Plasma-polymerized acetylene nanofilms modified by nitrogen ion implantation

Thin films were prepared by plasma enhanced chemical vapour deposition (PECVD) from a mixture of acetylene and argon, and post deposition-treated by plasma immersion ion implantation (PIII). The effect of PIII on the nanofilms properties was evaluated as a function of treatment time. The average thickness and roughness were diminished upon PIII. On the other hand, hardness (0.7-3.9 GPa) and elastic modulus (29-54 GPa) increased upon 60 min of ion bombardment. Such results are ascribed mainly to the densification of the film structure caused by the increment in the crosslinking degree with increasing the energy deposited in the films. Wettability of the samples, investigated by contact angle measurements, was reduced (from 64 to 21°) right after PIII. This result, attributed to the introduction of polar groups in the film structure, was not preserved as the sample was aged in atmosphere. After aging, contact angles were larger than 70° but still smaller than 90°. Although the wettability has decreased with aging, the hydrophilic character of the samples was preserved. For certain treatment times, nitrogen PIII turned the plasma-polymerized acetylene films smoother, denser, mechanically and tribologicaly more resistant than the as-deposited material. © 2013 Elsevier B.V.

Cyclic Fatigue Resistance of Rotary Nickel-Titanium Instruments Submitted to Nitrogen Ion Implantation

Introduction: The aim of this study was to assess cyclic fatigue resistance in rotary nickel-titanium instruments submitted to nitrogen ion implantation by using a custom-made cyclic fatigue testing apparatus. Methods: Thirty K3 files, size #25, taper 0.04, were divided into 3 experimental groups as follows: group A, 12 files exposed to nitrogen ion implantation at a dose of 2.5 x 10(17) ions/cm(2), accelerating voltage of 200 kV, currents of 1 mu A/cm(2), 130 degrees C temperature, and vacuum conditions of 10 x 10(-6) torr for 6 hours; group B, 12 nonimplanted files; and group C, 6 files submitted to thermal annealing for 6 hours at 130 degrees C. One extra file was used for process control. All files were submitted to a cyclic fatigue test that was performed with an apparatus that allowed the instruments to rotate freely, simulating rotary instrumentation of a curved canal (40-degree, 5-mm radius curve). An electric motor handpiece was used with a contra-angle of 16:1 at an operating speed of 300 rpm and a torque of 2 N-cm. Time to failure was recorded with a stopwatch in seconds and subsequently converted to number of cycles to fracture. Data were analyzed with the Student t test (P < .05). Results: Ion-implanted instruments reached significantly higher cycle numbers before fracture (mean, 510 cycles) when compared with annealed (mean, 428 cycles) and nonimplanted files (mean, 381 cycles). Conclusions: Our results showed that nitrogen ion implantation improves cyclic fatigue resistance in rotary nickel-titanium instruments. Industrial implementation. of this surface modification technique would produce rotary nickel-titanium instruments with a longer working life. (J Endod 2010;36:1183-1186)

Corrosion resistance enhancement of SAE 1020 steel after Chromium implantation by nitrogen ion recoil

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Effects of nitrogen ion irradiation on plasma polymerized films produced from titanium tetraiso pro poxide-oxygen-helium mixtures

In this work films were produced by the plasma enhanced chemical vapor deposition (PECVD) of titanium tetraisopropoxide-oxygen-helium mixtures and irradiated with 150 keV singly-charged nitrogen ions (N(+)) at fluences, phi, between 10(14) and 10(16) cm(-2). Irradiation resulted in compaction, which reached about 40% (measured via the film thickness) at the highest fluence. Infrared reflection-absorption spectroscopy (IRRAS) revealed the presence of Ti-O bonds in all films. Both O-H and C-H groups were present in the as-deposited films, but the density of each of these decreased with increasing phi and was absent at high phi, indicating a loss of hydrogen. X-ray photoelectron spectroscopy (XPS) analyses revealed an increase in the C to Ti atomic ratio as phi increased, while the O to Ti ratio hardly altered, remaining at around 2.8. The optical gap of the films, derived from data obtained by ultraviolet-visible spectroscopy (UVS), remained at about 3.6 eV for all fluences except the highest, for which an abrupt fall to around 1.0 eV was observed. For the irradiated films, the electrical conductivity, measured using the two-point method, showed a systematic increase with increasing phi. (c) 2008 Elsevier B.V. All rights reserved.

