Aluminum phosphate was deposited onto bundles of carbon fibers and flat glassy carbon substrates using atomic layer deposition by exposing them to alternating pulses of trimethylaluminum and triethylphosphate vapors. Energy dispersive X-ray spectroscopy (EDXS) and solid state nuclear magnetic resonance (SS-NMR) spectra confirmed that the coating comprises aluminum phosphate (orthophosphate as well as other stoichiometries). Scanning electron microscopic (SEM) images revealed that the coatings are uniform and conformal. After coating, the fibers are still separated from each other like the uncoated fibers. Thermogravimetric analysis (TGA) indicates an improvement of oxidation resistance of the coated fibers compared to uncoated fibers.
A series of cationic diblock copolymers, poly(N-isopropylacrylamide)(48)-block-poly((3-acrylamidopropyl)trimethylammonium chloride)(X), abbreviated as PNIPAAM(48)-b-PAMPTMA(+)(X) (X = 0, 6, 10, 14, and 20), has been synthesized, and their adsorption onto silicon oxynitride from aqueous solution has been investigated using dual polarization interferometry. The polymer adsorption was modeled by using a lattice mean-field theory, and a satisfactory consistency between theory and experiments was found in terms of surface excess and layer thickness. Both theory and experiments show that the adsorption is limited by steric repulsion for X < X(max) and by electrostatic interactions for X > X(max). Modeling demonstrates that significant surface charge regulation occurs due to adsorption. Both the nonionic and cationic block exhibit nonelectrostatic affinity to silicon oxynitride and thus contribute to the driving force for adsorption, and modeling is used for clarifying how changes in the nonelectrostatic affinity affects the surface excess. The segments of the nonionic and cationic blocks seem less segregated when both have a nonelectrostatic affinity for the surface compared to the case where the segments had no surface affinity. Adsorption kinetics was investigated experimentally. Two kinetic regimes were observed: the adsorption rate is initially controlled by the mass transfer rate to the surface and at higher coverage is limited by the attachment rate.
High temperature-resistant fabrics can be used as a reinforcement structure in ceramic matrix composites. They often need a coating for oxidation protection and mechanical decoupling from the matrix. Atomic layer deposition (ALD) provides very thin conformal coatings even deep down into complex or porous structures and thus might be a suitable technique for this purpose. Carbon fiber fabrics (size 300 mm × 80 mm) and SiC fiber fabrics (size 400 mm × 80 mm) were coated using ALD with a multilayer system: a first layer made of 320 cycles of alumina (Al2O3) deposition, a second layer made of 142 cycles of titania-furfuryl alcohol hybrid (TiO2-FFA), and a third layer made of 360 cycles of titanium phosphate (TixPOy). Scanning electron microscopy reveals that the coatings are uniform and that the thickness of each layer is almost independent of the place in the reactor while coating. Appearance and thickness do not show any dependence on the type of fiber used as a substrate. Energy dispersive x-ray spectroscopy confirmed the expected elemental composition of each layer. Thermogravimetric analysis under oxidizing environment revealed that the first layer increases the onset temperature of fiber oxidation significantly, while the following two layers improve the oxidative protection only to a much smaller degree. Varying the geometry and size of the sample holder and especially the stacking of several fabric specimens on top of each other allowed increasing the total area of coated fabric up to 560 cm2 per batch. It was demonstrated that four-layered fiber coatings could be obtained with high uniformity even on these much more complicated geometries.
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