The study of metal nitride layer formation by solid-state reactions

A new solid-state reaction to form metal nitrides has been investigated. It was confirmed that single phase chromium nitride is formed by a solid-state diffusion reaction between iron nitride and chromium chloride powders at temperatures between 570-700°C. The discovered reaction can be applied to form chromium nitride coatings on tool steels for metal forming applications.

Structural and mechanical properties of room temperature sputter deposited CrN coatings

Chromium nitride (CrN) thin films were deposited at room temperature on silicon and glass substrates using DC reactive magnetron sputtering in Ar + N-2 plasma. Structure and mechanical properties of these films were examined by using XRD, FESEM and nanoindentation techniques. XRD studies revealed that films are of mixed phase at lower nitrogen partial pressure (P-N2) and single phase at higher (P-N2). Microscopy results show that the films were composed of non-equiaxed columns with nanocrystallite morphology. The hardness and elastic modulus of the films increase with increasing nitrogen partial pressure (P-N2). A maximum hardness of similar to 29 GPa and elastic modulus of 341 GPa were obtained, which make these films useful for several potential applications. (C) 2012 Elsevier Ltd. All rights reserved.

Weldability of duplex stainless steel

Duplex stainless steels (DSSs) have many advantages due to the unique structural combination of ferrite and austenite grains. The structural change of these materials is very complex during welding, and it deteriorates the functional properties. This research investigates different welding processes such as laser beam, resistance, tungsten inert gas, friction stir, submerged arc, and plasma arc weldings considering the research available in the literature. The welding mechanism, change of material structure, and control parameters have been analyzed for every welding process. This analysis clearly shows that DSS melts in all most all welding processes, but the thermal cycle and maximum heat input are different. This difference affects the resulting structure and functional properties of the weld significantly.

Aging behaviour of 25Cr-17Mn high nitrogen duplex stainless steel

The precipitation behaviour of a nickel free stainless steel containing 25% chromium, 17% manganese and 0.54% nitrogen, with duplex ferritic-austenitic microstructure, was studied using several complementary techniques of microstructural analysis after aging heat treatments between 600 and 1 000 degrees C for periods of lime between 15 and 6 000 min. During aging heat treatments, ferrite was decomposed into sigma phase and austenite by a eutectoid reaction, like in the Fe-Cr-Ni duplex stainless steel. Chromium nitride precipitation occurred in austenite, which had a high nitrogen supersaturation. Some peculiar aspects were observed in this austenite during its phase transformations. Chromium nitride precipitation occurred discontinuously in a lamellar morphology, such as pearlite in carbon steels. This kind of precipitation is not an ordinary observation in duplex stainless steels and the high levels of nitrogen in austenite can induce this type of precipitation, which has not been previously reported in duplex stainless steels. After chromium nitride precipitation in austenite, it was also observed sigma phase formation near the cells or colonies of discontinuously precipitated chromium nitride. Sigma phase formation was made possible by the depletion of nitrogen in those regions. Time-temperature-transformation (precipitation) diagrams were determined.

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.

Influence of chromium concentration on the optical-electronic properties of ruby microstructures

Films of amorphous aluminium nitride (AlN) were prepared by conventional radio frequency sputtering of an Al + Cr target in a plasma of pure nitrogen. The Cr-to-Al relative area determines the Cr content, which remained in the similar to 0-3.5 at% concentration range in this study. Film deposition was followed by thermal annealing of the samples up to 1050 degrees C in an atmosphere of oxygen and by spectroscopic characterization through energy dispersive x-ray spectrometry, photoluminescence and optical transmission measurements. According to the experimental results, the optical-electronic properties of the Cr-containing AlN films are highly influenced by both the Cr concentration and the temperature of the thermal treatments. In fact, thermal annealing at 1050 degrees C induces the development of structures that, because of their typical size and distinctive spectral characteristics, were designated by ruby microstructures (RbMSs). These RbMSs are surrounded by a N-rich environment in which Cr(3+) ions exhibit luminescent features not present in other Cr(3+)-containing systems such as ruby, emerald or alexandrite. The light emissions shown by the RbMSs and surroundings were investigated according to the Cr concentration and temperature of measurement, allowing the identification of several Cr(3+)-related luminescent lines. The main characteristics of these luminescent lines and corresponding excitation-recombination processes are presented and discussed in view of a detailed spectroscopic analysis.

