Carbon fiber fabrics, consisting of interwoven bundles of 3000 single fibers, were coated with Al2O3 using the atomic layer deposition (ALD) process, exposing the fabrics to alternating pulses of trimethyl aluminium and water vapors. The thickness and uniformity of the coatings were investigated using scanning electron microscopy (SEM) and thermogravimetric analysis (TGA). The obtained coatings were conformal, 84 ALD cycles gave rise to approximately 20‐nm‐thick coatings and 168 ALD cycles to approximately 40‐nm‐thick coatings. It was found, that a uniform coating can be obtained at a purge time of 40 seconds. Reducing purge times below 20 seconds gives rise to increased particle growth and thus the coating becomes inhomogeneous. Initially, the samples that were coated had a size of 2×10 cm (thickness 0.3 mm). The size of the fabric was subsequently increased up to 8×20 cm and a uniform coating of the same quality was obtained. By oxidizing the coated fabrics, fabrics composed of interwoven alumina microtubes were obtained. Infiltration of the microtubes with solutions of two distinguishable fluorescent dyes showed that interchange of the dyes between warp and weft microtubes occurs, but is absent at approximately 20% of the crossovers. Taking all our findings into account, we conclude that the majority of the fibers were separated from each other by the coating prior to the oxidation. This work demonstrates that ALD is a suitable method to produce thin, conformal coatings on the surface of carbon fiber fabrics.
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.
A thermal atomic layer deposition process with precursors tris(trimethylsilyl) phosphate (TTMSP), titanium tetrachloride (TiCl4), and water was used with various pulse sequences in order to deposit titanium phosphate onto bundles of carbon fibers (diameter of one filament = 7 μm, 6000 filaments per bundle) and flat silicon substrates. Pulse sequence 1, TTMSP/N2/TiCl4/N2, which comprises no water, yields no significant deposition. Pulse sequence 2, TTMSP/N2/H2O/N2/TiCl4/N2, which comprises a water pulse, yields a mixed phosphate/oxide coating and shows a self-limiting character at 200 °C with a growth per cycle of 0.22 nm cycle−1. Wet chemical analysis of the coating revealed a ratio of Ti:P between 3:1 and 2:1 in reasonable agreement with the composition Ti2.4P1O7 obtained from X-ray photoelectron spectroscopy. Thus, the deposited material can approximately be described as a mixture of Ti¾PO4 and TiO2 in a molar ratio of 1:1.5. The coating shifts the temperature of the onset of oxidation—3% weight loss in thermogravimetry—of the carbon fibers from 630 °C (uncoated C-fiber) to 750 °C (with the titanium phosphate coating).
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