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- Title
- SYNTHESIS, PROCESSING AND CHARACTERIZATION OF NANOCRYSTALLINE TITANIUM DIOXIDE.
- Creator
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Qiu, Shipeng, Kalita, Samar, University of Central Florida
- Abstract / Description
-
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...
Show moreTitanium 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.
Show less - Date Issued
- 2006
- Identifier
- CFE0001432, ucf:47036
- Format
- Document (PDF)
- PURL
- http://purl.flvc.org/ucf/fd/CFE0001432
- Title
- INVESTIGATION OF THERMAL, ELASTIC AND LOAD-BIASED TRANSFORMATION STRAINS IN NITI SHAPE MEMORY ALLOYS.
- Creator
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Qiu, Shipeng, Vaidyanathan, Raj, University of Central Florida
- Abstract / Description
-
Polycrystalline NiTi shape memory alloys have the ability to recover their original, pre-deformed shape in the presence of external loads when heated through a solid-solid phase transformation from a lower-symmetry B19' martensite phase to a higher-symmetry B2 austenite phase. The strain associated with a shape memory alloy in an actuator application typically has thermal, elastic and inelastic contributions. The objective of this work was to investigate the aforementioned strains by...
Show morePolycrystalline NiTi shape memory alloys have the ability to recover their original, pre-deformed shape in the presence of external loads when heated through a solid-solid phase transformation from a lower-symmetry B19' martensite phase to a higher-symmetry B2 austenite phase. The strain associated with a shape memory alloy in an actuator application typically has thermal, elastic and inelastic contributions. The objective of this work was to investigate the aforementioned strains by recourse to in situ neutron diffraction experiments during selected combinations of heating, cooling and/or mechanical loading. The primary studies were conducted on polycrystalline Ni49.9Ti50.1 specimens on the Spectrometer for MAterials Research at Temperature and Stress (SMARTS) at Los Alamos National Laboratory. Quantitative information on the phase-specific strain, texture and phase fraction evolution was obtained from the neutron data using Rietveld refinement and single-peak analyses, and compared with macroscopic data from extensometry. First, the lattice strain evolution during heating and cooling in an unloaded sample (i.e., free-recovery experiment) was studied. The lattice strain evolution remained linear with temperature and was not influenced by intergranular stresses, enabling the determination of a thermal expansion tensor that quantified the associated anisotropy due to the symmetry of B19' NiTi. The tensor thus determined was subsequently used to obtain an average coefficient of thermal expansion that was consistent with macroscopic dilatometric measurements and a 30,000 grain polycrystalline self-consistent model. The accommodative nature of B19' NiTi was found to account for macroscopic shape changes lagging (with temperature) the start and finish of the transformation. Second, the elastic response of B19' martensitic NiTi variants during monotonic loading was studied. Emphasis was placed on capturing and quantifying the strain anisotropy which arises from the symmetry of monoclinic martensite and internal stresses resulting from intergranular constraints between individual variants and load re-distribution among variants as the texture evolved during variant reorientation and detwinning. The methodology adopted took into account both tensile and compressive loading given the asymmetric response in the texture evolution. Plane specific elastic moduli were determined from neutron measurements and compared with those determined using a self-consistent polycrystalline deformation model and from recently reported elastic stiffness constants determined via ab initio calculations. The comparison among the three approaches further helped understand the influence of elastic anisotropy, intergranular constraint, and texture evolution on the deformation behavior of polycrystalline B19' NiTi. Connections were additionally made between the assessed elastic properties of martensitic NiTi single crystals (i.e., the single crystal stiffness tensor) and the overall macroscopic response in bulk polycrystalline form. Lastly, the role of upper-cycle temperature, i.e., the maximum temperature reached during thermal cycling, was investigated during load-biased thermal cycling of NiTi shape memory alloys at selected combinations of stress and temperature. Results showed that the upper-cycle temperature, under isobaric conditions, significantly affected the amount of transformation strain and thus the work output available for actuation. With the objective of investigating the underlying microstructural and micromechanical changes due to the influence of the upper-cycle temperature, the texture evolution was systematically analyzed. While the changes in transformation strain were closely related to the evolution in texture of the room temperature martensite, retained martensite in the austenite state could additionally affect the transformation strain. Additionally, multiple thermal cycles were performed under load-biased conditions in both NiTi and NiTiPd alloys, to further assess and understand the role of retained martensite. Dimensional and thermal stabilities of these alloys were correlated with the volume fraction and texture of retained martensite, and the internal strain evolution in these alloys. The role of symmetry, i.e., B19' monoclinic martensite vs. B19 orthorhombic martensite in these alloys was also assessed. This work not only established a methodology to study the thermal and elastic properties of the low symmetry B19' monoclinic martensite, but also provided valuable insight into quantitative micromechanical and microstructural changes responsible for the thermomechanical response of NiTi shape memory alloys. It has immediate implications for optimizing shape memory behavior in the alloys investigated, with extension to high temperature shape memory alloys with ternary and quaternary elemental additions, such as Pd, Pt and Hf. This work was supported by funding from NASAÂÂ's Fundamental Aeronautics Program, Supersonics Project (NNX08AB51A) and NSF (CAREER DMR-0239512). It benefited additionally from the use of the Lujan Neutron Scattering Center at Los Alamos National Laboratory, which is funded by the Office of Basic Energy Sciences (Department of Energy) and is operated by Los Alamos National Security LLC under DOE Contract DE-AC52-06NA25396.
Show less - Date Issued
- 2010
- Identifier
- CFE0003362, ucf:48440
- Format
- Document (PDF)
- PURL
- http://purl.flvc.org/ucf/fd/CFE0003362