Influence of chromium content on the dry machining performance of cathodic arc evaporated TiA1N coatings

Physical vapour deposition (PVD) titanium aluminium nitride coated cutting tools are used extensively in global manufacturing for reducing production costs and improving productivity in a number of aggressive metal-cutting operations, namely, dry and high-speed machining. In this investigation, the performance of Ti1−xAlxN and Ti1−x−yAlxCryN coatings was assessed on Co-HSS twist drills used to machine grey cast iron. The failure criterion for drills was defined as a critical sized flank wear land at the outer corners of the drills. Using this criterion, the average tool life of uncoated twist drills was increased by factors of 2.5, 3.0 and 3.0 by Ti0.59Al0.41N, Ti0.27Al0.19Cr0.54N and Ti0.21Al0.14Cr0.65N coatings, respectively. Notwithstanding the similar increase in average tool life, the Ti1−x−yAlxCryN coatings produced more consistent results than the Ti1−xAlxN coated drills with standard deviations of 67, 3 and 19 holes, respectively. This result has significant practical implications in manufacturing, since drills are not replaced on an individual basis, but rather on a preset tool change frequency. The present paper discusses the performance of Ti1−xAlxN and Ti1−x−yAlxCryN coated drills in terms of average and practical drill life and concludes with remarks on the characterisation of PVD coatings and their significance on the performance of Co-HSS twist drills when dry machining grey cast iron.

Transition of chromium oxyhydroxide nanomaterials to chromium oxide : a hot stage Raman spectroscopic study

The transition of disc-like chromium hydroxide nanomaterials to chromium oxide nanomaterials has been studied by hot stage Raman spectroscopy. The structure and morphology of α-CrO(OH) synthesised using hydrothermal treatment was confirmed by X-ray diffraction and transmission electron microscopy. The Raman spectrum of α-CrO(OH) is characterised by two intense bands at 823 and 630 cm-1 attributed to ν1 CrIII-O symmetric stretching mode, bands at 1179 cm-1 attributed to CrIII-OH δ deformation modes. No bands are observed above 3000 cm-1. The absence of characteristic OH vibrational bands may be due to short hydrogen bonds in the α-CrO(OH) structure. Upon thermal treatment of α-CrO(OH), new Raman bands are observed at 599, 542, 513, 396, 344 and 304 cm-1, which are attributed to Cr2O3. This hot-stage Raman study shows that the transition of α-CrO(OH) to Cr2O3 occurs before 350 °C.

Transition of synthetic chromium oxide gel to crystalline chromium oxide : a hot stage Raman spectroscopic study

Chromium oxide gel material was synthesised and appeared to be X-ray amorphous. The changes in the structure of the synthetic chromium oxide gel were investigated using hot-stage Raman spectroscopy based upon the results of thermogravimetric analysis. The thermally decomposed product of the synthetic chromium oxide gel in nitrogen atmosphere was confirmed to be crystalline Cr2O3 as determined by the hot-stage Raman spectra. Two bands were observed at 849 and 735 cm-1 in the Raman spectrum at 25 °C, which were attributed to the symmetric stretching modes of O-CrIII-OH and O-CrIII-O. With temperature increase, the intensity of the band at 849 cm-1 decreased, while the band at 735 cm-1 increased. These changes in intensity are attributed to the loss of OH groups and formation of O-CrIII-O units in the structure. A strongly hydrogen bonded water H-O-H bending band was found at 1704 cm-1 in the Raman spectrum of the chromium oxide gel, however this band shifted to around 1590 cm-1 due to destruction of the hydrogen bonds upon thermal treatment. Six new Raman bands were observed at 578, 540, 513, 390, 342 and 303 cm-1 attributed to the thermal decomposed product Cr2O3. The use of the hot-stage Raman microscope enabled low-temperature phase changes brought about through dehydration and dehydroxylation to be studied.

The effect of hexagonal boron nitride additive on the effectiveness of grease-based lubrication of a steel surface

Purpose: The purpose of this paper is to study the sliding and the vibrating fretting tests mechanism of h-BN micro-particles when used as a lubricating grease-2 additive. Design/methodology/approach: The fretting tests were conducted on steel/steel contacts using both vibrating fretting apparatus and the shaftsleeve slide fitted tester. The wear scars were characterized with profilometry. The tribological properties of grease-2 compounded with h-BN additive were also compared to those obtained for the commercial product Militec-4. Findings: The experiment showed significant differences between the results obtained from the vibrating fretting and the shaft-sleeve sliding fitted tests. Adding h-BN to the lubricant leads to a better performance in the shaft-sleeve slide regime than in the steel/steel vibrating test condition. Originality/value: The results of the experimental studies demonstrate the potential of h-BN as an additive for preventing fretting sliding, and can very useful for further application of compound grease-2 with h-BN additive in industrial equipment.