeed, the original steel microstructure is well preserved even in the nitrogen diffusion layer. Nitrogen profiles show a case depth of about similar to 43 mu m after nine hours of nitriding process. These results indicate that pulsed plasma nitriding is highly efficient even at such low temperatures and that at this process temperature it is possible to form thick and hard nitrided layers with satisfactory mechanical properties. This process can be particularly interesting to enhance the surface hardness of tool steels without exposing the workpiece to high temperatures and altering its bulk microstructure. (c) 2012 Elsevier B.V. All rights reserved.

New insights into the mechanism of low-temperature active-screen plasma nitriding of austenitic stainless steel

Low-temperature active-screen plasma nitriding is an effective surface engineering technology to improve the wear and corrosion resistance of austenitic stainless steel through the formation of expanded austenite. The material sputtered from the active screen and redeposited on the specimens has been suggested to play an important role in the nitriding mechanism involved. This paper reports a patterned deposition layer, which is in correlation with the grain orientation of polycrystalline specimens. This has provided new insights into the nitriding mechanism. © 2012 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

On the fundamental mechanisms of active screen plasma nitriding

The nitriding mechanisms of conventional DC plasma treatments have been extensively studied and discussed, but no general agreement has been reached thus far. The sputtering and redeposition theory is among the most accepted ones but, even though this mechanism is feasible, its contribution to the nitriding effect is under question. Furthermore, the novel active screen plasma nitriding technique has been successful in treating samples left at floating potential, where sputtering can not be considered to play a major role. Therefore, it has been proposed that the material sputtered from the cathodic mesh of the active screen furnace (auxiliary cathode) and deposited onto the treated specimens is involved in the mass transfer of nitrogen. The contribution made by this transferred material is the focus of attention of the present study. The hardening effect on the treated specimens showed considerable correlation with the deposition layer, and the XRD analysis of this deposited material yielded possible FeN and FexN peaks. This finding supports the deposition of iron nitrides and their subsequent decomposition on the treated substrate as a mechanism of significance to the plasma nitriding treatments conducted in active screen experimental settings.

Study of active screen plasma processing conditions for carburising and nitriding austenitic stainless steel

Active screen (AS) is an advanced technology for plasma surface engineering, which offers some advantages over conventional direct current (DC) plasma treatments. Such surface defects and process instabilities as arcing, edge and hollow cathode effects can be minimised or completely eliminated by the AS technique, with consequent improvements in surface quality and material properties. However, the lack of information and thorough understanding of the process mechanisms generate scepticism in industrial practitioners. In this project, AISI 316 specimens were plasma carburised and plasma nitrided at low temperature in AS and DC furnaces, and the treated samples were comparatively analysed. Two diagnostic techniques were used to study the plasma: optical fibre assisted optical emission spectroscopy, and a planar electrostatic probe. Optimum windows of treatment conditions for AS plasma nitriding and AS plasma carburising of austenitic stainless steel were identified and some evidence was obtained on the working principles of AS furnaces. These include the sputtering of material from the cathodic mesh and its deposition on the worktable, the generation of additional active species, and the electrostatic confinement of the plasma within the operative volume of the furnace.

Sliding wear behavior of plasma nitrided Austenitic Stainless Steel Type AISI 316LN in the temperature range from 25 to 400 degrees C at 10(-4) bar

There is a research knowledge gap for the dry wear data of nitride treated Stainless Steel in high temperature and high vacuum environment. In order to fill this gap, plasma nitriding was done on austenitic Stainless Steel type AISI 316LN (316LN SS) and dry sliding wear tests have been conducted at 25 degrees C, 200 degrees C and 400 degrees C in high vacuum of 1.6 x 10(-4) bar. The two different slider material (316LN SS and Colmonoy) and two different sliding speeds (0.0576 m/s and 0.167 m/s) have been used. The tribological parameters such as friction coefficient, wear mechanism and volume of metal loss have been evaluated. Scanning Electron Microscopy (SEM) was used to study the surface morphology of the worn pins and rings. Electronic balancing machine was used to record the mass of metal loss during wear tests. The 2D optical profilometer was used to measure the depth of the wear track. The Plasma Nitride treated 316LN SS rings (PN rings) exhibit excellent wear resistance against 316LN SS pin and Colmonoy pin at all temperatures. However, PN ring vs. Colmonoy pin Pair shows better wear resistance than PN ring vs. 316LN SS pin Pair at higher temperature. (C) 2012 Elsevier B.V. All rights reserved.

Microstructure and dry sliding wear resistance evaluation of plasma nitrided austenitic stainless steel type AISI 316LN against different sliders

In this work, Plasma Nitriding was carried out at a temperature of 570 degrees C on nuclear grade austenitic stainless steel type AISI 316 LN (316LN SS) in a gas mixture of 20% N-2-80% H-2 to improve the surface hardness and thereby sliding wear resistance. The Plasma Nitride (PN) treated surface has been characterized by Vickers microhardness measurements, Scanning Electron Microscopic (SEM) examination, X-ray Diffraction (XRD) and sliding wear assessment. The average thickness of the PN layer was found to be 70 mu m. Microhardness measurements showed a significant increase in the hardness from 210 HV25g (unnitrided sample) to 1040 HV25g (Plasma Nitrided sample). The XRD reveals that PN layer consists of CrN, Fe4N and Fe3N phases along with austenite phase. The tribological parameters such as the friction coefficient and wear mechanism have been evaluated at ambient conditions for PN treated ring (PN ring) vs. ASTM A453 grade 660 pin (ASTM pin), PN ring vs. Nickel based alloy hard faced pin (Colmonoy pin), PN ring vs. 316LN SS pin and 316LN SS ring vs. 316LN SS pin. The wear tracks have been analyzed by SEM, Energy Dispersive X-ray Analysis (EDX) and Optical Profilometry. The untreated 316LN SS ring vs. 316LN SS pin produced severe wear and was characterized by a combination of delamination and adhesion wear mechanism, whereas wear mechanism of the PN rings reveals mild abrasion and a transfer layer from pin materials. (C) 2012 Elsevier B.V. All rights reserved.

