Titanium dioxide, Sol-gel, Nanopowder, Synthesis, Mechanical properties
Titanium dioxide (TiO2), one of the basic ceramic materials, has found a variety of applications in industry and in our daily life. It has been shown that particle size reduction in this system, especially to nano regime, has the great potential to offer remarkable improvement in physical, mechanical, optical, biological and electrical properties. This thesis reports on the synthesis and characterization of the nanocrystalline TiO2 ceramic in details. The study selected a simple sol-gel synthesis process, which can be easily controlled and reproduced. Titanium tetraisopropoxide, isopropanol and deionized water were used as starting materials. By careful control of relative proportion of the precursor materials, the pH and peptization time, TiO2 nanopowder was obtained after calcination at 400oC. The powder was analyzed for its phases using X-ray powder diffraction (XRD) technique. Crystallite size, powder morphology and lattice fringes were determined using high-resolution transmission electron microscopy (HR-TEM). Differential scanning calorimetry (DSC) and thermal gravimetric analysis (TGA) were used to study the thermal properties. As-synthesized powder was uniaxially compacted and sintered at elevated temperature of 1100-1600oC to investigate the effects of sintering on nano powder particles, densification behavior, phase evolution and mechanical properties. Microstructure evolution as a function of sintering temperature was studied by scanning electron microscopy (SEM). The results showed that 400oC was an optimum calcination temperature for the as-synthesized TiO2 powder. It was high enough to achieve crystallization, and at the same time, helped minimize the thermal growth of the crystallites and maintain nanoscale features in the calcined powder. After calcination at 400oC (3 h), XRD results showed that the synthesized nano-TiO2 powder was mainly in single anatase phase. Crystallite size was first calculated through XRD, then confirmed by HR-TEM, and found to be around 5~10 nm. The lattice parameters of the nano-TiO2 powder corresponding to this calcination temperature were calculated as a=b=0.3853 nm, c=0.9581 nm, α=β=γ=90o through a Rietveld refinement technique, which were quite reasonable when comparing with the literature values. Considerable amount of rutile phase had already formed at 600oC, and the phase transformation from anatase to rutile fully completed at 800oC. The above rutilization process was clearly recorded from XRD data, and was in good corresponding to the DSC-TGA result, in which the broad exothermic peak continued until around 800oC. Results of the sintered TiO2 ceramics (1100oC-1600oC) showed that, the densification process continued with the increase in sintering temperature and the highest geometric bulk sintered density of 3.75 g/cm3 was achieved at 1600oC. The apparent porosity significantly decreased from 18.5% to 7.0% in this temperature range, the trend of which can be also clearly observed in SEM micrographs. The hardness of the TiO2 ceramics increased with the increase in sintering temperature and the maximum hardness of 471.8±30.3 HV was obtained at 1600oC. Compression strength increased until 1500oC and the maximum value of 364.1±10.7 MPa was achieved; after which a gradual decrease was observed. While sintering at ambient atmosphere in the temperature range of 1100oC-1600oC helped to improve the densification, the grain size also increased. As a result, though the sintered density at 1600oC was the highest, large and irregular-shaped grains formed at this temperature would lead to the decrease in the compression strength.
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Master of Science in Materials Science and Engineering (M.S.M.S.E.)
College of Engineering and Computer Science
Mechanical, Materials and Aerospace Engineering;
Materials Science and Engineering
Length of Campus-only Access
Masters Thesis (Open Access)
Qiu, Shipeng, "Synthesis, Processing And Characterization Of Nanocrystalline Titanium Dioxide" (2006). Electronic Theses and Dissertations. 913.