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.

Stable colloidal suspensions of nanostructured zirconium oxide synthesized by hydrothermal process

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

Effect of the fluorination of DLC film on the corrosion protection of aluminum alloy (AA 5052)

It is presented a study conducted on the physical and electrochemical properties of fluorinated a-C:H films deposited onto a commercial aluminum alloy (AA 5052). The coatings were deposited from mixtures of 91% of acetylene and 9% of argon by plasma immersion ion implantation and deposition technique, PIIID. Total gas pressure was 44 Pa and deposition time (t(dep)) was varied from 300 to 1200 s. The depositing plasmas were generated by the application of radiofrequency power (13.56 MHz, 100W) to the upper electrode and high voltage negative pulses (2400 V. 300 Hz) to the sample holder. Fluorine was incorporated in a post-deposition plasma treatment (13.56 MHz, 70W, 13 Pa) generated from sulfur hexafluoride atmosphere. Chemical structure and composition of the films were investigated using infrared reflectance/absorbance spectroscopy and X-ray photoelectron spectroscopy. The corrosion resistance of the layers was determined by electrochemical impedance spectroscopy (EIS) in a 3.5% NaCl solution, at room temperature. Films presented good adhesion to the substrates and are classified as hydrogenated amorphous carbon (a-C:H) with oxygen traces. Fluorine was detected in all the samples after the post-deposition treatment being its proportion independent on the deposition time. Film thickness presented different tendencies with t(dep), revealing the variation of the deposition rate as a function of the deposition time. Such fluorinated a-C:H films improved the corrosion resistance of the aluminum surface. In a general way the corrosion resistance was higher for films prepared with lower deposition times. The variation of sample temperature with t(dep) was found to be decisive for the concentration of defects in the films and, consequently, for the performance of the samples in electrochemical tests. Results are interpreted in terms of the energy delivered to the growing layer by ionic bombardment. (C) 2010 Elsevier B.V. All rights reserved.

Lanthanide-Containing Light-Emitting Organic-Inorganic Hybrids: A Bet on the Future

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

Hydrogenated amorphous carbon as protective coating for a forming tool

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

Microstructure and phase evolution of SrTiO3 thin films on Si prepared by the use of polymeric precursors

The use of polymeric precursors was employed in preparing SrTiO3 thin films by dip coating using Si (111) as substrate. Crack free films were obtained after sintering at temperatures ranging from 550 to 1000°C. The microstructure, characterized by SEM, shows the development of dense polycrystalline films with smooth surface and mean grain size of 52 nm, for films sintered at 1000°C. Grazing incident angle XRD characterization of these films shows that the SrTiO3 phase crystallizes from an inorganic amorphous matrix. No intermediate crystalline phase was identified.

Ceramic coating for refractories protection against carbon oxidation, Part 1: Protection mechanisms

For retarding carbon oxidation in refractories during the preheating of metallurgical furnaces, a ceramic coating, made mainly of sodium phosphosilicate and clay was developed. The coating presents high adherence to the substrate with no swelling. The coating was characterized by thermal analysis, X-ray diffraction at room temperature (XRD) and at high temperature (HTXRD), X-ray fluorescence and scanning electronic microscopy (SEM). The glass transition temperature is reached at 800 °C and only glassy phase is observed above this temperature. Thus the mechanism of protection seems to be the formation of a glassy phase on the surface of the refractory, and the coating tends to be more efficient at temperatures higher than 800 °C.

