Nanoindentation mechanical properties characterization of glassy polymeric carbon treated with ion beam

Phenolic resins when heat treated in inert atmosphere up to 1000 degreesC become glassy polymeric carbon (GPC), a chemically inert and biocompatible material useful for medical applications, such as in the manufacture of heart valves and prosthetic devices. In earlier work we have shown that ion bombardment can modify the surface of GPC, increasing its roughness. The enhanced roughness, which depends on the species, energy and fluence of the ion beam, can improve the biocompatibility of GPC prosthetic artifacts. In this work, ion bombardment was used to make a layer of implanted ions under the surface to avoid the propagation of microcracks in regions where cardiac valves should have pins for fixation of the leaflets. GPC samples prepared at 700 and 1500 degreesC were bombarded with ions of silicon. carbon, oxygen and gold at energies of 5, 6, 8 and 10 MeV, respectively, and fluences between 1.0 x 10(13) and 1.0 x 10(16) ions/cm(2). Nanoindentation hardness characterization was used to compare bombarded with non-bombarded samples prepared at temperatures up to 2500 degreesC. The results with samples not bombarded showed that the hardness of GPC increases strongly with the heat treatment temperature. Comparison with ion bombarded samples shows that the hardness changes according to the ion used, the energy and fluence. (C) 2002 Elsevier B.V. B.V. All rights reserved.

Effects of ion beam on nanoindentation characteristics of glassy polymeric carbon surface

Glassy polymeric carbon (GPC) is a useful material for medical applications due to its chemical inertness and biocompatible characteristics. Mitral and aortic and hydrocephalic valves are examples of GPC prosthetic devices that have been fabricated and commercialized in Brazil. In this work, ion beam was used to improve the mechanical characteristics of GPC surface and therefore to avoid the propagation of microcracks where the cardiac valves are more fragile. A control group of phenolic resin samples heat-treated at 300, 400, 700, 1000, 1500, and 2500 degrees C was characterized by measuring their hardness and Young's reduced elastic modulus with the depth of indentation. The control group was compared to results obtained with samples heat-treated at 700, 1000, and 1500 degrees C and bombarded with energetic ions of silicon, carbon, oxygen, and gold at energies of 5, 6, 8, and 10 MeV, respectively, with fluences between 10x10(13) and 10x10(16) ions/cm(2). GPC nonbombarded samples showed that hardness depends on the heat treatment temperature (HTT), with a maximum hardness for heat treatment at 1000 degrees C. The comparison between the control group and bombarded group also showed that hardness, after bombardment, had a greater increase for samples prepared at 700 degrees C than for samples prepared at higher temperatures. The Young's elastic modulus presents an exponential relationship with depth. The parameters obtained by fitting depend on the HTT and on the ion used in the bombardment more than on energy and fluence. The hardness results show clearly that bombardment can promote carbonization, increase the linkage between the chains of the polymeric material, and promote recombination of broken bonds in lateral groups that are more numerous for samples heat-treated at 700 degrees C. (c) 2004 Elsevier B.V. All rights reserved.

Ion beam analysis of a-C:H films on alloy steel substrate

An a-C:H thin film deposited by plasma immersion ion implantation and deposition on alloy steel (16MnCr5) was analyzed using a self-consistent ion beam analysis technique.In the self-consistent analysis, the results of each individual technique are combined in a unique model, increasing confidence and reducing simulation errors.Self-consistent analysis, then, is able to improve the regular ion beam analysis since several analyses commonly used to process ion beam data still rely on handling each spectrum independently.The sample was analyzed by particle-induced x-ray emission (for trace elements), elastic backscattering spectrometry (for carbon), forward recoil spectrometry (for hydrogen) and Rutherford backscattering spectrometry (for film morphology).The self-consistent analysis provided reliable chemical information about the film, despite its heavy substrate.As a result, we could determine precisely the H/C ratio, contaminant concentration and some morphological characteristics of the film, such as roughness and discontinuities.© 2013 Elsevier B.V.All rights reserved.

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)

Helium ion irradiation of polymer films deposited from TMS-Ar plasmas

Polymer films synthesized from plasmas of a tetramethylsilane - Ar mixture were modified by irradiation with 170 keV He ions at fluences ranging from 1 x 10(14) to 1 x 10(16) cm(-2). As revealed by infrared spectroscopy, the ion beam produced intense bond rearrangements, such as the depletion of bonding groups (C-H and Si-H), and induced the formation of new ones, such as O-H and Si-O. From the nanoindentation measurements, a remarkable increase in the surface hardness of the films was observed as the ion fluence was increased. The increases in hardness were accompanied by an increase in the film compaction as shown by using a combination of RBS and film thickness measurements. From both hardness and infrared measurements A was concluded that, under the He ion bombardment, the polymer structure is transformed into a silicon oxycarbide network.

XPS investigation of plasma-deposited polysiloxane films irradiated with helium ions

This work describes an XPS investigation of plasma-deposited polysiloxane films irradiated with 170 keV He+ ions at fluences, Phi, ranging from 1 x 10(14) to 1 x 10(16) cm(-2). Modifications in the atomic concentrations of the surface atoms with (D were revealed by changes in the [O]/[Si], [O]/[C] and [C]/[Si] atomic ratios. Surface chemical structure modifications were evidenced by the increasing C1s peak width and asymmetry as Phi was increased, due to the formation of ether and carboxyl functionalities. Moreover, structural transformations were indicated by the positive binding energy shift of the Si2p peaks, due to the increasing Si oxidation. Correlations of the XPS data with other results from previous work on polysiloxanes illustrate the role of ion beam-induced bond breaking on the structural modifications.

