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.

Synthesis and characterization of nano silicon and titanium nitride powders using atmospheric microwave plasma technique

We have demonstrated a simple, scalable and inexpensive method based on microwave plasma for synthesizing 5 to 10 g/h of nanomaterials. Luminescent nano silicon particles were synthesized by homogenous nucleation of silicon vapour produced by the radial injection of silicon tetrachloride vapour and nano titanium nitride was synthesized by using liquid titanium tetrachloride as the precursor. The synthesized nano silicon and titanium nitride powders were characterized by XRD, XPS, TEM, SEM and BET. The characterization techniques indicated that the synthesized powders were indeed crystalline nanomaterials.

Approaches to alpha-amino acids via rearrangement to electron-deficient nitrogen: Beckmann and Hofmann rearrangements of appropriate carboxyl-protected substrates

The titled approaches were effected with various 2-substituted benzoylacetic acid oximes 3 (Beckmann) and 2-substituted malonamic acids 9 (Hofmann), their carboxyl groups being masked as a 2,4,10-trioxaadamantane unit (an orthoacetate). The oxime mesylates have been rearranged with basic Al2O3 in refluxing CHCl3, and the malonamic acids with phenyliodoso acetate and KOH/MeOH. Both routes are characterized by excellent overall yields. Structure confirmation of final products was conducted with X-ray diffraction in selected cases. The final N-benzoyl and N-(methoxycarbonyl) products are alpha-amino acids with both carboxyl and amino protection; hence, they are of great interest in peptide synthesis.

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 vitro bioactivity and cytocompatibility properties of spark plasma sintered HA-Ti composites

The present study reports the results of the detailed in vitro bioactivity and cytocompatibility properties of the hydroxyapatite (HA) and the HA-titanium (HA-Ti) composite with varying amount of Ti (5, 10, and 20 wt %), densified using spark plasma sintering process (SPS). Using this technique and tailoring suitable processing parameters, it has been possible to retain both HA and Ti in the sintered ceramics. Importantly, the uniquely designed SPS processing with suitably chosen parameters enables in achieving better mechanical properties, such as higher indentation fracture toughness (similar to 1.5 MPa m1/2) in HA-Ti composites compared with HA. X-ray diffraction and scanning electron microscopic (SEM) observations reveal good bioactivity of the HA-Ti composites with the formation of thick, flaky, and porous apatite layer when immersed in simulated body fluid at 37 degrees C and pH of 7.4. Atomic absorption spectroscopic analysis of the simulated body fluid solution reveals dynamic changes in Ca+2 ion concentration with more dissolution of Ca+2 ion from the HA-20Ti composite. However, the measurements with inductively coupled plasma spectrometer do not record dissolution of Ti+4 ions. Transmission electron microscopic analysis indicates weak crystalline nature of the apatite and confirms the formation of fine-scale apatite crystals. MTT assay, fluorescence, and SEM study demonstrate good cell viability and cell adhesion/proliferation of the Saos -2 cells, cultured on the developed composites under standard culture condition, and the difference in cell viability has been discussed in reference to substrate composition and roughness. Overall, HA-Ti composites exhibit comparable and even better in vitro bioactivity and cytocompatibility properties than HA. (c) 2012 Wiley Periodicals, Inc. J Biomed Mater Res Part B: Appl Biomater, 2013.

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.

Substrate impact on the growth of InN nanostructures by droplet epitaxy

The substrate effect on InN nanostructures grown by droplet epitaxy has been studied. InN nanostructures were fabricated on Si(111), silicon nitride/Si(111), AlN/Si(111) and Ge(100) substrates by droplet epitaxy using an RF plasma nitrogen source. The morphologies of InN nanostructures were investigated by field emission scanning electron microscopy (FESEM). The chemical bonding configurations of InN nanostructures were examined by x-ray photoelectron spectroscopy (XPS). Photoluminescence spectrum slightly blue shifted compared to the bulk InN, indicating a strong Burstein-Moss effect due to the presence of high electron concentration in the InN dots.

