In this thesis, a novel in-situ method for incorporating nanoscale ceramic particles into metal has been developed. The ceramic phase is introduced as an organic-polymer precursor that pyrolyzes in-situ to produce a ceramic phase within the metal melt. The environment used to shield the melt from burning also protects the organic precursor from oxidation. The evolution of volatiles (predominantly hydrogen) as well as the mechanical stirring causes the polymer particles to fragment into nanoscale dispersions of a ceramic phase. These “Polymer-based In-situ Process-Metal Matrix Composites” (PIP-MMCs) are likely to have great generality, because many different kinds of organic precursors are commercially available, for producing oxides, carbides, nitrides, and borides. Also, the process would permit the addition of large volume fractions of a ceramic phase, enabling nanostructural design, and production of MMCs with a wide range of mechanical properties, meant especially for high temperature applications. An important and noteworthy feature of the present process, which distinguishes it from other methods, is that all the constituents of the ceramic phase are built into the organic molecules of the precursor (e.g., polysilazanes contain silicon, carbon, and nitrogen); therefore, a reaction between the polymer and the host metal is not required to produce the dispersion of the refractory phase. The polymer precursor powder, with a mean particle size of 31.5 µm, was added equivalent to 5 and 10 weight % of the melt (pure magnesium) by a liquid metal stir-casting technique. SEM and OM microstructural observations show that in the cast structure the pyrolysis products are present in the dendrite boundary region in the form of rod/platelets having a thickness of 100 to 200 nm. After extrusion the particles are broken down into fine particles, having a size that is comparable to the thickness of the platelets, in the 100 to 200 nm range, and are distributed more uniformly. In addition, limited TEM studies revealed the formation of even finer particles of 10-50 nm. X-ray diffraction analysis shows the presence of a small quantity of an intermetallic phase (Mg2Si) in the matrix, which is unintended in this process. There was a significant improvement in mechanical properties of the PIP-MMCs compared to the pure Mg. These composites showed higher macro-and micro-hardness. The composite exhibited better compressive strength at both room temperature and at elevated temperatures. The increase in the density of PIP-composites is less than 1% of Mg. Five weight percent of the precursor produced a two-fold increase in the room-temperature yield strength and reduced the steady state creep rate at 723 K by one to two orders of magnitude. PIP-MMCs showed higher damping capacity and modulus compared to pure Mg, with the damping capacity increasing by about 1.6 times and the dynamic modulus by 11%-16%. PIP-composites showed an increase in the sliding wear resistance by more than 25% compared to pure Mg.

M. Tech. (Department of Chemistry, Faculty of Applied and Computer Sciences), Vaal University of Technology. / In chemical bath deposition (CBD) method, deposition of metal chalcogenide semiconducting thin films occurs due to substrate maintained in contact with a dilute chemical bath containing metal and chalcogenide ions. Semiconducting nickel sulphide (NiS) and iron sulphide (FeS) thin films have been prepared on a glass substrate by varying the deposition parameters such as the concentration of solutions, deposition time, temperature and pH. Multi-layered thin films were deposited on glass substrate and the spin-cast conductive polymer, poly (3.4-ethylenedioxythiopene) polystyrene sulfonate (PEDOT: PSS) was intercalated. The characterization of the films was carried out using UV-Vis spectroscopy, scanning electron microscopy (SEM) coupled with energy-dispersive X-ray spectroscopy (EDX), atomic force microscopy (AFM) and X-ray diffraction (XRD). Single layer nickel sulphide was deposited at room temperature, pH 10 and the deposition period of 3 hours, triethanolamine was used as the complexing agent. Iron sulphide was deposited for 6 hours at 70 °C with the pH of 2.5 using EDTA as a complexing agent. Generally the iron and nickel sulphide were prepared from their respective nickel or iron salt and the thiourea or thiosulfate as a source of sulphide ions in solution. SEM and AFM results show that the FeS film is evenly coated and has uniform grain size with the roughness of ~22.4 nm and thickness of ~23.8 nm. The optical absorption analysis of FeS showed the band gap energy of ~2.9 eV which blue shifted from the bulk. The EDX analysis confirms the compositions of iron and sulphur in FeS films. XRD pattern showed amorphous films for both FeS and NiS thin films due to the amorphous nature of the glass substrate. The optical data of NiS film were analysed and exhibited the band gap energy of ~3.5 eV and ~3.3 eV for successive ionic layer adsorption and reaction (SILAR), which is the modified CBD, both blue shifted from the bulk. The films were observed to have thickness value of ~35.7 nm and ~2.3 nm SILAR with the roughness of ~112.5 nm and ~35.4 nm SILAR from AFM results. SEM confirmed the uniformly distributed film presented by AFM analysis. The chemical composition of Ni and S were confirmed by EDX spectra. The PEDOT: PSS was intercalated between the FeS as the first layer and NiS as the top layer which gave the thickness of ~18.7 nm and roughness of ~115.2 nm from AFM analysis. PEDOT: PSS acted as a passive layer that protects and stabilize the FeS layer and NiS as the third active layer which enhanced the optical absorption of the film when using SILAR method for solar application.