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.

Low-frequency, high-density, inductively coupled plasma sources : operation and applications

Operation regimes, plasma parameters, and applications of the low-frequency (∼500 kHz) inductively coupled plasma (ICP) sources with a planar external coil are investigated. It is shown that highly uniform, high-density (ne∼9×1012 cm-3) plasmas can be produced in low-pressure argon discharges with moderate rf powers. The low-frequency ICP sources operate in either electrostatic (E) or electromagnetic (H) regimes in a wide pressure range without any Faraday shield or an external multipolar magnetic confinement, and exhibit high power transfer efficiency, and low circuit loss. In the H mode, the ICP features high level of uniformity over large processing areas and volumes, low electron temperatures, and plasma potentials. The low-density, highly uniform over the cross-section, plasmas with high electron temperatures and plasma and sheath potentials are characteristic to the electrostatic regime. Both operation regimes offer great potential for various plasma processing applications. As examples, the efficiency of the low-frequency ICP for steel nitriding and plasma-enhanced chemical vapor deposition of hydrogenated diamond-like carbon (DLC) films, is demonstrated. It appears possible to achieve very high nitriding rates and dramatically increase micro-hardness and wear resistance of the AISI 304 stainless steel. It is also shown that the deposition rates and mechanical properties of the DLC films can be efficiently controlled by selecting the discharge operating regime.

Nitride synthesis using ammonia and hydrazine - a thermodynamic panorama

Because of the wide variety of projected applications of ultrapure nitrides in advanced technologies, there is interest in developing new cost-effective methods of synthesis. Explored in this study is the use of ammonia and hydrazine for the synthesis of nitrides from oxides, sulfides and chlorides. Even when the standard Gibbs energy change for the nitridation reactions involved are moderately positive, the reaction can be made to proceed by lowering the partial pressure of the product gas below its equilibrium value. Use of a metastable form of precursor in the nanometric size range is an alternative method to facilitate nitridation. Ellingham-Richardson-Jeffes diagrams are used for a panoramic presentation of the driving force for each set of reactions as a function of temperature. Oxides are the least promising precursors for nitride synthesis; sulfides offer a larger synthetic window for many useful nitrides such as BN, AlN, InN, VN, TiN, ThN and Si3N4. The standard Gibbs free energy changes for reactions involving chlorides with either ammonia or hydrazine are much more negative. Hydrazine is a more powerful nitriding agent than ammonia. The metastability of hydrazine requires that it be introduced into a reactor through a water-cooled lance. The use of volatile halides with ammonia or hydrazine offers the potential for synthesis of pure and doped nanocrystalline nitrides. Nitride thin films can also be prepared by suitable adaptations of the chloride route. (C) 2002 Kluwer Academic Publishers.

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.

In-situ synthesis of AlN powders and composite AlN powders with yttrium addition

Using Al-Mg and Al-Mg-Y alloys as raw materials and nitrogen as gas reactants, AIN powders and composite AIN powders by in-situ synthesis method were prepared. AIN lumps prepared by the nitriding of Al-Mg and Al-Mg-Y alloys have porous microstructure, which is favorable for pulverization. They have high purity, containing 1.23 % (mass fraction) oxygen impurity, and consisted of AIN single phase . The average particle size of AIN powders is 6.78 mum. Composite AlN powders consist of AlN phases and rare, earth oxide Y2O3 phase. The distribution of particle size of AIN powders shows two peaks. In view, of packing factor, AIN powders with such size distribution can easily be sintered to high density.

Synthesis of GaN nanorods with vertebra-like morphology

GaN nanorods with vertebra-like morphology were synthesized by nitriding Ga2O3/ZnO films at 1000 degrees C for 20min. Ga2O3 thin films and ZnO middle layers were pre-deposited in turn on Si(111) substrates by r.f. magnetron sputtering system. In the flowing ammonia ambient, ZnO was reducted to Zn and Zu sublimated at 1000 degrees C. Ga2O3 was reducted to Ga2O and Ga2O reacted with NH3 to synthesize GaN nanorods in the help of the sublimation of Zn. The structure and morphology of the nanorods were studied by X-ray diffraction (XRD) and scanning electron microscopy (SEM), The composition of GaN nanorods was studied by energy dispersive spectroscopy (EDS) and fourier transform infrared (FTIR) system.

