Transparent and conductive ZnO : Al thin films prepared by sol-gel dip-coating

Aluminum doped zinc oxide polycrystalline thin films (AZO) were prepared by sol-gel dip-coating process. The sol was prepared from an ethanolic solution of zinc acetate using lithium hydroxide or succinic acid as hydrolytic catalyst. The quantity of aluminum in the sol was varied from 1 to 10 mol%. The structural characteristics studied by X-ray diffractometry were complemented by resistivity measurements and UV-Vis-NIR spectroscopy. The films are transparent from the near ultraviolet to the near infrared, presenting an absorption cut-off at almost 290 nm, irrespective of the nature of the catalyst and doping level. The best conductors were obtained for the AZO films containing 3 mol% of aluminum, prepared under acidic and basic catalysis and sintered at 450 degreesC. Their optical band-gap of 4.4 eV calculated from the absorption cut-off is larger than the values for band-gap widening predicted by the standard model for polar semiconductors. These polycrystalline films are textured with preferential orientation of grains along the wurtzite c-axis or the (100) direction. (C) 2003 Elsevier Ltd. All rights reserved.

Deposition of controlled thickness ultrathin SnO2 : Sb films by spin-coating

The technological interest in transparent conductive oxide films (TCOs) has motivated several works in processing techniques, in order to obtain adequate routes to application. In this way, this work describes a new route to obtain antimony-doped tin oxide (ATO) films, based in colloidal dispersions of oxide nanocrystals. The nanoparticles were obtained by a hydrolisis method, using SnCl2 and SbCl3 in ethanolic solutions. The residual halides were removed by dyalisis, obtaining a limpid and transparent colloidal suspension. By this, the method offers the advantage of producing ultrathin films without organic contaminants. This route was employed to produce films with 5, 10, 14, and 18 mol% Sb doping, with thickness ranging from 40 to 70 nm. The physical characterization of the samples showed a uniform layer deposition, resulting in good packing density and high transmittance. A preliminar electrical study confirmed the low electrical resistivity even in the ultrathin films, in such level similar of reported data. The method described is similar in some aspects to layer-by-layer (LbL) techniques, allowing fine control of thickness and interesting properties for ultrathin films, however, with low cost when compared to similar routes.

Preparation of 9/65/35 PLZT thin films deposited by a dip-coating process

Crack-free polycrystalline PLZT (Pb,a)(Zr,Ti)O-3 thin films with the perovskite structure were prepared by dir-coating using the Pechinis process. Lead acetate, hydrated lanthanum carbonate, zirconium n-propoxide and titanium isopropoxide were used as raw materials. The viscosity of the solution was adjusted in the range of 20 to 56 cP and the films were deposited by a dip-coating process on silicon (100) as substrate. Solutions with ionic concentration of 0.1 and 0.2 M were used. Thin film deposition was accomplished by dipping the substrates in the solution with control of withdrawal speed from 5 to 20 mm/min. The thin films were thermally treated in two steps: at 300 degreesC amid 650 degreesC. The influence of withdrawal speed. viscosity, heating rate and ionic concentration on the morphology of PLZT thin film was discussed. (C) 2001 Elsevier B.V. Ltd. All rights reserved.

Comparative study of the efficacies of nine assay methods for the dextransucrase synthesis of dextran

A comparative study of nine assay methods for dextransucrase and related enzymes has been made. A relatively widespread method for the reaction of dextransucrase with sucrose is the measurement of the reducing value of D-fructose by alkaline 3,5-dinitrosalicylate (DNS) and thereby the amount of D-glucose incorporated into dextran. Another method is the reaction with C-14-sucrose with the addition of an aliquot to Whatman 3MM paper squares that are washed three times with methanol to remove C-14-D-fructose and unreacted C-14-sucrose, followed by counting of C-14-dextran on the paper by liquid scintillation counting (LSC). It is shown that both methods give erroneous results. The DNS reducing value method gives extremely high values due to over-oxidation of both D-fructose and dextran, and the C-14-paper square method gives significantly low values due to the removal of some of the C-14-dextran from the paper by methanol washes. In the present study, we have examined nine methods and find two that give values that are identical and are an accurate measurement of the dextransucrase reaction. They are (1) a C-14-sucrose/dextransucrase digest in which dextran is precipitated three times with three volumes of ethanol, dissolved in water, and added to paper and counted in a toluene cocktail by LSC: and (2) precipitation of dextran three times with three volumes of ethanol from a sucrose/dextransucrase digest, dried, and weighed. Four reducing value methods were examined to measure the amount of D-fructose. Three of the four (two DNS methods, one with both dextran and D-fructose and the other with only D-fructose, and the ferricyanide/arsenomolybdate method with is-fructose) gave extremely high values due to over-oxidation of D-fructose, D-glucose, leucrose, and dextran. (C) 2011 Elsevier Ltd. All rights reserved.