Densification kinetics, phase assemblage and hardness of spark plasma sintered Cu-10 wt% TiB2 and Cu-10 wt% TiB2-10 wt% Pb composites

The present work demonstrates the synthesis of Cu-10 wt% TiB2 composites with a theoretical density of more than 90% by tailoring the spark plasma sintering (SPS) conditions in the temperature range of 400-700 degrees C. Interestingly, 10 wt% Pb addition to Cu-10 wt% TiB2 lowers the sinter density and the difference in the densification behavior of the investigated compositions was discussed in reference to the current profile recorded during a SPS cycle. The sintering kinetics and phase assemblage were also discussed in reference to surface melting of the constituents prior to bulk melting temperature, temperature dependent wettability of Pb on Cu, diffusion kinetics of Cu as well as the formation of various oxides. An important result is that a high hardness of around 2 GPa and relative density close to 92% qtheoretical was achieved for the Cu-10 wt% TiB2-10 wt% Pb composite, and such a combination has never been achieved before using any conventional processing route.

On the densification mechanisms and properties of Cu-Pb and Cu-Pb-TiB2 nanocomposites densified using spark plasma sintering

The present paper is aimed to understand the sub-processes triggered by rapid heating during spark plasma sintering as well as to assess the extent to which densification and properties of metallic materials can be enhanced using such superfast consolidation process. Using nanocrystalline Cu-Pb as a model system, the influence of Pb as well as TiB2 addition on the densification mechanisms and properties are discussed. Importantly, a high hardness of 2 GPa is achieved in Cu-based nanocomposites. (C) 2013 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

Spark plasma sintering may lead to phase instability and inferior mechanical properties: A case study with TiB2

In contrast to the widely reported beneficial aspects of spark plasma sintering in developing materials with better properties, we report here two interesting aspects recorded with difficult-to-sinter titanium diboride: (a) in situ formation of second phase (TiB) and (b) inferior hardness (by similar to 30%) and elastic modulus (by similar to 20%) for spark plasma sintered TiB2, with respect to hot pressed TiB2. The formation of TiB is discussed with reference to the enhanced reaction kinetics in the presence of pulsed electric field. (C) 2013 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

Flow cytometry analysis of human fetal osteoblast fate processes on spark plasma sintered hydroxyapatite-titanium biocomposites

Hydroxyapatite (HA)-based biocomposites have been widely investigated for a multitude of applications and these studies have been largely driven to improve mechanical properties (toughness and strength) without compromising cytocompatibility properties. Apart from routine cell viability/proliferation analysis, limited efforts have been made to quantify the fate processes (cell proliferation, cell cycle, and cell apoptosis) of human fetal osteoblast (hFOB) cells on HA-based composites, in vitro. In this work, the osteoblast cell fate process has been studied on a model hydroxyapatite-titanium (HA-Ti) system using the flow cytometry. In order to retain both HA and Ti, the novel processing technique, that is, spark plasma sintering, was suitably adopted. The cell fate processes of hFOBs, as evaluated using a flow cytometry, revealed statistically insignificant differences among HA-10 wt % Ti and HA and control (tissue culture polystyrene surface) in terms of osteoblast apoptosis, proliferation index as well as division index. For the first time, we provide quantified flow cytometry results to demonstrate that 10 wt % Ti additions to HA do not have any significant influence on the fate processes of human osteoblast-like cells, in vitro.

Dielectric and electrical conductivity properties of multi-stage spark plasma sintered HA-CaTiO3 composites and comparison with conventionally sintered materials

One of the different issues limiting the wider application of monolithic hydroxyapatite (HA) as an ideal bone replacement material is the lack of reasonably good electrical transport properties. The comprehensive electrical property characterization to evaluate the efficacy of processing parameters in achieving the desired combination of electroactive properties is considered as an important aspect in the development of HA-based bioactive material. In this perspective, the present work reports the temperature (RT-200 degrees C) and frequency (100 Hz-1 MHz) dependent dielectric properties and AC conductivity for a range of HA-CaTiO3 (HA-CT) composites, densified using both conventional pressureless sintering in air as well as spark plasma sintering in vacuum. Importantly, the AC conductivity of spark plasma sintered ceramics similar to upto 10(-5) (Omega cm)(-1)] are found to be considerably higher than the corresponding pressureless sintered ceramics similar to upto 10(-8) (Omega cm)(-1)]. Overall, the results indicate the processing route dependent functional properties of HA-CaTiO3 composites as well as related advantages of spark plasma sintering route. (C) 2013 Elsevier Ltd. All rights reserved.