Estudo das características físico-químicas e biológicas pela adesão de osteoblastos em superfícies de titânio modificadas pela nitretação em plasma

SILVA, J. S. P. Estudo das características físico-químicas e biológicas pela adesão de osteoblastos em superfícies de titânio modificadas pela nitretação em plasma. 2008. 119 f. Tese (Doutorado) - Faculdade de Medicina, Universidade de São Paulo. São Paulo, 2008.

Nitriding in cathodic cage of stainless steel AISI 316: influence of sample position

R.R.M. de Sousa et al. Nitriding in cathodic cage of stainless steel AISI 316: Influence of sample position. Vacuum, [s.l.], n.83, 2009. Disponivel em: plasma.ct.ufrn.br/index.php?id=5>. Acesso em: 04 out.2010.

A Comparati ve Study of Mechanical and Tribological Properties of AISI-304 and AISI-316 Submitted to Glow Discharge Nitriding

Mechanical and tribological properties of AISI 304 and AISI 316 stainless steels submitted to glow discharge ion nitriding are reported. The atmosphere was 20:80 - N2:H2 with substrate temperatures ranging from 300 to 500 °C. Treatment at 300 °C produced expanded austenite (γN) in both steels. Increasing the temperature, the phases γ′-Fe4N and ε- Fe2+xN were present and the latter is the major phase for AISI 304. At 500 °C, the CrN phase was also identified in both steels. Hardnesses of about 13-14 GPa at near surface regions were obtained in both steels. Moreover, AISI 316 nitrided at 500 °C has the deepest hard layer. Tribological tests showed that wear can be reduced by up to a factor of six after the nitriding processes, even for a working temperature of 300 °C. The profiles during and after nanoscratch tests did not reveal significant differences after nitriding processes in both steels.

Effect of cooling rate on properties of plasma nitrided AISI 1010 steel

In this work, AISI 1010 steel samples were plasma nitrided into 20% N 2 100 Pa and 400 Pa for N 2 and H 2 , respectively), temperatures of 500 and 580 °C, during 2 h. Three different procedures for cooling were accomplished after nitriding. In the first procedure the cooling occurred naturally, that is, the sample was kept on substrate holder. In the second one the sample was pulled off and cooling in a cold surface. Finally, in the third cooling process the sample was pulled off the substrate holder down into special reservoir filled with oil held at ambient temperature. The properties of the AISI 1010 steel samples were characterized by optical and electron microscopy, X-ray diffraction, Mössbauer spectroscopy and microhardness tests. Thermal gradient inside the sample kept on substrate holder during cooling process was measured by three inserted thermocouples at different depths. When samples were cooled rapidly the transformation of ϵ-Fe 2 − 3 N to γ′-Fe 4 N was inhibited. Such effect is indicated by the high concentration of ϵ-Fe compound zone. To get solid state solution of nitrogen in the diffusion zone, instead of precipitates of nitride phases, the cooling rate should be higher than a critical value of about 0.95 °C/s. When this value is reached at any depth of the diffusion zone, two distinct diffusion zones will appear. Temperature gradients were measured inside the samples as a consequence of the plasma treatment. It's suggested the need for standardization of the term “treatment temperature” for plasma treatment because different nitrided layer properties could be reported for the same “treatment temperature”.

Avaliação do desempenho do aço D6 tratado termicamente e netretado em plasma com gaiola catódica visando aplicação industrial

In this research there was an evaluation of the best conditions of nitriding in plasma within a cathodic cage at an atmosphere of 80% N2-20%H2 in samples of tool manganese steel AISI D6, cold working, treated thermally in the following conditions: tension relief, treated thermally to temperature of maximum heat, temperate heat and temperate and temperate heat. A pressure of 2.5mbar and temperatures of 400 and 300ºC com treatment time of two and three hours were used to evaluate its performance as cutting tool (punch) of bicycle backs. Hardness, micro-structural aspects (layer thickness, interface, grain size etc), and crystal phases on the surface were appraised. When treated to tension relief, thermally treated to maximum heat temperature, temperature and temperate heat, the samples presented hardness levels of 243HV, 231HV, 832HV, and 653HV, respectively. The best nitrification conditions were: four hours and 300ºC for heat samples. A superficial hardness of 1000HV and a 108µm thickness for the nitrided layer were found in these samples

Avaliação do desempenho do aço AISI D2 tratado termicamente e nitretado em plasma com gaiola catódica visando aplicação industrial

In the research, steel samples tool AISI D2, treated thermally, in the conditions: relief of tension, when maximum, seasoned and seasoned was treated thermally in the temperature of revenimento and revenida had been nitrited in plasma with cathodic cage, in atmosphere of 80%N2:20%H2. One used pressure of 2,5 mbar, 400 and 480°C temperatures with treatment time of 3 and 4 hours, with the objective to evaluate its performance in pipes cut tool. It was compared that the performance of the same steel when only thermally treated, both with tension relief. It was evaluated its hardness. Microstructural aspects (the layer thickness, interface, graisn size, etc) and crystalline phases on the surface. Besides, it was verified accomplishment possibility of nitriding simultaneous to annealing treatment. The tempering samples had presented hardness levels of 600 HV, while in nitrited samples these values had been 1100 HV