Date of Award

Spring 2011

Document Type

Dissertation

Degree Name

Doctor of Philosophy in Chemical Engineering - (Ph.D.)

Department

Chemical, Biological and Pharmaceutical Engineering

First Advisor

Rajesh N. Dave

Second Advisor

Ecevit Atalay Bilgili

Third Advisor

Boris Khusid

Fourth Advisor

Norman W. Loney

Fifth Advisor

Sankaran Sundaresan

Abstract

Nano-materials are the focus of many research activities due to the desirable properties imparted from their small grain size and high interfacial surface area. However, these materials are highly cohesive powders in the dry state and typically form large agglomerates, leading to a diminished surface area or even grain growth, which minimizes the effectiveness of these nanomaterials. This dissertation addresses the issue of mixing nanopowders constituents by deagglomerating them and achieving simultaneous mixing so that even after inevitable reagglomeration, the effectiveness of large interfacial surface area may be preserved.

Nano-particle mixtures were prepared using the environmentally benign dry mixing methods of Stirring in Supercritical Fluids and the Rapid Expansion of High Pressure and Supercritical Suspensions (REHPS). Stirring in Supercritical Fluids was capable of producing course scale nano-particle mixtures that were comparable to mixtures produced with more traditional liquid solvents, without the necessity of filtration and caking issues that are typically associated with them. The REHPS process was capable of producing high-quality mixtures on the sub-micron scale, and was made far superior when the nano-powders were first pre-mixed by stirring to decrease inhomogeneity of the feed. It was also shown that in general, conditions that enhanced turbulent shear stress, and thereby deagglomeration, also enhanced mixing, however this effect could be obscured by inhomogeneities introduced by the feed mixtures.

Previous authors have suggested that the primary deagglomeration mechanism is the explosive expansion of the carbon dioxide from within the agglomerate as it transitions from a high pressure to an ambient environment. In this study two other deagglomeration mechanisms were proposed, namely intense turbulent shear stress imparted by the fluid in the nozzle and impaction with the Mach disc near the exit of the nozzle. Explosive expansion was observed to have almost no effect on nozzle deagglomeration and subsequent mixing. It has been shown that the turbulent shear stress and the residence time under shear were the dominant factors related to agglomerate breakage, while impaction with the Mach disc has played a minimal role.

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