Date of Award

Fall 2010

Document Type

Dissertation

Degree Name

Doctor of Philosophy in Materials Science and Engineering - (Ph.D.)

Department

Committee for the Interdisciplinary Program in Materials Science and Engineering

First Advisor

Rajesh N. Dave

Second Advisor

Zafar Iqbal

Third Advisor

Kwabena A. Narh

Fourth Advisor

S. Mitra

Fifth Advisor

Ecevit Atalay Bilgili

Abstract

Nanoparticles and nanocomposites offer unique properties that arise from their small size, large surface area, and the interactions of phases at their interfaces, and are attractive for their potential to improve performance of drugs, biomaterials, catalysts and other highvalue- added materials. However, a major problem in utilizing nanoparticles is that they often lose their high surface area due to grain growth. Creating nanostructured composites where two or more nanosized constituents are intimately mixed can prevent this loss in surface area, but in order to obtain homogeneous mixing, de-agglomeration of the individual nanoparticle constituents is necessary.

Due to high surface area, nano-particles form very large, fractal agglomerates. The structure of these agglomerates can have a large agglomerate composed of subagglomerates (SA), which itself consists of primary agglomerates (PA), that contain chain or net like nano-particle structures; typically sub-micron size. Thus the final agglomerate has a hierarchical, fractal structure, and depending upon the forces applied, it could break down to a certain size scale. The agglomerates can be fairly porous and fragile or they could be quite dense, based on primary particle size and its surface energy. Thus depending upon the agglomerate strength at different length scales, one could achieve deagglomeration and subsequent mixing at varying length scale. A better understanding of this can have a major impact on the field of nano-structured materials; thus the long term objective of this project is to gain fundamental understanding of deagglomeration and mixing of nano-agglomerates.

Dry mixing is in general not effective in achieving desired mixing at nanoscale, whereas wet mixing suffers from different disadvantages like nanomaterial of interest should be insoluble, has to wet the liquid, and involves additional steps of filtration and drying. This research examines the use of environmentally friendly a novel approach based on use of small magnetic particles as mixing media is introduced that achieves a high-degree of mixing at scales of about a micron. The method is tested for binary mixture of alumina/silica and silica/titania. Various parameters such as processing time, size of the magnets, and magnetic particle to powder mixed ratio are considered. Experiments are carried out in batch containers in liquid and dry mediums, as well as a fluidized bed set-up.

Homogeneity of Mixing (HoM), defined as the compliment of the Intensity of Segregation, was evaluated at the micron scale through field-emission scanning electron microscopy (FESEM) and the energy dispersive x-ray spectroscopy (EDS). Secondary electron images, along with elemental mappings, were used to visualize the change in agglomerate sizes. Compositional percent data of each element were obtained through an EDS spatial distribution point analysis and used to obtain quantitative analysis on the homogeneity of the mixture. The effect of magnet impaction on mixing quality was examined on the HoM of binary mixtures. The research shows that HoM improved with magnetically assisted impaction mixing techniques indicating that the HoM depends on the product of processing time with the number of magnets. In a fluidized bed set-up, MAIM not only improved dispersion, but it was also found that the magnetic particles served to break down the larger agglomerates, to reduce the minimum fluidization velocity, to delay the onset of bubbling, and to convert the fluidization behavior of ABF powder to APF. Thus MAIM techniques may be used to achieve mixing of nanopowders at a desired HoM through adjusting the number of magnets and processing time; and its inherent advantages are its simplicity, an environmentally benign operation, and reduced cost as compared with wet mixing techniques.

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