Current Search: transmission electron microscopy (x)
View All Items
(1 - 5 of 5)
- Title
- TRANSMISSION ELECTRON MICROSCOPY STUDIES IN SHAPE MEMORY ALLOYS.
- Creator
-
TIYYAGURA, MADHAVI, VAIDYANATHAN, RAJ, University of Central Florida
- Abstract / Description
-
In NiTi, a reversible thermoelastic martensitic transformation can be induced by temperature or stress between a cubic (B2) austenite phase and a monoclinic (B19') martensite phase. Ni-rich binary compositions are cubic at room temperature (requiring stress or cooling to transform to the monoclinic phase), while Ti-rich binary compositions are monoclinic at room temperature (requiring heating to transform to the cubic phase). The stress induced transformation results in the superelastic...
Show moreIn NiTi, a reversible thermoelastic martensitic transformation can be induced by temperature or stress between a cubic (B2) austenite phase and a monoclinic (B19') martensite phase. Ni-rich binary compositions are cubic at room temperature (requiring stress or cooling to transform to the monoclinic phase), while Ti-rich binary compositions are monoclinic at room temperature (requiring heating to transform to the cubic phase). The stress induced transformation results in the superelastic effect, while the thermally induced transformation is associated with strain recovery that results in the shape memory effect. Ternary elemental additions such as Fe can additionally introduce an intermediate rhombohedral (R) phase between the cubic and monoclinic phase transformation. This work was initiated with the broad objective of connecting the macroscopic behavior in shape memory alloys with microstructural observations from transmission electron microscopy (TEM). Specifically, the goals were to examine (i) the effect of mechanical cycling and plastic deformation in superelastic NiTi; (ii) the effect of thermal cycling during loading in shape memory NiTi; (iii) the distribution of twins in martensitic NiTi-TiC composites; and (iv) the R-phase in NiTiFe. Both in situ and ex situ lift out focused ion beam (FIB) and electropolishing techniques were employed to fabricate shape memory alloy samples for TEM characterization. The Ni rich NiTi samples were fully austenitic in the undeformed state. The introduction of plastic deformation (8% and 14% in the samples investigated) resulted in the stabilization of martensite in the unloaded state. An interlaying morphology of the austenite and martensite was observed and the martensite needles tended to orient themselves in preferred orientations. The aforementioned observations were more noticeable in mechanically cycled samples. The observed dislocations in mechanically cycled samples appear to be shielded from the external applied stress via mismatch accommodation since they are not associated with unrecoverable strain after a load-unload cycle. On application of stress, the austenite transforms to martensite and is expected to accommodate the stress and strain mismatch through preferential transformation, variant selection, reorientation and coalescence. The stabilized martensite (i.e., martensite that exists in the unloaded state) is expected to accommodate the mismatch through variant reorientation and coalescence. On thermally cycling a martensitic NiTi sample under load through the phase transformation, significant variant coalescence, variant reorientation and preferred variant selection was observed. This was attributed to the internal stresses generated as a result of the thermal cycling. A martensitic NiTi-TiC composite was also characterized and the interface between the matrix and the inclusion was free of twins while significant twins were observed at a distance away from the matrix-inclusion interface. Incorporating a cold stage, diffraction patterns from NiTiFe samples were obtained at temperatures as low as -160ºC. Overall, this work provided insight in to deformation phenomena in shape memory materials that have implications for engineering applications (e.g., cyclic performance of actuators, engineering life of superelastic components, stiffer shape memory composites and low-hysteresis R-phase based actuators). This work was supported in part by an NSF CAREER award (DMR 0239512).
Show less - Date Issued
- 2005
- Identifier
- CFE0000500, ucf:46462
- Format
- Document (PDF)
- PURL
- http://purl.flvc.org/ucf/fd/CFE0000500
- Title
- Study of Surface Passivation Behavior of Crystalline Silicon Solar Cells.
