Interface analysis and design in powders, green bodies, and components as a function of pressureless and pressure-assisted sintering

Motivation

Components in high-temperature applications such as refractory furnace linings in melt-casting processes or heat shields for gas turbines require materials that are designed for operating temperatures of around 1500°C. Coarse-grained engineering ceramics, including those based on aluminum oxide, meet the requirements concerning chemical and oxidative resistance. The service life of such components is still severely limited due to thermal shock caused by the large thermal gradients. With the addition of a metallic component and, consequently, an increased electrical conductivity, resistive pre-heating of the parts can significantly increase service life. Research into the combination of aluminum oxide and the refractory metals niobium or tantalum within the DFG research group FOR3010 appears to be particularly promising because of their similar thermal expansion behavior. During the sintering of the composites, the formation of further phases through a reaction of the powders with each other and/or with the atmosphere as well as element segregation at grain boundaries can have a decisive effect on the material properties. It is of interest whether these can be specifically influenced by adjusting the synthesis conditions such as temperature, pressure, and sintering additives.

Objectives

  • Multiscale investigation of the microstructure of pressureless and pressure-assisted sintered castables to determine the phases and segregations present
  • Re-creation and targeted investigation of selected reactions on heat-treated magnetron-sputtered layered composites
  • Understanding of the reactions taking place and how to influence them by adjusting the processing parameters

Investigations

  • X-ray diffraction and scanning electron microscopic investigations for structure determination and microstructure analysis
  • Atom probe tomography and transmission electron microscopy for nanoscale structure analysis
  • Determination of layer adhesion energies using hydrogen loading

Funding

Research Group 3010 "Refrabund" by Deutschen Forschungsgemeinschaft

The project is performed by the APT group.

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Phase segmented backscattered electron (BSE) image indicating a reaction between Al2O3 and Ta (yellow)
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Reconstructed atom probe tomography (APT) tip specimen showing the presence of niobium oxide close to a niobium-alumina interface
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Transmission electron micrograph (TEM) of a carbon interlayer at a Nb-Al2O3 interface