Paul Dill, Florian Pachel, Christian Militzer, A. Held, G. Puchas, Stefan Knohl, W. Krenkel, C. Tegenkamp, W. Goedel
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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. 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引用次数: 2
摘要
耐高温织物可作为陶瓷基复合材料的增强结构。它们通常需要一层氧化保护和与基体机械解耦的涂层。原子层沉积(ALD)提供非常薄的适形涂层,甚至深入到复杂或多孔结构中,因此可能是用于此目的的合适技术。碳纤维织物(尺寸为300 mm × 80 mm)和SiC纤维织物(尺寸为400 mm × 80 mm)采用ALD进行多层涂层:第一层由320次氧化铝(Al2O3)沉积制成,第二层由142次钛-糠醇杂化物(TiO2-FFA)制成,第三层由360次磷酸钛(TixPOy)制成。扫描电镜显示,涂层是均匀的,每层的厚度几乎与涂层在反应器中的位置无关。外观和厚度与用作衬底的纤维类型没有任何关系。能量色散x射线光谱学证实了每一层预期的元素组成。氧化环境下的热重分析表明,第一层显著提高了纤维的氧化起始温度,而后两层对纤维的氧化保护作用的提高程度要小得多。改变样品架的几何形状和尺寸,特别是将几个织物样品堆叠在一起,可以将每批涂层织物的总面积增加到560平方厘米。结果表明,即使在这些更复杂的几何形状上,也可以获得高度均匀的四层纤维涂层。
Atomic layer deposition onto fabrics of carbon and silicon carbide fibers : Preparation of multilayers comprising alumina, titania-furfuryl alcohol hybrid, and titanium phosphate
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.