The oxidation and scale crystallization kinetics of Hi‐NicalonTM‐S SiC fibers were measured after oxidation in dry air between 700° and 1400°C. Scale thickness, composition, and crystallization were characterized by TEM with EDS, supplemented by SEM and optical microscopy. TEM was used to distinguish oxidation kinetics of amorphous and crystalline scales. Oxidation initially produces an amorphous silica scale that incorporates some carbon. Growth kinetics of the amorphous scale was analyzed using the flat‐plate Deal‐Grove model. The activation energy for parabolic oxidation was 248 kJ/mol. The scales crystallized to tridymite and cristobalite, starting at 1000°C in under 100 h and 1300°C in under 1 h. Crystallization kinetics had activation energy of 514 kJ/mol with a time growth exponent of 1.5. Crystalline silica nucleated at the scale surface, with more rapid growth parallel to the surface. Crystalline scales cracked from thermal residual stress and phase transformations during cool‐down, and during oxidation from tensile hoop growth stress. High growth shear stress was inferred to cause intense dislocation plasticity near the crystalline SiO2–SiC interphase. Crystalline scales were thinner than amorphous scales, except where growth cracks allowed much more rapid oxidation.
Hi‐Nicalon™‐S SiC fiber strengths and Weibull moduli were measured after oxidation for up to 100 hours between 700°C and 1400°C in wet and dry air. SiO2 scale thickness and crystallization extent were measured by TEM. The effect of furnace environment on trace element levels in the SiO2 scales was characterized by secondary ion mass spectroscopy. Crystallization kinetics and Deal‐Grove oxidation kinetics for glass and crystalline scale, and the transition between them, were modeled and determined. Crystallization retards oxidation kinetics, and scale that formed in the crystalline state was heavily deformed by the growth stress accompanying SiC oxidation volume expansion. Glass scales formed in dry air slightly increased fiber strength. Glass scales formed in wet air did not increase strength, and in some cases significantly decreased strength. Scales more than 200 nm thick were usually partially or completely crystallized, which degraded fiber strength. Contamination of scales by trace impurities such as Al and Ca during heat treatment inhibited crystallization. The oxidation kinetics and the strengths of oxidized Hi‐Nicalon™‐S fibers are compared with previous studies on SiC fibers, bulk SiC, and single‐crystal SiC. Empirical relationships between oxidation temperature, time, scale thickness, and strength are determined and discussed.
Fiber‐reinforced ceramic composites achieve high toughness through distributed damage mechanisms. These mechanisms are dependent on matrix cracks deflecting into fiber/matrix interfacial debonding cracks. Oxidation resistance of the fiber coatings often used to enable crack deflection is an important limitation for long‐term use in many applications. Research on alternative, mostly oxide, coatings for oxide and non‐oxide composites is reviewed. Processing issues, such as fiber coatings and fiber strength degradation, are discussed. Mechanics work related to design of crack deflecting coatings is also reviewed, and implications on the design of coatings and of composite systems using alternative coatings are discussed. Potential topics for further research are identified.
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