Effect of Nitrogen Ion Implantation on the Flexibility of Rotary Nickel-Titanium Instruments

Introduction: The aim of this study was to assess the effect of nitrogen ion implantation on the flexibility of rotary nickel-titanium (NiTi) instruments as measured by the load required to bend implanted and nonimplanted instruments at a 30 degrees angle. Methods: Thirty K3 files, size #40, 0.02 taper and 25-mm length, were allocated into 2 groups as follows: group A, 15 files exposed to nitrogen ion implantation at a dose of 2.5 x 10(17) ions/cm(2), voltage 200 KeV, current density 1 mu A/cm(2), temperature 130 degrees C, and vacuum conditions of 10 x 10(-6) mm Hg for 6 hours; and group B, 15 nonimplanted files. One extra file was used for process control. All instruments were subjected to bend testing on a modified troptometer, with measurement of the load required for flexure to an angle of 30 degrees. The Mann-Whitney U test was used for statistical analysis. Findings with P <.05 were considered significant. Results: The mean load required to bend instruments at a 30 degrees angle was 376.26 g for implanted instruments and 383.78 g for nonimplanted instruments. The difference was not statistically significant. Conclusions: Our findings show that nitrogen ion implantation has no appreciable effect on the flexibility of NiTi instruments. (J Endod 2012;38:673-675)

Modification of surface properties of Ti-16Si-4B powder alloy by plasma immersion ion implantation

Results of the surface modification of Ti-16Si-4B powder alloy by nitrogen ion implantation are presented, together with the experimental description of the preparation of that powder by high-energy ball milling and hot pressing. The phase structure, chemical composition and morphology of sample surfaces were observed by utilizing X-ray diffractometer (XRD), atomic force microscope (AFM) and scanning electron microscopy (SEM). A tribological characterization was carried out with a ball-on-disc tribometer and an SEM. Friction coefficient is compared with the one obtained for Ti-6Al-4V alloy and the wear scars characterized by SEM/EDS (energy dispersive spectroscopy). The concentration profile of the detected elements have been investigated using Auger electron spectroscopy (AES) depth profiling. Our results show that a shallow implanted layer of oxygen and nitrogen ions were obtained at the Ti-16Si -4B alloy surface, sufficient to modify slightly its tribological properties. Crown Copyright (C) 2011 Published by Elsevier Ltd. All rights reserved.

X-ray photoelectron spectroscopy analysis of zirconium nitride-like films prepared on Si(100) substrates by ion beam assisted deposition

Thin zirconium nitride films were prepared on Si(l 00) substrates at room temperature by ion beam assisted deposition with a 2 keV nitrogen ion beam. Arrival rate ratios ARR(N/Zr) used were 0.19, 0.39, 0.92, and 1.86. The chemical composition and bonding structure of the films were analyzed with X-ray photoelectron spectroscopy (XPS). Deconvolution results for Zr 3d, Zr 3p(3/2), N 1s, O 1s, and C 1s XPS spectra indicated self-consistently the presence of metal Zr-0, nitride ZrN, oxide ZrO2, oxymnide Zr2N2O, and carbide ZrC phases, and the amounts of these compounds were influenced by ARR(N/Zr). The chemical composition ratio N/Zr in the film increased with increasing ARR(N/Zr) until ARR(N/Zr) reached 0.92, reflecting the high reactivity of nitrogen in the ion beam, and stayed almost constant for ARR(N/Zr) >= 1, the excess nitrogen being rejected from the growing film. A considerable incorporation of contaminant oxygen and carbon into the depositing film was attributed to the getter effect of zirconium. (C) 2007 Elsevier B.V. All rights reserved.