Effects of tungsten carbide thermal spray coating by HP/HVOF and hard chromium electroplating on AISI 4340 high strength steel

In cases of decorative and functional applications, chromium results in protection against wear and corrosion combined with chemical resistance and good lubricity. However, pressure to identify alternatives or to improve conventional chromium electroplating mechanical characteristics has increased in recent years, related to the reduction in the fatigue strength of the base material and to environmental requirements. The high efficiency and fluoride-free hard chromium electroplating is an improvement to the conventional process, considering chemical and physical final properties. One of the most interesting, environmentally safer and cleaner alternatives for the replacement of hard chrome plating is tungsten carbide thermal spray coating, applied by the high velocity oxy-fuel (HVOF) process. The aim of this study was to analyse the effects of the tungsten carbide thermal spray coating applied by the HP/HVOF process and of the high efficiency and fluoride-free hard chromium electroplating (in the present paper called 'accelerated'), in comparison to the conventional hard chromium electroplating on the AISI 4340 high strength steel behaviour in fatigue, corrosion, and abrasive wear tests. The results showed that the coatings were damaging to the AISI 4340 steel behaviour when submitted to fatigue testing, with the tungsten carbide thermal spray coatings showing the better performance. Experimental data from abrasive wear tests were conclusive, indicating better results from the WC coating. Regarding corrosion by salt spray test, both coatings were completely corroded after 72 h exposure. Scanning electron microscopy technique (SEM) and optical microscopy were used to observe crack origin sites, thickness and adhesion in all the coatings and microcrack density in hard chromium electroplatings, to aid in the results analysis. © 2001 Elsevier Science B.V. All rights reserved.

An investigation of electrolytic surface damages and electroplated crhomium effects on fatigue behavior of high strength steel

Fatigue crack initiation occurs at the surface, although sub surface nucleation has also been reported. Localized imperfections like inclusions close to surface and surface small pits can result in crack sources. Coatings are not always beneficial by fatigue point of view too. Mechanical properties of the covering material can change considerably the fatigue behavior of base metal due to residual surface stresses, to micro cracks or to hydrogen embrittlement. This paper is concerned with analysis of electrolytic etch on the fatigue resistance of a 35NCD16 high strength steel in a mechanical condition of (1760 - 1960) MPa, and analysis of electroplated hard chromium effects on the fatigue resistance in a strength condition of 989 MPa. Hardness impression was used as a reference parameter in case of electrolytic etch. In both cases, experimental data showed that fatigue strength of 35NCD16 steel was considerably reduced. Copyright © 2001 Society of Automotive Engineers, Inc.

Inorganic nanoparticles in organic-inorganic hybrid hosts for planar waveguides

Planar waveguides have been prepared on the ZrO2-(3-glycidiloxypropyl)trimethoxysilane (GPTS) system. Stable sols containing ZrO2 nanoparticles have been prepared and characterized by Photon Correlation Spectroscopy. The nanosized sol was embedded in (3-glycidoxipropyl)trimethoxisilane (GPTS) used as a hybrid host for posterior deposition. The opticalparameters of the waveguides such as refractive index, thickness and propagating modes and attenuation coefficient were measured at 632.8. 543.5 and 1550 nm by the prism coupling technique as a function of the Zr02 content. The planar waveguides present thickness of a few microns and support well confined propagating modes. Er doped samples display weak and broad (δλ≈96nm) emission at 1.5 μm.

Dental implants: Surface modification of cp-Ti using plasma spraying and the deposition of hydroxyapatite

The commercial pure titanium (cp-Ti) is currently being used with great success in dental implants. In this work we investigate how the cp-Ti implants can be improved by modifying the metal surface morphology, on which a synthetic material with properties similar to that of the inorganic part of the bone, is deposited to facilitate the bone/implant bonding. This synthetic material is the hydroxyapatite, HA, a calcium-phosphate ceramic. The surface modification consists in the application of a titanium oxide (TiO2) layer, using the thermal aspersion - plasma spray technique, with posterior deposition of HA, using the biomimetic method. The X-ray diffraction (XRD), Scanning Electron Microscopy (SEM) with Energy Dispersive X-ray (EDX) and Diffuse Reflectance Infrared Fourier Transform (DRIFT) techniques have been used for characterizing phases, microstructures and morphologies of the coatings. The TiO2 deposit shows a mixture of anatase, rutilo and TiO2-x phases, and a porous and laminar morphology, which facilitate the HA deposition. After the thermal treatment, the previously amorphous structured HA coating, shows a porous homogeneous morphology with particle size of about 2-2.5 μm, with crystallinity and composition similar to that of the biological HA.

