Plasma enhanced chemical vapor deposition of titanium(IV) ethoxide-oxygen-helium mixtures

Thin films were deposited by plasma enhanced chemical vapor deposition from titanium (IV) ethoxide (TEOT)-oxygen-helium mixtures. Actinometric optical emission spectroscopy was used to obtain the relative plasma concentrations of the species H, CH, O and CO as a function of the percentage of oxygen in the feed, R(ox). The concentrations of these species rise with increasing R(ox) and tend to fall for R(ox) greater than about 45%. As revealed by a strong decline in the emission intensity of the actinometer Ar as R(ox) was increased, the electron mean energy or density (or both) decreased as greater proportions of oxygen were fed to the chamber. This must tend to reduce gas-phase fragmentation of the monomer by plasma electrons. As the TEOT flow rate was fixed, however, and since the species H and CH do not contain oxygen, the rise in their plasma concentrations with increasing R(ox) is explained only by intermediate reactions involving oxygen or oxygen-containing species. Transmission infrared (IRS) and X-ray photoelectron (XPS) spectroscopies were employed to investigate film structure and composition. The presence of CH(2), CH(3), C=C, C-O and C=O groups was revealed by IRS. In addition, the presence of C-O and C=O groups was confirmed by XPS, which also revealed titanium in the +4 valence state. The Ti content of the films, however, was found to be much less than that of the monomer material itself. (C) 2007 Elsevier B.V. All rights reserved.

Controlled fluorination of a-C:F:H films by PECVD of ethylene-hexafluorobenzene mixtures

Highly fluorinated plasma polymers are chemically inert,acid resistant and have low friction coefficients, thereby being useful in chemical laboratories and for tribological applications. Here we report the plasma polymerization of ethylene-hexafluorobenzene mixtures by PECVD. The principal parameter of interest is the proportion of C(6)F(6) in the feed, R(F). Films were analyzed using near-normal and grazing-angle Infrared Reflection Absorption Spectroscopy (IRRAS), the latter being particularly useful for detecting modes not usually observed at near-normal incidence. The presence of CH and CF(x) (x=1 to 2) groups was thus confirmed in films deposited with R(F)>= 40%. Depending on R(F) IRRAS also revealed the presence of -CH(x) (x=1 to 3) -C=C, -C=O and phenyl rings. Deconvolution of C is spectra obtained by X-ray Photoelectron Spectroscopy (XPS) confirmed the presence of CH, CF and CF(2) groups in films deposited with R(F)>= 40%. Atomic ratios of F:C calculated from the XPS spectral data show that the degree of fluorination rises with increasing RF Some unbound fluorine is present in the films. Post-deposition reactions account for the presence of oxygen (similar to 5%) in the films. Surface energies, determined from contact angle measurements, fall with increasing R(F). (C) 2008 Elsevier B.V. All rights reserved.

Developments in hot-filament metal oxide deposition (HFMOD)

Hot-filament metal oxide deposition (HFMOD) is a variant of conventional hot-filament chemical vapor deposition (HFCVD) recently developed in our laboratory and successfully used to obtain high-quality, uniform films of MOx WOx and VOx. The method employs the controlled oxidation of a filament of a transition metal heated to 1000 degrees C or more in a rarefied oxygen atmosphere (typically, of about 1 Pa). Metal oxide vapor formed on the surface of the filament is transported a few centimetres to deposit on a suitable substrate. Key system parameters include the choice of filament material and diameter, the applied current and the partial pressures of oxygen in the chamber. Relatively high film deposition rates, such as 31 nm min(-1) for MoOx, are obtained. The film stoichiometry depends on the exact deposition conditions. MoOx films, for example, present a mixture of MoO2 and MoO3 phases, as revealed by XPS. As determined by Li+ intercalation using an electrochemical cell, these films also show a colouration efficiency of 19.5 cm(2) C-1 at a wavelength of 700 nm. MOx and WOx films are promising in applications involving electrochromism and characteristics of their colouring/bleaching cycles are presented. The chemical composition and structure of VOx films examined using IRRAS (infrared reflection-absorption spectroscopy), RBS (Rutherford backscattering spectrometry) and XPS (X-ray photoelectron spectrometry) are also presented. (c) 2007 Elsevier B.V. All rights reserved.

