AbstractsEngineering

New reaction paths for advanced SiAlON/TiN composites

by Pauline Calloch




Institution: Victoria University of Wellington
Department:
Year: 2015
Keywords: Sialon; Thermal properties; Oxidation
Record ID: 1308586
Full text PDF: http://hdl.handle.net/10063/4167


Abstract

This thesis demonstrates how selected ceramic additives, including titanium nitride (TiN), impact upon the “chemistry ↔ microstructure ↔ properties” relationship as it applies to composites in the generic Sialon-TiN composite field. Examination and optimisation of this feedback loop enables control of industrially important thermal, electrical and engineering properties of β-Sialon based ceramics. The effects of a range of additives on the nitridation and sintering of β-Sialon composite bodies have been studied and the chemical and mechanical properties of the sintered bodies have been measured. The additives can be divided in three groups: nitridation additives which improve the yield and the rate of the reaction; sintering aids; and additives that improve resistance to thermal shock. A suite of additives consisting of a mixture of calcium aluminate cement, yttrium aluminium garnet and boron nitride was found to deliver an optimum set of mechanical properties with a fracture toughness achieved of over 4 MPa.m-1/2. This thesis also reports a new reaction path for the formation of a β-Sialon/TiN composite by the reaction bonding of aluminium powder coated with nanosized titania. In this novel technique, the aluminium reacts under an inert atmosphere with titania to form alumina and a TixAly intermediate which is then nitrided to form aluminium nitride and titanium nitride. The addition of a suitable silicon phase enables the formation of a β-Sialon phase under nitrogen at high temperature. The TiN was added in the range 1 to 10 wt% (0.6 to 6 vol%). The effects of milling time on the aluminium powder particle size distribution and reactivity have been studied, with a minimum of two days milling time required to modify the particle shape and reduce melting coagulation during firing. Firing parameters have been optimised, using XRD and MAS-NMR to monitor the samples’ composition and SEM to observe their microstructure. The reduction of titania by aluminium was completed at 900 ºC for 4 hours in an argon atmosphere and the nitridation of the titanium aluminide at 1400 ºC for 3 hours in a nitrogen flow. The nitridation and sintering of the β-Sialon/TiN composite were both performed in nitrogen at 1400 ºC and 1600 ºC, respectively. A low level of addition of TiN (1 wt%) has shifted the composition toward the AlN corner of the Sialon behaviour diagram, forming α-Sialon and AlN polytypes. Other levels of addition in the studied range formed a dense β-Sialon/TiN composite. The TiN inclusions are found at the grain boundaries but are of insufficient volume fraction to form a continuous network in the Sialon matrix. Mechanical and electrical properties of the newly fabricated β-Sialon/TiN composites have been measured. These properties were generally improved by the highest levels of TiN addition: Young’s modulus (up to 210 GPa), hardness (up to 17.7 GPa), fracture toughness (up to 3.3 MPa.m-1/2) and compressive strength (up to 188 MPa). However the presence of TiN had no impact on the resistance to thermal shock and…