- Creator
-
Ali, Haider, Schoenfeld, Winston, Coffey, Kevin, Gaume, Romain, Thomas, Jayan, Chanda, Debashis, University of Central Florida
- Abstract / Description
-
To achieve efficiencies approaching the theoretical limit of 29.4% for industrially manufactured solar cells based on crystalline silicon, it is essential to have very low surface recombination velocities at both the front and rear surfaces of the silicon substrate. Typically, the substrate surfaces feature contacted and uncontacted regions, and recombination should be limited for both to maximize the energy conversion efficiency.Uncontacted silicon surfaces are often passivated by the...
Show moreTo achieve efficiencies approaching the theoretical limit of 29.4% for industrially manufactured solar cells based on crystalline silicon, it is essential to have very low surface recombination velocities at both the front and rear surfaces of the silicon substrate. Typically, the substrate surfaces feature contacted and uncontacted regions, and recombination should be limited for both to maximize the energy conversion efficiency.Uncontacted silicon surfaces are often passivated by the deposition of silicon nitride (SiNx) or an aluminum oxide film with SiNx as capping layer (Al2O3/SiNx stack). Further, proper surface preparation and cleaning of Si wafers prior to deposition also plays an important role in minimizing surface recombination. In the present work, the effect of various cleans based on different combinations of HCl, HF, HNO3, and ozonated deionized water (DIO3) on surface passivation quality of boron-diffused and undiffused {100} n-type Cz Si wafers was studied. It was observed that for SiNx passivated Si, carrier lifetime was strongly influenced by cleaning variations and that a DIO3-last treatment resulted in higher lifetimes. Moreover, DIO3+HF+HCl?HF?DIO3 and HNO3?HF?HNO3 cleans emerged as potential low-cost alternatives to HCl/HF clean in the photovoltaics industry.Transmission electron microscopy (TEM) studies were carried out to get insight into the origin of variation in carrier lifetimes for different cleans. Changes in the surface cleans used were not found to have a significant impact on Al2O3/SiNx passivation stacks.ivHowever, an oxide-last cleaning step prior to deposition of SiNx passivation layers was found to create a 1-2 nm SiOx tunnel layer resulting in excellent carrier lifetimes.For contacted regions, low surface recombination can be achieved using passivated carrier selective contacts, which not only passivate the silicon surface and improve the open circuit voltage, but are also carrier selective. This means they only allow the majority carrier to be transported to the metal contacts, limiting recombination by reducing the number of minority carriers. Typically, carrier selectivity is achieved using a thin metal oxide layer, such as titanium oxide (TiO2) for electron-selective contacts and molybdenum oxide (MoOx) for hole-selective contacts. This is normally coupled with a very thin passivation layer (e.g., a-Si:H, SiOx) between the silicon wafer and the contact.In the present work, TiO2-based electron-selective passivated rear contacts were investigated for n-type c-Si solar cells. A low efficiency of 9.8% was obtained for cells featuring a-Si:H/TiO2 rear contact, which can be attributed to rapid degradation of surface passivation of a-Si:H upon FGA at 350(&)deg;C due to hydrogen evolution leading to generation of defect states which increases recombination and hence a much lower Voc of 365 mV is obtained. On the other hand, 21.6% efficiency for cells featuring SiO2/TiO2 rear contact is due to excellent passivation of SiO2/TiO2 stack upon FGA anneal, which can be attributed to the presence of 1-2 nm SiO2 layer whose passivation performance improves upon FGA at 350(&)deg;C whereas presence of large number of oxygen vacancies in TiO2-x reduces rear contact resistivity.vLikewise, MoOx-based contacts were investigated as hole-selective front contacts for an n-type cell with a boron-doped emitter. It has been previously reported that cell efficiencies up to 22.5% have been achieved with silicon heterojunction solar cells featuring a front contact wherein MoOx is inserted between a-Si:H(i) and hydrogenated indium oxide (IO:H). However, device performance and FF degrades upon annealing beyond 130(&)deg;C. In this work, contact resistivity measurements by TLM technique in combination with TEM studies revealed that degradation of device performance is due to oxygen diffusion into MoOx upon annealing in air which reduces concentration of oxygen vacancies in MoOx and increases contact resistivity. The increase in contact resistivity reduces FF resulting in deterioration of device performance.