HMDSO plasma polymerization and thin film optical properties

Thin films were deposited from hexamethyldisiloxane (HMDSO) in a glow discharge supplied with radiofrequency (rf) power. Actino-metric optical emission spectroscopy was used to follow trends in the plasma concentrations of the species SiH (414.2 nm), CH (431.4 nm), CO (520.0 nm), and H (656.3 nm) as a function of the applied rf power (range 5 to 35 W). Transmission infrared spectroscopy (IRS) was employed to characterize the molecular structure of the polymer, showing the presence of Si-H, Si-O-Si, Si-O-C and C-H groups. The deposition rate, determined by optical interferometry, ranged from 60 to 130 nm/min. Optical properties were determined from transmission ultra violet-visible spectroscopy (UVS) data. The absorption coefficient α, the refractive index n, and the optical gap E04 of the polymer films were calculated as a function of the applied power. The refractive index at a photon energy of 1 eV varied from 1.45 to 1.55, depending on the rf power used for the deposition. The absorption coefficient showed an absorption edge similar to other non-crystalline materials, amorphous hydrogenated carbon, and semiconductors. For our samples, we define as an optical gap, the photon energy E04 corresponding to the energy at an absorption of 104 cm-1. The values of E04 decreased from 5.3 to 4.6 as the rf power was increased from 5 to 35 W. © 1995.

Problems related to the employment of thin uranium films as neutron dosimeters

Thin uranium films built on muscovite mica basis and obsidian samples having known ages were irradiated with thermal neutrons at the IPEN/CNEN reactor, São Paulo. Comparing thin film performance with the obsidian one, it was observed that the latter feel a greater neutron fluence. Nominal fluences at the used facility are in agreement with the results obtained analysing the obsidian samples. A probable hypothesis to explain this disagreement, namely, the uranium loss from the thin films, was ruled out. © 1995.

Plasma-deposition of Ag-containing polyethyleneoxide-like coatings

Ag-containing polyethyleneoxide (FEO)-like thin films have been deposited in Radio Frequency Glow Discharges fed with vapors of diethyleneglycol-dimethyl-ether and argon. Proper experimental conditions have been utilized in order to fragment the monomer in the glow and, at the same time, sputter Ag from the silver RF cathode of the reactor, in a way that polyethyleneoxide(PEO)-like coatings with embedded Ag clusters have been deposited at the ground electrode. The composition of the coatings has been investigated by means of different techniques; the plasma process has been investigated by means of Actinometric Optical Emission Spectroscopy. A correlation has been found between the amount of silver embedded in the coatings and that sputtered in the discharge, monitored by actinometry, that could eventually be utilized to control in situ the deposition process.

Preparation of films from aluminum acetylacetonate by plasma sputtering

Aluminum acetylacetonate has been reported as a precursor for the deposition of alumina films using different approaches. In this work, alumina-containing films were prepared by plasma sputtering this compound, spread directly on the powered lowermost electrode of a reactor, while grounding the substrates mounted on the topmost electrode. Radiofrequency power (13.56 MHz) was used to excite the plasma from argon atmosphere at a working pressure of 11 Pa. The effect of the plasma excitation power on the properties of the resulting films was studied. Film thickness and hardness were measured by profilometry and nanoindentation, respectively. The molecular structure and chemical composition of the layers were analyzed by Fourier transform infrared spectroscopy and energy dispersive spectroscopy. Surface micrographs, obtained by scanning electron microscopy, allowed the determination of the sample morphology. Grazing incidence X-ray diffraction was employed to determine the structure of the films. Amorphous organic layers were deposited with thicknesses of up to 7 μm and hardness of around 1.0 GPa. The films were composed by aluminum, carbon, oxygen and hydrogen, their proportions being strongly dependent on the power used to excite the plasma. A uniform surface was obtained for low-power depositions, but particulates and cracks appeared in the high-power prepared materials. The presence of different proportions of aluminum oxide in the coatings is ascribed to the different activations promoted in the metalorganic molecule once in the plasma phase. Copyright © 2013 John Wiley & Sons, Ltd. Copyright © 2013 John Wiley & Sons, Ltd.

Effect of diamond-like carbon thin film coated acrylic resin on candida albicans biofilm formation

