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Abstract
There is currently a worldwide effort for advances in micro and nanotechnologies due to their high potential for technological applications in fields such as microelectromechanical systems (MEMS), organic electronics and structural microstructures for aerospace. In these applications, carbon nanotube/polymer nanocomposites represent interesting material options compared to conventional resins for their enhanced mechanical and electrical properties. However, several significant scientific and technological challenges must first be overcome in order to rapidly and cost-effectively fabricate nanocomposite-based microdevices. Fabrication techniques have emerged for fabricating one- of two-dimensional (1D/2D) nanocomposite structures but few techniques are available for three-dimensional (3D) nanocomposite structures. The overall objective of this thesis is the development of a manufacturing technique allowing the fabrication of 3D structures of single-walled carbon nanotube (C-SWNT)/polymer nanocomposite.
This thesis reports the development of a direct-write fabrication technique that greatly extends the fabrication space for 3D carbon nanotube/polymer nanocomposite structures. The UV-assisted direct-write (UV-DW) technique employs the robotically-controlled micro-extrusion of a nanocomposite filament combined with a UV exposure that follows the extrusion point. Upon curing, the increased rigidity of the extruded filament enables the creation of multi-directional shapes along the trajectory of the extrusion point.
The C-SWNT material is produced by laser ablation of a graphite target and purified using a nitric acid reflux. The as-grown and purified material is characterized under transmission electron microscopy and Raman spectroscopy. The purification procedure successfully graphed carboxylic groups on the surface of the C-SWNTs, shown by X-ray photoelectron spectroscopies. An incorporation procedure in the polymer is developed involving a non-covalent functionalization of the nanotubes by zinc protoporphyrin IX molecule and high shear mixing using a three-roll mill. The incorporation of the C-SWNTs into the resin led to an increase of the viscosity and the apparition of a shear thinning behaviour, characterized by capillary viscometry.
The nanocomposite UV-curing behavior is characterized under differential scanning calorimetry coupled with a UV source. A further adjustment of the shear thinning behavior using fumed silica enabled the UV-DW fabrication of microbeams. Mechanical characterization reveals significant increase in both strength (by ∼64%) and modulus (by more than 15 times). These mechanical enhancements are attributed to both the covalent and the non-covalent functionalizations of the C-SWNTs. Nanocomposite spring networks composed of three micro-coils fabricated using the UV-DW technique are mechanically tested under compression and show a rigidity of ∼11.5 mN/mm. A micro-coil is also deposited between two uneven electrodes and a 10−6 S/cm electrical conductivity is measured. Nanocomposite scaffold structures are also deposited using the UV-DW technique.
This thesis also reports the fabrication of 3D micro structured beams reinforced with the C-SWNT/polymer nanocomposite by using an approach based on the infiltration of 3D microfluidic networks. The 3D microfluidic network is first fabricated by the direct-write assembly method, which consists of the robotized deposition of fugitive ink filaments on an epoxy substrate, forming a 3D micro structured scaffold. After encapsulating the 3D micro-scaffold structure with an epoxy resin, the fugitive ink is liquefied and removed, resulting in a 3D network of interconnected microchannels. This microfluidic network is then infiltrated by the C-SWNT/polyurethane nanocomposite and subsequently cured. The final samples consist of rectangular beams having a complex 3D-skeleton structure of C-SWNT/polyrner nanocomposite fibers, adapted to offer better performance under flexural solicitation. Dynamic mechanical analysis in flexion show an increase of 12.5% in the storage modulus under 35°C compared to the resin infiltrated beams.
The manufacturing techniques demonstrated here, i.e. UV assisted direct writing and the infiltration of 3D microfluidic networks, open new prospects for the achievement of 3D reinforced micro structures that could find application in organic electronics, MEMS, sensor, tissue engineering scaffolds and aerospace.
