Investigation of the Effect of Temperature on the Microstructure and Mechanical Properties of the Ultra-High Temperature Ceramic Composite ZrB2-SiC-TiC Using the Multi-Step SPS Method.

Document Type : Original Article

Authors

1 Department of Materials Engineering - Isfahan University of Technology

2 Department of Materials Engineering, Isfahan University of Technology, Isfahan 84156-83111, Iran.

Abstract

The sintering of ZrB2 presents significant challenges due to its covalent bonding and the high temperatures required for the process. Prior research has demonstrated that incorporating up to 20% by volume of SiC as an additive can enhance both the sintering process and the mechanical properties of ZrB2-based composites. The objective of this study was to fabricate and characterize an ultra-high temperature ceramic composite composed of ZrB2 with 20 vol% SiC, utilizing the Spark Plasma Sintering (SPS) method with a multi-step approach at various temperatures. Additionally, the study sought to investigate the influence of a TiC additive on the microstructural evolution and mechanical properties of the composite. The research focused on assessing the impact of sintering temperature, ranging from 1600°C to 1900°C under a pressure of 30 MPa, in the presence of a 10% TiC additive. The introduction of up to 10% by volume of TiC into the ZrB2-20 vol% SiC composite, followed by sintering at 1800°C for 5 minutes, resulted in the formation of (Zr,Ti)B2 and (Ti,Zr)C solid solutions within the matrix. These solid solutions, along with reactions involving surface oxides such as ZrO2 and B2O3, contributed to a 15% increase in relative density. Furthermore, notable enhancements were observed in mechanical properties, including a 14% increase in hardness, a 12% increase in elastic modulus, a 20% increase in fracture strength, and an 8% increase in fracture toughness. A comparative analysis with previous studies revealed that employing a multi-step SPS technique, as opposed to a single-step process, significantly reduced the temperature and soacking time to achieve a relative density exceeding 99%. However, it was also observed that increasing the maximum sintering temperature to 1900°C in the ZrB2-20 vol% SiC-10 vol% TiC composite resulted in excessive grain growth and a slight decrease in relative density by approximately 1%.

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