Surface Corrosion of Ti-16Si-4B Powder Alloy Implanted With Nitrogen by Plasma-Based Technique

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Modification of surface properties of Ti-16Si-4B powder alloy by plasma immersion ion implantation

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Study of magnetic field enhanced plasma immersion ion implantation in Silicon

A comparison between experimental measurements and numerical calculations of the ion current distribution in plasma immersion ion implantation (PIII) with external magnetic field is presented. Later, Silicon samples were implanted with nitrogen ion to analyze the effect on them. The magnetic field considered is essentially non-uniform and is generated by two magnetic coils installed on vacuum chamber. The presence of both, electric and magnetic field in PIII create a crossed ExB field system, promoting drift velocity of the plasma around the target. The results found shows that magnetized electrons drifting in ExB field provide electron-neutral collision. The efficient ionization increases the plasma density around the target where a magnetic confinement is formed. As result, the ion current density increases, promoting significant changes in the samples surface properties, especially in the surface wettability.

Amorphous silicon carbonitride films modified by plasma immersion ion implantation

Amorphous silicon carbonitride (a-SiCN:H) films were deposited from hexamethyldisilazane (HMDSN) organic compounds via radio-frequency (RF) glow discharges. Afterwards the films were bombarded, from 15 to 60 min, with nitrogen ions using Plasma Immersion Ion Implantation (PIII) technique. X-ray photoelectron spectroscopy (XPS) showed that O-containing groups increased, while C-C and/or C-H groups decreased with treatment time. This result indicates chemical alterations of the polymeric films with the introduction of polar groups on the surface, which changes the surface wettability. In fact, the hydrophobic nature of a-SiCN:H films (contact angle of 100 degrees) was changed by nitrogen ion implantation and, and after aging in atmosphere air, all samples preserved the hydrophilic character (contact angle <80 degrees) independently of treatment time. The exposure of the films to oxygen plasma was performed to evaluate the etching rate, which dropped from 24% to 6% while the implantation time increased from 15 to 60 min. This data suggests that Pill increased the film structure strength, probably due to crosslinking enhancement of polymeric chains. Therefore, the treatment with nitrogen ions via Pill process was effective to modify the wettability and oxidation resistance of a-SiCN:H films. (C) 2014 Elsevier Ltd. All rights reserved.

Superconductivity in metal-mixed ion-implanted polymer films

Ion implantation of normally insulating polymers offers an alternative to depositing conjugated organics onto plastic films to make electronic circuits. We used a 50 keV nitrogen ion beam to mix a thin 10 nm Sn/Sb alloy film into the subsurface of polyetheretherketone and report the low temperature properties of this material. We observed metallic behavior, and the onset of superconductivity below 3 K. There are strong indications that the superconductivity does not result from a residual thin film of alloy, but instead from a network of alloy grains coupled via a weakly conducting, ion-beam carbonized polymer matrix. (c) 2006 American Institute of Physics.

Investigation of the effects of low energy high dose ion bombardment in metals and compound semiconductors