Plasmonic structures fabricated by interference lithography for sensor applications

In this work we demonstrate the use of holographic lithography for generation of large area plasmonic periodic structures. Submicrometric array of holes, with different periods and thickness, were recorded in gold films, in areas of about 1 cm2, with homogeneity similar to that of samples recorded by Focused Ion Beam. In order to check the plasmonic properties, we measured the transmission spectra of the samples. The spectra exhibit the typical surface plasmon resonances (SPR) in the infrared whose position and width present the expected behavior with the period of the array and film thickness. The shift of the peak position with the permittivity of the surrounding medium demonstrates the feasebility of the sample as large area sensors. © 2009 SPIE.

Adsorption of dihydrogen phosphate ion on platinum electrodes in aqueous media monitored by probe-beam deflection

Probe-beam deflection (PBD) was used to monitor concentration gradients of anions adjacent to the surface of a platinum electrode in acidic aqueous media containing H3PO4. PBD can measure the potential-dependent extent of adsorption of H2PO4- on the Pt electrode surface and permits the Langmuir isotherm to be fitted to the experimental data. The value thus obtained for the surface concentration was 1.3 × 10-11 mol mm -2, or 1.7 atoms of Pt per H2PO4-. Also, the electron transfer number obtained was 0.24, signifying an incomplete transfer of charge, and the equilibrium constant is 1.80 suggesting a reversible adsorption process. © 2005 Elsevier B.V. All rights reserved.

Projected length annealing of etched Sm-152 ion tracks in apatite

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Nanohardness of a Ti thin film and its interface deposited by an electron beam on a 304 SS substrate

The results of nanohardness measurements at a film surface and film-substrate interface are presented and discussed. An electron beam device was used to deposit a Ti film on a 304 stainless steel (304 SS) substrate. The diluted interface was obtained by thermal activated atomic diffusion. The. Ti film and Ti film-304 SS interface were analyzed by energy dispersive spectrometry and were observed using atomic force microscopy. The nanohardness of the Ti film-304 SS system was measured by a nanoindentation technique. The results showed the Ti film-304 SS interface had a higher hardness value than the Ti film and 304 SS substrate. The Ti film surface had a lower hardness due to the presence of a TiO2 thin layer.

Argon ion implantation inducing modifications in the properties of benzene plasma polymers

Benzene plasma polymer films were bombarded with Ar ions by plasma immersion ion implantation. The treatments were performed using argon pressure of 3 Pa and 70 W of applied power. The substrate holder was polarized with high voltage negative pulses (25 kV, 3 Hz). Exposure time to the immersion plasma, t, was varied from 0 to 9000 s. Optical gap and chemical composition of the samples were determined by ultraviolet-visible and Rutherford backscattering spectroscopies, respectively. Film wettability was investigated by the contact angle between a water drop and the film surface. Nanoindentation technique was employed in the hardness measurements. It was observed growth in carbon and oxygen concentrations while there was decrease in the concentration of H atoms with increasing t. Furthermore, film hardness and wettability increased and the optical gap decreased with t. Interpretation of these results is proposed in terms of the chain crosslinking and unsaturation. (C) 2002 Elsevier B.V. B.V. All rights reserved.

Plasma immersion ion implantation of nitrogen into H13 steel under moderate temperatures

Ion implantation of nitrogen into samples of tempered and quenched H13 steel was carried out by plasma immersion technique. A glow discharge plasma of nitrogen species was the ion source and the negative high voltage pulser provided 10-12 kV, 60 mu s duration and 1.0-2.0 kHz frequency, flat voltage pulses. The temperatures of the samples remained between 300 and 450 degrees C, sustained solely by the ion bombardment. In some of the discharges, we used a N-2 + H-2 gas mixture with 1:1 ratio. PIII treatments as long as 3, 6, 9 and up to 12 h were carried out to achieve as thickest treated layer as possible, and we were able to reach over 20 mu m treated layers, as a result of ion implantation and thermal (and possibly radiation enhanced) diffusion. The nitrogen depth profiles were obtained by GDOS (Glow Discharge Optical Spectroscopy) and the exact composition profiles by AES (Auger Electron Spectroscopy). The hardness of the treated surface was increased by more than 250%, reaching 18.8 GPa. No white layer was seen in this case. A hardness profile was obtained which corroborated a deep hardened layer, confirming the high efficacy of the moderate temperature PIII treatment of steels. (c) 2005 Elsevier B.V. All rights reserved.

The effect of N+ ion energy on the properties of ion bombarded plasma polymer films

This work describes the influence of the ion bombardment on the electrical, optical and mechanical properties of polymer films deposited from radio-frequency plasmas of benzene. Irradiations were conducted using N+ at 5 x 10(19) ions/m(2), varying the ion energy, E-0, from 0 to 150 keV. Film elemental composition was determined by Rutherford backscattering spectroscopy. Electrical resistivity and hardness were obtained by the two-point probe and nanoindentation technique, respectively. Ultraviolet-visible spectroscopy was employed to investigate the optical constants of the samples. Etching rate was determined by exposure of the films to reactive oxygen plasmas. Ion bombardment induced gradual loss of H and increase in C and O concentrations with Eo. As a consequence the electrical, optical and mechanical properties were drastically affected. Interpretation of these results is proposed in terms of chain cross-linking and unsaturation. (C) 2001 Elsevier B.V. B.V. All rights reserved.