Erbium-activated HfO2-based waveguides for photonics

70SiO2 - 30HfO2 planar waveguides, activated by Er3+ concentration ranging from 0.3 to 1 mol%, were prepared by solgel route, using dip-coating deposition on silica glass substrates. The waveguides showed high densification degree, effective intermingling of the two components of the film, and uniform surface morphology. Propagation losses of about 1 dB/cm were measured at 632.8 nm. When pumped with 987 nm or 514.5 nm continuous-wave laser light, the waveguides showed the 4I 13/2→4I15/2 emission band with a bandwidth of 48 nm. The spectral features were found independent both on erbium content and excitation wavelength. The 4I13/2 level decay curves presented a single exponential profile, with a lifetime between 2.9-5.0 ms, depending on the erbium concentration.

Powder processing and In Vivo evaluation of a titanium porous coating implant

The processing of titanium porous coatings using powder metallurgy technique to achieve a porous structure that allows osseointegration with bone tissue was discussed. The porous microstructure exhibited micropores and interconnected macropores with size ranges that allowed bone ingrowth. The macropores in the coatings were originated from the binder evaporation while the micropore was related with the porous titanium powder and the low compaction pressure used. The in vivo evaluation indicated that osseointegration had occurred between the bone and porous material.

Evaluation of Ir-based modifiers in the simultaneous determination of As, Bi, Pb, Sb, and Se in milk by graphite furnace atomic absorption spectrometry

Different modifiers (IrCl3, W+IrCl3, Zr+IrCl 3) and coatings (Ir, W-Ir, Zr-Ir) were evaluated for the simultaneous determination of arsenic, bismuth, lead, antimony, and selenium in milk by graphite furnace atomic absorption spectrometry using the 'end-capped' transversely heated graphite atomizer (THGA). Integrated platform, pretreated with Zr-Ir as permanent modifier, was elected as the optimum surface modification resulting in up to 250 firings. Two additional recoatings were possible without significant changes in the analytical performance (750 firings). For 20 μL of matrix-matched standard solutions using diluted (1:10) milk samples, typical correlation coefficients between integrated absorbance and analyte concentration (5.00-20.0 μg/L) was always better than 0.999. The levels of the analytes found in commercial milk samples were lower than the limit of detection: 2.9 μg/L As, 2.9 μg/L Bi, 1.8 μg/L Pb, 1.9 μg/L Sb, and 2.5 μg/L Se. Recoveries were found within the following intervals: 88-114% for As, 89-118% for Bi, 89-113% for Pb, 91-115% for Sb, and 92-115% for Se. The relative standard deviations (n = 12) were ≤2% (As), ≤ 5% (Bi), ≤ 1.4% (Pb), ≤ 3% (Sb), and 5% (Se), and the respective calculated characteristic masses were 54 pg As, 55 pg Bi, 40 pg Pb, 56 pg Sb, and 51 pg Se.

Temporal evolution of sulfated zirconia sol-gel during dip coating: Analysis of mass drainage with time-varying refractive index

The formation of sulfated zirconia films from a sol-gel derived aqueous suspension is subjected to double-optical monitoring during batch dip coating. Interpretation of interferometric patterns, previously obscured by a variable refractive index, is now made possible by addition of its direct measurement by a polarimetric technique in real time. Significant sensitivity of the resulting physical thickness and refractive index curves (uncertainties of ±7 nm and ±0.005, respectively) to temporal film evolution is shown under different withdrawal speeds. As a first contribution to quantitative understanding of temporal film formation with varying nanostructure during dip coating, detailed analysis is directed to the stage of the process dominated by mass drainage, whose simple modeling with temporal t-1/2 dependence is verified experimentally. © 2006 Elsevier B.V. All rights reserved.