The poly(furfuryl alcohol) is highly indicated to obtain advanced carbonaceous materials due mainly to its good carbon yield (around 50%) and a controllable cure reaction. In the processing of some carbonaceous materials, such as monolithic vitreous carbon, it is necessary to make sure that the material has the smallest porosity to be used in nobler applications such as heart valves and aerospace integrated systems. In this manuscript, a design of experiments was used to study the influence of viscosity, pH, and moisture in the porosity of the cured material. This study shows that the moisture exerts a significant influence on the porosity and the trend of the results lead to conclude that lower viscosity and moisture, and the use of non-neutralized poly(furfuryl alcohol) resins lead to obtain materials with better quality.
The present work investigates the surface finishing of two mould tool steels (WNr 1.2738~P20 and WNr 1. 4305) after polishing by conventional method and automatic laboratory equipment. These steels are employed in the fabrication of polymer injection moulds due to its good machinability, homogeneous microstructure and hardness. The polishing process was performed in laboratory by manual and automated processes. The surface finishing was measured by mechanical and optical methods. In the manual polishing, SiC paper grit 320, 600 and 1200 was used. Final polishing was carried out with polishing cloth containing 0.3 μm alumina suspension or 6 μm and 1 μm diamond suspension. Alternately, polishing of steel specimens in the specially developed laboratory automatic equipment was performed using a large rotating disc at 140 rpm, nominal pressures of 0.013 Pa, 0.139 Pa and 0.244 Pa and diamond paste with particle size 1 μm. Surface finish of specimens were compared as a function of the particle size and polishing time by three methods: the roughness parameter Rz (mean of maximum roughness depth) using a stylus probe, light reflectance with an integrating sphere connected to a spectrophotometer, and reflected diffuse light intensity analysis of a He-Ne laser. Specimen surface images were also obtained by an optical microscope to compare the topography after polishing. From the plot of roughness measurements versus particle size and intensity of diffuse light versus particle size, it was observed that both roughness parameter Rz and the intensity of diffuse light decreased linearly with the abrasive particle size for the manual polishing method. The method of light reflectance measurements shows an approximately constant value of 55 % for all particle size. Therefore, the better methods to assess surface finish of tool steels are the roughness parameter Rz and the intensity of diffuse light by laser method. For the automatic polishing, the results show that there is an optimized time for minimum roughness which is 5 minute. Other relevant aspects of surface finish by particle abrasion are also discussed.
This study compares the influence of different acid catalysts on the polymerization rate of polyfurfuryl alcohol (PFA) precursor and especially on the respective porosity of Monolithic Vitreous Carbon (MVC) produced from that. Five acid catalysts commonly used were compared: p-toluenesulfonic (PTLS), hydrochloric, sulfuric, nitric, and phosphoric. A fixed molar concentration of catalyst was diluted in PFA resin under room pressure and temperature. The time dependence of PFA resin polymerization was investigated by optical transmittance of PFA films, and the polymerization degree, characterized by ATR spectroscopy and thermogravimetry. MVC samples prepared with the same PFA resin and each catalyst were carbonized up to 1200 8C, under inert atmosphere. MVC porosity was studied by nitrogen adsorption/desorption, and by SEM and optical microscopy. Higher polymerization degree and higher residual mass were obtained with faster catalysts. No direct relation between the polymerization rate and the acid force was observed. PTLS promoted the fastest PFA polymerization process and the sulfuric acid, the slowest one. MVC samples were obtained by slow carbonization. MVC presented low specific surface S BET from 1.4 to 7.4 m 2 /g. Nitric acid catalyst contributed the most to micropores formation. Micrometric apparent porosity was smaller for the catalysts having longer polymerizations times, such as phosphoric and sulfuric acid. Phosphoric catalyst corresponded to the lowest porosity in MVC. As the polymerization time increased, the average size of the micrometric surface pores tended to augment. The MVC macroscopic porosity increased with the S BET increment. Acid catalysts choice exerted a fundamental role on the porosity of MVC. V C 2016 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2016, 133, 43272.
This work describes the laser annealing of a-SiC and a-SiC x N y films deposited on (100) Si and quartz substrates by RF magnetron sputtering. Two samples of a-SiC x N y thin films were produced under different N 2 /Ar flow ratios. Rutherford backscattering spectroscopy (RBS), Raman analysis and Fourier transform infrared spectrometry (FTIR) techniques were used to investigate the composition and bonding structure of as-deposited and laser annealed SiC and SiC x N y films.
The role of substrate ion bombardment on the structural and H bonding properties of hydrogenated amorphous germanium (a-Ge:H) films was studied by infrared (ir) spectroscopy. A Kaufman type ion source was used to produce an Ar1 beam directed towards a Ge target for a- Ge:H ion beam sputtering deposition in a H2-containing vacuum chamber. A low energy (100 eV) H2++Ar+ beam obtained from an additional ion source was allowed to impinge directly on the substrate during film growth at various beam currents.It was found that substrate bombardment by 100 eV ions favors the formation of voids, as deduced from the increasing contribution of the surface-like Ge-H stretching mode to the ir spectrum with increasing ion current. The void density was reduced below the ir detection limit by totally removing the ion beam on the substrate while keeping all other parameters fixed. For this condition, we observe no or very small surface-like contributions to the ir spectra, irrespective of substrate temperature (25-260°C) or growth rate used. A narrowing of the infrared Ge-H stretching mode peak is observed with increasing deposition temperature, indicating a concomitant tendency towards a more ordered structure.
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