Growth and properties of nonpolar a-plane GaN grown on r-sapphire by plasma assisted molecular beam epitaxy

The growth of nonpolar a- plane (1 1 -2 0) orientation of the GaN epilayers were confirmed by high resolution x-ray diffraction studies. An in-plane orientation relationship was found to be 0 0 0 1] GaN parallel to -1 1 0 1] sapphire and -1 1 0 0] GaN parallel to 1 1 -2 0] sapphire. SEM image shows the reasonably smooth surface. The photoluminescence spectrum shows near band emission (NBE) at 3.439 eV. The room temperature I-V characteristics of Au/a-GaN schottky diode performed. The Schottky barrier height (phi(b)) and the ideality factor (eta) for the Au/a-GaN schottky diode found to be 0.50 eV and 2.01 respectively.

Gas Phase Oxygen Quenching Studies of Ketone Tracers for Laser-Induced Fluorescence Applications in Nitrogen Bath Gas

In this paper we report the quantitative oxygen quenching effect on laser-induced fluorescence of acetone, methyl ethyl ketone, and 3-pentanone at low pressures (approximate to 700torr) with oxygen partial pressures up to 450torr. Nitrogen was used as a bath gas in which these molecular tracers were added in different quantities according to their vapor pressure at room temperature. These tracers were excited by using a frequency-quadrupled, Q-switched, Nd:YAG laser (266nm). Stern-Volmer plots were found to be linear for all the tracers, suggesting that quenching is collisional in nature. Stern-Volmer coefficients (k(sv)) and quenching rate constants (k(q)) were calculated from Stern-Volmer plots. The effects of oxygen on the laser-induced fluorescence of acetone, methyl ethyl ketone, and 3-pentanone were compared with each other. Further, the Smoluchowski theory was used to calculate the quenching parameters and compared with the experimental results.

RF plasma MOCVD of Y2O3 thin films: Effect of RF self-bias on the substrates during deposition

Yttrium oxide (Y203) thin films have been deposited by radio frequency plasma assisted metal organic chemical vapor deposition (MOCVD) process using (2,2,6,6-tetramethy1-3,5-heptanedionate) yttrium (commonly known as Y(thd)3) precursor in a plasma of argon and oxygen gases at a substrate temperature of 350 C. The films have been deposited under influence of varying RF self-bias (-50 V to 175 V) on silicon, quartz, stainless steel and tantalum substrates. The deposited coatings are characterized by glancing angle X-ray diffraction (GIXRD), Fourier transform infrared spectroscopy (FTIR), X-ray photoelectron spectroscopy (XPS), spectroscopic ellipsometry and scanning electron microscopy (SEM). GIXRD and FTIR results indicate deposition of Y2 03 (BCC structure) in all cases. However, XPS results indicate nonstoichiometric cubic phase deposition on the surface of deposited films. The degree of nonstoichiometry varies with bias during deposition. Ellipsometry results indicate that the refractive index for the deposited films is varying from 1.70 to 1.83 that is typical for Y203. All films are transparent in the investigated wavelength range 300-1200 nm. SEM results indicate that the microstructure of the films is changing with applied bias. Results indicate that it is possible to deposit single phase cubic Y203 thin films at low substrate temperature by RF plasma MOCVD process. RF self-bias that decides about the energy of impinging ions on the substrates plays an important role in controlling the texture of deposited Y203 films on the substrates. Results indicate that to control the structure of films and its texture, it is important to control the bias on the substrate during deposition. The films deposited at high bias level show degradation in the crystallinity and reduction of thickness. (C) 2013 Elsevier B.V. All rights reserved.