Purpose: The purpose of this study was to evaluate the effect of diamond-like carbon thin films doped and undoped with silver nanoparticles coating poly(methyl methacrylate) (PMMA) on Candida albicans biofilm formation. The control of biofilm formation is important to prevent oral diseases in denture users. Materials and Methods: Forty-five PMMA disks were obtained, finished, cleaned in an ultrasonic bath, and divided into three groups: Gc, no surface coating (control group); Gdlc, coated with diamond-like carbon film; and Gag, coated with diamond-like carbon film doped with silver nanoparticles. The films were deposited using a reactive magnetron sputtering system (physical vapor deposition process). The specimens were characterized by optical profilometry, atomic force microscopy, and Rutherford backscattering spectroscopy analyses that determined differences in chemical composition and morphological structure. Following sterilization of the specimens by γ-ray irradiation, C. albicans (ATCC 18804) biofilms were formed by immersion in 2 ml of Sabouraud dextrose broth inoculated with a standardized fungal suspension. After 24 hours, the number of colony forming units (cfu) per specimen was counted. Data concerning biofilm formation were analyzed using ANOVA and the Tukey test (p < 0.05). Results: C. albicans biofilm formation was significantly influenced by the films (p < 0.00001), reducing the number of cfu, while not affecting the roughness parameters (p > 0.05). The Tukey test showed no significant difference between Gdlc and Gag. Films deposited were extremely thin (∼50 nm). The silver particles presented a diameter between 60 and 120 nm and regular distribution throughout the film surface (to Gag). Conclusion: Diamond-like carbon films, doped or undoped with silver nanoparticles, coating the base of PMMA-based dentures could be an alternative procedure for preventing candidosis in denture users. © 2013 by the American College of Prosthodontists.

Deposition of Al2O3 by resistive evaporation and thermal oxidation of Al to be applied as a transparent FET insulating layer

Alumina thin films have been obtained by resistive evaporation of Al layer, followed by thermal oxidation by means of annealing in appropriate atmosphere (air or O2-rich), with variation of annealing time and temperature. Optical and structural properties of the investigated films reveal that the temperature of 550 °C is responsible for reasonable oxidation, which is accelerated up to 8 times for O2-rich atmosphere. Results of surface electrical resistivity and Raman spectroscopy are in good agreement with these findings. Surprisingly, X-ray and Raman data suggest also the crystallization of Si nuclei at glass substrate-alumina interface, which would come from the soda-lime glass used as substrate. © 2013 Elsevier Ltd and Techna Group S.r.l.

Structural, microstructural, optical and electrical properties of (Pb,Ba,Sr)TiO3 films growth on conductive LaNiO3-coated LaAO(3)(100) and Pt/Ti/SiO2/Si substrates

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

PEDOT:PSS self-assembled films to methanol crossover reduction in Nafion (R) membranes

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

Sprayed films of europium complexes toward light conversion devices

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

Tetraethylortossilicate plasma thin film with hydrophilic and hydrophobic characteristics: Use on passive mixers

This work aims to obtain plasma thin film composites with hydrophobic/hydrophilic alternated regions, which are useful for the production of miniaturized mixers. These regions were acquired by two different strategies: either the codeposition of TEOS and HFE plasma thin films or the exposition of TEOS plasma films to ultraviolet radiation (UVA and UVC). These films were characterized by several chemical and physical techniques. The refractive indexes vary from 1.4 to 1.7; infrared and photoelectron spectroscopy detect Si-O-Si and CHn species. Silicone-like structures with high or low number of amorphous carbon microparticles and with fluorinated organic clusters were produced. Cluster dimensions were in the 1-5 mm range and they are made of graphite or COF (carbon/oxygen/fluorine) compounds. Scanning electron and optical microscopy showed rough surfaces. Water contact angles were 90º; however, for TEOS films that value changed after 6 hr of UVC exposure. Moreover, after UV exposure, organic polar compounds could be adsorbed in those films and water was not. The passive mixer performance was simulated using the FemLab 3.2® program and was tested with 20 nm thick films on a silicon wafer, showing the capacity of these films to be used in such devices.

Composite Thin Film Obtained Using Tetraethoxysilane and Aimed at VOCs Detection

The aim of this work was production of tetraethoxysilane (TEOS) plasma polymerized thin films and optimization of their physical-chemical characteristic for sensor development. The films were analyzed using several techniques. It was possible to produce composites (graphite clusters imbibed by silicon oxide film) made from only one reactant (TEOS). Deposition rate can vary significantly, reaching a maximum of 30 nm/min; cluster formation and their size widely depending on deposition parameters. The film surface was hydrophobic but can be wetted by organic compounds, probably due to carbon radicals. These films are good candidates for sensor development.

Study of photoinduced birefringence vs As content in thin GeAsS films

Thin films of GeAsS glass are prepared by e-beam evaporation technique. Photoinduced birefringence (PIB) is studied as function of the As content with concentrations ranging from 10% to 40%. Raman spectroscopy is used as additional tool to explain the corresponding changes undergone by the material system. The breakdown of homopolar bonds is suggested as a possible mechanism of photo induced structural changes leading to the creation of the PIB.