IMPACT OF HEAT TREATMENT AND OXIDATION OF C/C COMPOSITES ON MICROSTRUCTURE AND PHYSICAL PROPERTIES

Author

Sardar S. Iqbal, Southern Illinois University CarbondaleFollow

Date of Award

12-1-2011

Degree Name

Doctor of Philosophy

Department

Engineering Science

First Advisor

Filip, Peter

Abstract

Carbon-carbon (C/C) composites are notable among engineering materials in aerospace and defense industries possessing excellent specific mechanical, thermal, frictional and wear properties. C/C maintain their properties at temperatures where most of the high end alloys give in, and maintain their dimensional stability at temperatures above 2000 oC. C/C is frequently used in aircraft and automotive industries as brake materials. However, frictional performance is dependent on various parameters: microstructure, fiber type, fiber orientation distribution, fiber/matrix interfacial bond, heat treatment, and oxidation. The present study in dissertation provides an insight into the impact of heat treatment, and oxidation on microstructure, mechanical and thermal properties. The heat treatment (performed at 1800, 2100, 2400 oC in argon) of two-directional (2-D) pitch-fiber with charred resin carbon matrix, and three-directional (3-D) PAN-fiber with CVI carbon matrix influenced microstructure, mechanical and thermal properties. Microstructure characterized by polarized light microscopy (PLM), XRD, and Raman spectroscopy changed with increasing heat treatment temperature. The RL microstructure of 3-D C/C progressively highly organized, whereas ISO microstructure of 2-D C/C's charred resin hardly organized into an ordered structure as evident from Raman spectroscopy and Raman profiling of polished samples. Pitch-fiber organized more than the ISO microstructure of charred resin matrix. On the other, PAN-fiber became more ordered, but was organization was lower than pitch-fiber. Thermal conductivity increased for both (2-D, 3-D C/C) materials in comparison to non-heat treated (NHT) C/Cs. Thermal conductivity of oxidized samples decreased significantly than non-oxidized samples. In-plane thermal conductivity of 3-D C/C was much higher than that of 2-D C/C, and was attributed to the rough laminar (RL) microstructure of carbon matrix and continuous PAN-fiber when compared to the short pitch-fiber in isotropic (ISO) carbon matrix. Mechanical properties (tensile, compressive, shear) deteriorated with increasing heat treatment. However, statistical analysis using ANOVA showed that there was not any significant difference between the NHT and heat treated C/C materials in terms of mechanical strength, modulus, failure strain and fracture energy. The oxidized samples of heat treated (1800/2100/2400 oC) C/C materials (2-D, 3-D) showed an appreciable decrease in mechanical strength and modulus than non-oxidized samples, with progressively heat treated C/C becoming more oxidation resistant than NHT C/C. The study demonstrated a highly inhomogeneous nature of C/C, and sample size is a very important parameter in governing mechanical properties. Since, the slightest change in the dimension of samples could bring about a radically different outcome in terms of mechanical properties, and can hardly be representative of the bulk properties. Therefore, in order to obtain a good estimate of the bulk properties, the sample size must be comparable to the bulk material. The research nonetheless showed the impact of sample size in estimating the mechanical properties of bulk properties, which are highly significant after statistical analysis, and, therefore, it must be taken into account to understand the processing-structure-property-analysis relationships.