The effect of low energy nitrogen molecular ion beam bombardment on metals and compound semiconductors has been studied, with the aim to investigate at the effects of ion and target properties. For this purpose, nitrogen ion implantation in aluminium, iron, copper, gold, GaAs and AIGaAs is studied using XPS and Angle Resolve XPS. A series of experimental studies on N+2 bombardment induced compositional changes, especially the amount of nitrogen retained in the target, were accomplished. Both monoenergetic implantation and non-monoenergetic ion implantation were investigated, using the VG Scientific ESCALAB 200D system and a d. c. plasma cell, respectively. When the samples, with the exception of gold, are exposed to air, native oxide layers are formed on the surfaces. In the case of monoenergetic implantation, the surfaces were cleaned using Ar+ beam bombardment prior to implantation. The materials were then bombarded with N2+ beam and eight sets of successful experiments were performed on each sample, using a rastered N2+ ion beam of energy of 2, 3, 4 and 5 keV with current densities of 1 μA/cm2 and 5 μA/cm22 for each energy. The bombarded samples were examined by ARXPS. After each complete implantation, XPS depth profiles were created using Ar+ beam at energy 2 ke V and current density 2 μA/cm2 . As the current density was chosen as one of the parameters, accurate determination of current density was very important. In the case of glow discharge, two sets of successful experiments were performed in each case, by exposing the samples to nitrogen plasma for the two conditions: at low pressure and high voltage and high pressure and low voltage. These samples were then examined by ARXPS. On the theoretical side, the major problem was prediction of the number of ions of an element that can be implanted in a given matrix. Although the programme is essentially on experimental study, but an attempt is being made to understand the current theoretical models, such as SATVAL, SUSPRE and TRIM. The experimental results were compared with theoretical predictions, in order to gain a better understanding of the mechanisms responsible. From the experimental results, considering possible experimental uncertainties, there is no evidence of significant variation in nitrogen saturation concentration with ion energy or ion current density in the range of 2-5 ke V, however, the retention characteristics of implantant seem to strongly depend on the chemical reactivity between ion species and target material. The experimental data suggests the presence of at least one thermal process. The discrepancy between the theoretical and experimental results could be the inability of the codes to account for molecular ion impact and thermal processes.

Nitrogen implantation of tool steels and engineering coatings

Ion implantation modifies the surface composition and properties of materials by bombardment with high energy ions. The low temperature of the process ensures the avoidance of distortion and degradation of the surface or bulk mechanical properties of components. In the present work nitrogen ion implantation at 90 keV and doses above 1017 ions/cm2 has been carried out on AISI M2, D2 and 420 steels and engineering coatings such as hard chromium, electroless Ni-P and a brush plated Co-W alloy. Evaluation of wear and frictional properties of these materials was performed with a lubricated Falex wear test at high loads up to 900 N and a dry pin-on-disc apparatus at loads up to 40 N. It was found that nitrogen implantation reduced the wear of AISI 420 stainless steel by a factor of 2.5 under high load lubricated conditions and by a factor of 5.5 in low load dry testing. Lower but significant reductions in wear were achieved for AISI M2 and D2 steels. Wear resistance of coating materials was improved by up to 4 times in lubricated wear of hard Cr coatings implanted at the optimum dose but lower improvements were obtained for the Co-W alloy coating. However, hardened electroless Ni-P coatings showed no enhancement in wear properties. The benefits obtained in wear behaviour for the above materials were generally accompanied by a significant decrease in the running-in friction. Nitrogen implantation hardened the surface of steels and Cr and Co-W coatings. An ultra-microhardness technique showed that the true hardness of implanted layers was greater than the values obtained by conventional micro-hardness methods, which often result in penetration below the implanted depth. Scanning electron microscopy revealed that implantation reduced the ploughing effect during wear and a change in wear mechanism from an abrasive-adhesive type to a mild oxidative mode was evident. Retention of nitrogen after implantation was studied by Nuclear Reaction Analysis and Auger Electron Spectroscopy. It was shown that maximum nitrogen retention occurs in hard Cr coatings and AISI 420 stainless steel, which explains the improvements obtained in wear resistance and hardness. X-ray photoelectron spectroscopy on these materials revealed that nitrogen is almost entirely bound to Cr, forming chromium nitrides. It was concluded that nitrogen implantation at 90 keV and doses above 3x1017 ions/cm2 produced the most significant improvements in mechanical properties in materials containing nitride formers by precipitation strengthening, improving the load bearing capacity of the surface and changing the wear mechanism from adhesive-abrasive to oxidative.

Implantação iônica por imersão em plasma - IIIP - de argônio, nitrogênio e hélio em hexametildissilazano polimerizado a plasma

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