Shaul
Shaul
Shaul
Shaul Avraham and Wayne D. Kaplan Department of Materials Engineering, Technion, Haifa, Israel. Ceramic matrix composites posses a wide range of applications due to increased fracture toughness, strength and thermal shock resistance, compared to monolithic ceramics. A relatively new approach to process ceramic matrix composites is based on infiltration of a porous oxide preform with liquid metal. This technique, termed I-3A (reaction infiltrated-3A), makes use of gas-pressure infiltration, squeeze casting and pressure casting [1]. An interpenetrating network of aluminide intermetallics reinforces the ceramic matrix, thus improving the mechanical properties of the composite. The resulted intermetallics possesses high melting temperatures and relatively low densities, thus the composite is applicable for elevated temperature applications. Powders of 50 vol.% Al2O3 and 50 vol.% TiO2 were attrition milled, uniaxially pressed and fired to a final density of 50%. A laboratory made squeeze caster was used for pressure infiltration of Al alloy into the preform [1]. A reduction reaction takes place between the liquid Al and the ceramic phases [2]. A further thermal treatment was conducted in different temperatures in order to insure a fully reacted sample. The contact angle is a crucial parameter affecting the infiltration process. Wetting experiment of Al alloys on fully dense TiO2 substrates were conducted in a tube furnace using a protective atmosphere. The contact angles were measured optically as function of temperature. Analysis of the wetting specimens will corroborate the infiltration kinetics and final microstructure. Experimental results from different analytical characterization methods were used to formulate the reaction model and kinetics. X-ray diffraction (XRD), scanning and transmission electron microscopy (SEM, TEM) were used to characterize the samples. The microstructure of the infiltrated samples and the interface reaction of the wetting specimens are crucial for the understanding of the reaction kinetics. X-ray analysis of the infiltrated specimen suggests that initially the reduction reaction takes place only in a partial manner. TEM analysis (figure 1) confirms the formation of Al3Ti. A subsequent heat treatment intensifies the reduction reaction, and may lead to the formation of a fully reacted specimen. The presence of Al-Ti-Si intermetallics, after heat treatment, has been detected by EDS in TEM and SEM (figure 2). The measured contact angle is well above 90, which suggests that no wetting exists. An increase in the Mg content in the Al alloy reduces the contact angle, but it is still greater then 90. The result of the reduction reaction is the formation of Al2O3 and MgAl2O4 [3], which was confirmed by SEM. During the infiltration stage Al3Ti and Si precipitates are formed. After heat treatments the amount of free Si diminishes while complex Al-Ti-Si compounds form. The characteristics of the Al3Ti(Si) intermetallic will be clarified by the combination of the Rietveld refinement method and TEM analysis of the casted aluminide sample.
The correlation of the results from controlled experiments with microstructural investigations using imaging and analytical electron microscopy and XRD methods will lead to a better understanding of the reaction kinetics in this complex system. This will help to refine the production process and explain the unique properties of ceramic matrix composites.
Figure 1: TEM micrograph of an infiltrated specimen. Selected area diffraction confirmed the presence of Al3Ti formed by the reduction of TiO2 by liquid Al.
Figure 2: TEM micrograph of an infiltrated specimen after heat treatment (650 C-3 hours). Quantitative EDS analysis indicates the presence of Al-Ti-Si intermetallics.
Acknowledgments Prof. N. Claussen & Dr. Peter Bayer for providing specimens. A. Tsvetkov is acknowledged for assisting with specimen preparation.
[1] Synthesis of aluminide-alumina composites by reactive squeeze casting, Beyer-P; Janssen-R; Claussen-N, Advanced-Engineering-Materials. vol.2, no.11; Nov. 2000; p.734-7.. [2] Formation of Al3Ti and Al2O3 from an Al-TiO2 system for preparing in-situ aluminium matrix composites, C.F. Feng, L. Froyen, Composites: Paet A 31 (2000) 385-390. [3] Role of magnesium in cast aluminium alloy matrix composites, B.C. Pai, Geetha Ramani, Journal of Materials science 30 (1995) 1903-1911.