The Phase- and Shape-Controlled Synthesis of Metal Sulfide Nano- and Micromaterials

Abstract

Chapter 1. Contains a literature review focusing on inorganic nano- and micromaterials with an emphasis on metal sulfides. The topics discussed include: the unique size and shape controlled properties of these materials, the processes known to govern their crystallisation, synthetic strategies developed to influence their structure, and the harmful impact these strategies may have on the environment. Chapter 2. Contains details of the experimental methods employed in this thesis; with a particular emphasis on the design, commissioning and testing of the novel hydrothermal injection reactor; which was constructed to address the environmental concerns discussed in the previous chapter. Also presented is the relevant theory concerning each of the analytical techniques used in this thesis. Chapter 3. The size, shape and phase control abilities of the hydrothermal injection reactor are tested in this chapter. Cadmium sulfide, a polymorphic material with extensively well studied crystallisation behaviour in both hot-injection and hydrothermal synthesis, was selected as the test subject. Chapter 4. Mapping of the synthetic CdS landscape is further explored in this chapter. This a achieved by expanding the list of reaction variables applied to CdS synthesis in both the hydrothermal injection reactor and in conventional hydrothermal methods. This chapter also assess the viability of rapidly processing and interpreting the vast quantity of X-ray diffraction data built up over the course of this synthetic exploration, by applying a statistical technique known as principal component analysis. Chapter 5. This chapter presents the development of robust synthetic route to hollow copper sulfide microspheres via a sacrificial sulfur template. This process also yielded a variety of complex, plant-like morphologies. The evolution of these morphologies is discussed in detail. Chapter 6. This chapter contains a brief outline of the planned future work stemming from this thesis, with an emphasis on redesigns of the hydrothermal injection reactor, the synthesis of additional target materials via the reactor and a deeper exploration of the templated metal sulfide hollow microspheres.