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Understanding and utilization of thermal gradients in spark plasma sintering for graded microstructure and mechanical properties

Date

2022

Authors

Preston, Alexander David, author
Ma, Kaka, advisor
Weinberger, Chris, committee member
Neilson, Jamie, committee member
Heyliger, Paul, committee member

Journal Title

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Volume Title

Abstract

Spark plasma sintering (SPS), also commonly known as electric field assisted sintering, utilizes high density electric currents and pressure to achieve rapid heating and significantly shorter sintering times for consolidating metal and ceramic powders, which could otherwise be difficult, time consuming, and energy intensive. SPS has attracted extensive research interests since the early 1990's, with the promise of efficient manufacturing of refractory materials, ultrahigh temperature ceramics, nanostructured materials, functionally graded materials, and non-equilibrium materials. Thermal gradients occur in SPS tooling and the samples during sintering, which can be a drawback if homogeneous properties are desirable, as the temperature inhomogeneity can lead to large gradients in microstructure such as porosity, grain size, and phase distribution. Many researchers have looked to mitigate or control these gradients by design and use of specialized tooling. However, the effect of the starting powder is relatively less investigated or overlooked. Feedstock powders can come in various shapes, particle size distributions, and surface chemistry. Effects of these powder characteristics on the SPS process and the consequent microstructure of the sintered parts remain as a gap in the fundamental knowledge of SPS. To fill in this gap, my research investigated the role of thermal gradients during SPS, and how the thermal gradients subsequently affect the location-specific pore distribution, and the consequent mechanical properties of the materials. From a practical point of view, design and fabrication of a bulk sample with a fully dense surface and an engineered pore architecture in the sample interior via one-step SPS will enable mechanical properties unattainable via conventional processing of fully dense bulk materials, such as alike combination of lightweight, high surface hardness, and wear resistance, and high toughness. Therefore, the overarching goal of my research was to provide fundamental insights into the material processing - microstructure - properties correlation so that the field assisted sintering technology can be advanced to control location-specific microstructure. To fulfill this goal, two metallic materials were selected in my study, austenitic stainless steel and commercially pure titanium, representing inherently heavy but widely used alloys, and a pure metal that is inherently lightweight, these materials were used to investigate the effects of powder morphology on the sintering behavior. The pure Ti was selected specifically to gain fundamental insight into the effect of powder shape on sintering, while mitigating the concern of alloying/precipitation events and integrating FEM with my experimental work. This work identified a relationship between decreasing pore size and increasing yield strength in stainless steel, which was attributed to fine precipitate formation surrounding submicron pores inducing local stiffening. Whereas larger pores where precipitates were not found are concluded to not have the necessary driving force for the precipitation event to occur. Ball milled stainless steel powders with higher aspect ratios were also shown to have smaller porosity gradients in comparison to their spherical gas atomized counterparts. A thermal electric finite element model is also proposed which incorporates the master sintering curve to simulate densification as an alternative to the more computationally costly and difficult to parametrize fully coupled thermal-electric-mechanical finite element model. Results from the combined model indicate strong agreement with experimental results within 2% accuracy of measured densification. Additionally, the model predicts higher porosity gradients for gas atomized powders in comparison to ball milled powders which is experimentally verified.

Description

2022 Summer.
Includes bibliographical references.

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Subject

pore characteristics
powder metallurgy
mechanical properties
spark plasma sintering
powder characteristics

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