Hydrogenated amorphous carbon as protective coating for a forming tool

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

Lubricating coating prepared by PIIID on a forming tool

In this work, the performance of a-C: H films produced by the hybrid Plasma Immersion Ion Implantation and Deposition technique as lubricating layers for a steel forming tool has been investigated. Hardened steel (AISI M2, 64 HRC) plates coated with a commercial TiN layer were used as substrates and the films were deposited in a vacuum chamber fitted with two parallel-plate electrodes. The discharges were generated in atmospheres composed of 91% C2H2 and 9% Ar by the application of radiofrequency power (13.56 MHz, 100 W) to the upper electrode while the lower one, also used as the sample holder, was biased with high voltage negative pulses (3.6 kV, 30 mu s, 300 Hz). A deposition time of 840 s was used. The effects of the gas pressure, p, on thickness, molecular structure, wettability, surface morphology and topography, hardness and friction coefficient of the films lwere investigated. Film thickness increased from 0.3 to 0.5 mu m when p was increased from 2.7 to 16.5 Pa. Generally, the films were slightly hydrophilic, with contact angles of around 84 degrees, and the deposition decreased the roughness of the steel. A polymer-like structure was detected in high pressure depositions and an amorphous carbon structure derived from the low pressure procedures. Hardness decreased from 8.2 to 7.0 GPa with increasing p. Improvement in tribological performance was indicated by the fall in the friction coefficient from 0.5 to 0.2 as the deposition pressure was reduced. Operating at the latter value (of mu) would lead to a significant reduction in wear and hence to significant economy in diverse industrial applications.

Bioactive coating on titanium implants modified by Nd:YVO4 laser

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Electrical and optical characteristics of SnO2 thin films prepared by dip coating from aqueous colloidal suspensions

Starting from aqueous colloidal suspensions, undoped and Nb5+ doped SnO2 thin films have been prepared by using the dip-coating sol gel process. X-ray diffraction results show that films are polycrystalline with crystallites of average size1-4nm. Decreasing the thickness of the films and increasing the Nb5+ concentration limits the crystallite size growth during firing. Complex impedance measurements reveal capacitive and resistive effects between adjacent crystallites or grains, characteristic of electrical potential barriers. The transfer of charge throughout these barriers determines the macroscopic electrical resistance of the layer. The analysis of the optical absorption spectra shows that the samples present more than 80% of their transmittance in the visible region and the value of the band gap energy increases with decreasing crystallite size. © 1997 Chapman & Hall.

Photodesorption and electron trapping in n-type SnO2 thin films grown by dip-coating technique

Thin films of undoped and Sb-doped (2 atg%) SnO2 have been prepared by sol-gel dip-coating technique on borosilicate glasses. Variation of photoconductivity excitation with wavelength and optical absorption indicate indirect bandgap transition with energy of ≅ 3.5 eV. Conductance as function of temperature indicates two levels of capture with 39 and 81 meV as activation energies, which may be related to an Sb donor and oxygen vacancy respectively. Electron trapping by these levels are practically destroyed by UV photoexcitation (305 nm) and heating in vacuum to 200°C. Gas analysis using a mass spectrometer indicates an oxygen related level, which may not be desorbed in the simpler O2 form.

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.

Improved Conductivity Induced by Photodesorption in SnO2 Thin Films Grown by a Sol-Gel Dip Coating Technique

Thin films of undoped and Sb-doped SnO2 have been prepared by a sol-gel dip-coating technique. For the high doping level (2-3 mol% Sb) n-type degenerate conduction is expected, however, measurements of resistance as a function of temperature show that doped samples exhibit strong electron trapping, with capture levels at 39 and 81 meV. Heating in a vacuum and irradiation with UV monochromatic light (305 nm) improve the electrical characteristics, decreasing the carrier capture at low temperature. This suggests an oxygen related level, which can be eliminated by a photodesorption process. Absorption spectral dependence indicates an indirect bandgap transition with Eg ≅ 3.5 eV. Current-voltage characteristics indicate a thermionic emission mechanism through interfacial states.

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.

Influencia del tratamiento térmico en la cristalización y rugosidad de películas delgadas de LiNbO3 depositadas por el método Spin Coating

Lithium niobate (LiNbO3) thin films with 1/1 stoichiometry were prepared by a spin-coating from polymeric precursor method. The films deposited on silicon (100) substrates, were thermally treated from 400° to 600°C for 3 hours in order to study the influence of thermal treatment on the crystallinity, microstructure, grain size and roughness. X-ray diffraction (XRD) results showed that LiNbO3 phase crystallizes at low temperature (400°C). It was observed by scanning electron microscopy (SEM) that it is possible to obtain dense thin films at temperatures around 500°C. The atomic force microscopy (AFM) results showed that the grain size and roughness are strongly influenced by the annealing temperature.

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.