The work contained within this thesis is concerned with the further innovation and the development of apparatus for the electrospinning method which in its most basic form is used to produce and deposit small diameter fibres of many polymers and other materials in a mat structure with random orientation of the deposited fibres. The focus of the innovation is concerned with expanding the ways of collecting these fibres by implementing newly developed techniques, building upon the conventional electrospinning technique and literature to create an advanced electrospinning system. The innovation can be split into the following areas of study: Development of apparatus for the control of the electrospinning process, apparatus for the control of the deposition of the fibres and the development of apparatus for coating conductive wires and other materials with electrospun polymer fibres. Each of the apparatus designed and tested within this work build upon previous examples of experimental apparatus created by other groups as discussed in the following chapters. The apparatus developed and described is a combination of incremental improvement and previously untried combinations of the work that as gone before. All the apparatus developed for use as part of the ectrospinning process were designed to be easily improved incrementally and the development cycles to achieve the final apparatus shown have also been included. The novelty within this work is concerned the development of apparatus for use with the electrospinning process and with the overall supporting systems that have been developed alongside them. The novelty of the apparatus used in conjunction with the electrospinning process includes a remotely controlled fibre printer that can print tracks of electrospun fibres creating shapes and patterns. The development of the apparatus is discussed in detail covering all mechanical and electronic considerations and design decisions. The final apparatus is shown to operate as desired with polymer tracks thicknesses of 20mm in width achieved. A novel apparatus was developed using multiple ground electrodes that were digitally controlled in conjunction with the electrospinning method to achieve a new method of layering aligned fibres in layers with alternating orientations. Also the apparatus can be used in an alternate mode which allows the selective electrospinning of aligned bundles of fibres between multiple electrodes in user defined patterns. The apparatus is shown to achieve good polymer fibre alignment between electrodes and also is shown to work as deigned in regard to the layering of the aligned fibres. An alternate way of using the apparatus is successfully demonstrated allowing the selective patterning of deposited fibre bundles between multiple electrodes. A polymer coating apparatus was also developed to extend the electrospinning method to create core-shell fibres as part of a larger system developed for creating smart textiles and fibrous sensors. The novel electrospinning apparatus is shown to be able to uniformly coat both the circumference and along the length over a comparatively long length of core-shell fibre. A deposition thickness of polymer between 36 μm and 242 μm was achieved by changing the coating speed. An alignment of the electrospun fibres along the length on the core wires is also shown and discussed. The core-shell fibres developed are used in conjunction with another developed apparatus piece that weaves a series of wires around the outer shell to create a three layer device consisting of an outer electrically conductive layer, an electrospun polymer layer and an electrically conductive core. The system is shown to successfully create these three layer devices.

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The continuous microreactor-assisted solution deposition (MASD) process was used for the deposition of CdS thin films on fluorine-doped tin oxide (FTO) glass. The MASD system, including a T-junction micromixer and a microchannel heat exchanger is capable of isolating the homogeneous particle precipitation from the heterogeneous surface reaction. The results show a dense nanocrystallite CdS thin films with a preferred orientation at (111) plane. Focused-ion-beam was used for TEM specimen preparation to characterize the interfacial microstructure of CdS and FTO layers. The band gap of the microreactor-assisted deposited CdS film was determined at 2.44 eV. X-ray Photon Spectroscopy show the bindings of energies of Cd 3d₃/₂, Cd 3d₅/₂, S 2p₃/₂ and S 2p₁/₂ at 411.7 eV, 404.8 eV, 162.1 eV, and 163.4 eV, respectively. The film growth kinetics was studied by measuring the film thickness deposited from 1 minute to 15 minutes in physical (FIB-TEM) and optical (reflectance spectroscopy) approaches. A growth model that accounts for the residence time in the microchannel using empirical factor (η) obtained from previous reported experimental data. Applying this factor in the proposed modified growth model gives a surface reaction rate of 1.61*10⁶ cm⁴ mole⁻¹s⁻¹, which is considerable higher than the surface reaction rates obtained from the batch CBD process. With the feature of separating homogeneous and heterogeneous surface reaction, the MASD process provides the capability to tailor the surface film growth rate and avoid the saturation growth regime in the batch process. An in situ spectroscopy technique was used to measure the UV-Vis absorption spectra of CdS nanoparticles formed within the continuous flow microreactor. The spectra were analyzed by fitting the sum of three Gaussian functions and one exponential function in order to calculate the nanoparticle size. This deconvolution analysis shows the formation of CdS nanoparticles range from 1.13 nm to 1.26 nm using a residence time from 0.26 s to 3.96 s. Barrier controlled coalescence mechanism seems to be a reasonable model to explain the experimental UV-Vis data obtained from the continuous flow microreactor, with a rate constant k' value of 2.872 s⁻¹. Using CFD, low skewness value of the RTD curve at high flow rate (short τ) suggests good radial mixing at high flow rate is responsible for the formation of smaller CdS nanoparticles with a narrower size distribution. The combination of CdS nanoparticle solution with MASD process resulted in the hindrance of CdS thin film deposition. It is hypothesized that the pre-existing sulfide (S²⁻) ions and CdS nanoparticles changes the chemical species equilibrium of thiourea hydrolysis reaction. Consequently, the lack of thiourea slows down the heterogeneous surface reaction. To test the scalability of the MASD process, a flow cell and reel-to-reel (R2R)-MASD system were setup and demonstrated for the deposition of CdS films on the FTO glass (6" x 6") substrate. The film deposition kinetics was found to be sensitive to the flow conditions within the heat exchanger and the substrate flow cell. The growth kinetics of the CdS films deposited by R2R-MASD process was investigated by with a deposition time of 2.5 min, 6.3 min, and 9 min. In comparison with the continuous MASD process, the growth rate in R2R-MASD is higher, however more difficult to obtain a linear relationship with the deposition time. / Graduation date: 2012 / Access restricted to the OSU Community at author's request from Jan. 13, 2012 - Jan. 13, 2013