X-ray diffraction, optical microscopy, and microhardness studies of gas nitrided titanium alloys and titanium aluminide

Thermochemical surface gas nitriding of ß21s, Timetal 205 and a Ti–Al alloy was conducted using differential scanning calorimeter equipment, in nominally pure nitrogen at 850 °C and 950 °C (ß21s), 730 °C and 830 °C (Timetal 205), and 950 °C and 1050 °C (Ti–Al) for 1 h, 3 h and 5 h. X-ray diffraction analyses showed new phases formed in the nitrided layer, depending on the alloy and the time and the temperature of nitriding. Microstructures were analyzed using optical microscopy. Cross-sectional microhardness profiles of cross-sectional samples after nitriding were obtained using a Knoop indenter.

Ammonia dissociation in the fluidised bed furnace

Ammonia dissociation is the controlling reaction for several important thermochemical heat treatment processes; nitriding, nitrocarburising (ferritic and austenitic) and carbonitriding. The fluidised bed furnace is a convenient and widely used medium for all of these treatments, yet understanding of the reaction in a fluidised bed context is minimal. This paper deals with the influence of process parameters on nitrogen activity aN; temperature, fluidising flowrate, ammonia inlet level, carbonaceous gas. Two basic behaviours were observed; inlet NH3-dependant and inlet NHr insensitive, with a transition region at intermediate temperatures. The nitrocarburising response of steel specimens was measured by optical microscopy of the layer thicknesses and glow discharge optical emission spectroscopy (GD-OES) determination of nitrogen depth-penetration profiles. aN was found by gas analysis of the exit stream ammonia with the aid of a dissociation burette.

Pure boron nitride nanowires produced from boron triiodide

A thick layer of pure boron nitride (BN) nanowires with a uniform diameter of 20 nm was synthesized for the first time using a CVD process with a new precursor of boron triiodide (BI3). Transmission electron microscopy revealed a nanocrystalline structure in the BN nanowires and the absence of any catalyst particle. Some BN nanowires self-assembled into thick threads up to several hundred micrometres long on top of the nanowire layer. The nitriding reactions and lack of catalyst suggest new formation mechanisms of the BN nanowires.

Synthesis of boron nitride nanotubes by boron ink annealing

Ball-milling and annealing is one effective method for the mass production of boron nitride nanotubes (BNNTs). We report that the method has been modified to a boron (B) ink annealing method. In this new process, the nanosize ball-milled B particles are mixed with metal nitrate in ethanol to form an ink-like solution, and then the ink is annealed in nitrogen-containing gas to form nanotubes. The new method greatly enhances the yield of BNNTs, giving a higher density of nanotubes. These improvements are caused by the addition of metal nitrate and ethanol, both of which can strongly boost the nitriding reaction, as revealed by thermogravimetric analysis. The size and structure of BNNTs can be controlled by varying the annealing conditions. This high-yield production of BNNTs in large quantities enables the large-scale application of BNNTs.

Microstructure and mechanical properties of nitrided and chromized short steel fiber reinforced aluminum based P/M composites

The present investigation is on the microstructure evolution and hardness of powder metallurgically processed Al- 0.5 wt.%Mg base 10 wt.% short steel fiber reinforced composites. The 0.38 wt.% C short steel fibers of average diameter 50µm and 500-800µm length were nitrided and chromized in a fluid bed furnace. Nitriding was carried out at 525°C for 90, 30 and 5 min durations. Chromizing was performed at 950°C for 53 and 7 min durations, using thermal reactive deposition (TRD) and diffusion technique. The treated fibers and resulting reaction interfaces were characterized using metallographic, microhardness and XRD techniques.

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.