Diblock copolymers have many interesting properties, which first and foremost include their ability to self-assemble into various ordered, regularly spaced domains with nanometer-scale feature sizes. The work in this dissertation can be logically divided into two parts - the first and the majority of this work describes the phase behavior of certain block copolymer systems, and the second discusses real applications possible with block copolymer templates. Many compressible fluids have solvent-like properties dependent on fluid pressure and can be used as processing aids similar to liquid solvents. Here, compressed CO2 was shown to swell several thin homopolymer films, including polystyrene and polyisoprene, as measured by high pressure ellipsometry at elevated temperatures and pressures. The ellipsometric technique was modified to produce accurate data at these conditions through a custom pressure vessel design. The order-disorder transition (ODT) temperatures of several poly(styrene-b-isoprene) diblock copolymers were also investigated by static birefringence when dilated with compressed CO2. Sorption of CO2 in each copolymer resulted in significant depressions of the ODT temperature as a function of fluid pressure, and the data above was used to estimate the quantitative amount of solvent in each of the diblock copolymers. These depressions were not shown to follow dilution approximation, and showed interesting, exaggerated scaling of the ODT at near-bulk polymer concentrations. The phase behavior of block copolymer surfactants was studied when blended with polymer or small molecule additives capable of selective hydrogen bonds. This work used small angle X-ray scattering (SAXS) to identify several low molecular weight systems with strong phase separation and ordered domains as small as 2-3 nanometers upon blending. One blend of a commercially-available surfactant with a small molecule additive was further developed and showed promise as a thin-film pattern transfer template. In this scenario, block copolymer thin films on domain thick with self-assembled feature sizes of only 6-7 nm were used as plasma etch resists. Here the block copolymer's pattern was successfully transferred into the underlying SiO2 substrate using CF4-based reactive ion etching. The result was a parallel, cylindrical nanostructure etched into SiO2.

Neutron detection is important in several fields, especially detection of illicit nuclear material. Historically, 3He has been the basis for these technologies. Modern realities have necessitated the development of new technologies and the exploration of new materials to meet this need. One potential solution is known as capture-gating, which is a measurement approach that is good at differentiating between incident neutrons and gamma rays. The key issue is that materials used in current capture-gating devices can suffer from poor optical performance. This is due to the fact that the these detectors, whether composed of a heterogeneous or homogeneous mixture of materials, are made of dissimilar materials. In the homogeneous case, this frequently results in a cloudy material (e.g. lithium-gadolinium-borate crystals), while heterogeneous cases suffer from index mismatch (e.g. glass inside a plastic scintillator). The goal of this thesis is material development and processing toward an index-matched, gadolinium-based glass, heterogeneous capture-gated neutron detector. This involved identifying the refractive index range of known gadolinium glasses and the development of polystyrene (PS) and polyvinyl toluene (PVT) co-polymers with a range of refractive indices. Specifically 1:3, 1:1, and 3:1 PS:PVT ratios were manufactured and their refractive indices were compared to those of pure PS and PVT. Two methods for uniform glass dispersion were explored; the use of a rotisserie oven and the use of centrifugal planetary mixer. Ellipsometry, refractometry, and spectroscopic transmission were all performed to optically evaluate the manufactured polymers and polymer/glass composites. The ability to produce a PS/PVT copolymer with a refractive index in the range of known gadolinium glasses was demonstrated. In addition, the benefit of matching the refractive indices when producing a glass/polymer composite was explored and the effect of index mismatch was observed. The ability to predict the refractive index of a PS/PVT blend was demonstrated but can still be improved upon. While a novel index-matched gadolinium-based heterogeneous capture-gated neutron detector was not developed as part of this work, progress was made on all material aspects to further develop a detector meeting that description. More work still needs to be done in fine tuning the index match of the glass and polymer components, in determining the ideal method of glass dispersion, and in producing larger samples.

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