Show less - Date Issued
- 2017
- Identifier
- CFE0006554, ucf:51351
- Format
- Document (PDF)
- PURL
- http://purl.flvc.org/ucf/fd/CFE0006554
- Title
- CHARACTERIZATION OF MICROSTRUCTURAL AND CHEMICAL FEATURES IN CU-IN-GA-SE-S-BASED THIN-FILM SOLAR CELLS.
- Creator
-
Halbe, Ankush, Heinrich, Helge, University of Central Florida
- Abstract / Description
-
Thin-film solar cells are potentially low-cost devices to convert sunlight into electricity. Improvements in the conversion efficiencies of these cells reduce material utilization cost and make it commercially viable. Solar cells from the Thin-Film Physics Group, ETH Zurich, Switzerland and the Florida Solar Energy Center (FSEC), UCF were characterized for defects and other microstructural features within the thin-film structure and at the interfaces using transmission electron microscopy ...
Show moreThin-film solar cells are potentially low-cost devices to convert sunlight into electricity. Improvements in the conversion efficiencies of these cells reduce material utilization cost and make it commercially viable. Solar cells from the Thin-Film Physics Group, ETH Zurich, Switzerland and the Florida Solar Energy Center (FSEC), UCF were characterized for defects and other microstructural features within the thin-film structure and at the interfaces using transmission electron microscopy (TEM). The present thesis aims to provide a feedback to these groups on their deposition processes to understand the correlations between processing, resulting microstructures, and the conversion efficiencies of these devices. Also, an optical equipment measuring photocurrents from a solar cell was developed for the identification of defect-prone regions of a thin-film solar cell. The focused ion beam (FIB) technique was used to prepare TEM samples. Bright-field TEM along with scanning transmission electron microscopy (STEM) and energy dispersive X-ray spectroscopy (EDS) including elemental distribution line scans and maps were extensively used for characterizing the absorber layer and interfaces both above and below the absorber layer. Energy-filtered transmission electron microscopy (EFTEM) was applied in cases where EDS results were inconclusive due to the overlap of X-ray energies of certain elements, especially molybdenum and sulfur. Samples from ETH Zurich were characterized for changes in the CIGS (Cu(In,Ga)Se2) microstructure due to sodium incorporation from soda-lime glass or from a post-deposition treatment with NaF as a function of CIGS deposition temperature. The CIGS-CdS interface becomes smoother and the small columnar CIGS grains close to the Mo back contact disappear with increasing CIGS deposition temperature. At 773 K the two sodium incorporation routes result in large differences in the microstructures with a significantly larger grain size for the samples after post-deposition Na incorporation. Porosity was observed in the absorber layer close to the back contact in the samples from FSEC. The reason for porosity could be materials evaporation in the gallium beam of the FIB or a processing effect. The porosity certainly indicates heterogeneities of the composition of the absorber layer near the back contact. A Mo-Se rich layer (possibly MoSe2) was formed at the interface between CIGS/CIGSS and Mo improving the quality of the junction. Other chemical heterogeneities include un-sulfurized Cu-Ga deposits, residual Se from the selenization/ sulfurization chamber in CIGS2 and the formation of Cu-rich regions which are attributed to decomposition effects in the Ga beam of the FIB. Wavy absorber surfaces were observed for some of the cells with occasional discontinuities in the metal grids. The 50 nm thick CdS layer, however, remained continuous in all the samples under investigation. For a sample with a transparent back contact, a 10 nm Mo layer was deposited on ITO (indium tin oxide) before deposition of the CIGS2 (Cu(In,Ga)S2) layer. EFTEM maps indicate that a MoS2 layer does not form for such a Mo/MoS2-ITO back contact. Instead, absorber layer material diffuses through the thin Mo layer onto the ITO forming two layers of CIGS2 on either side of Mo with different compositions. Furthermore, an optical beam induced current (OBIC) system with micron level resolution was successfully developed and preliminary photocurrent maps were acquired to microscopically identify regions within a thin-film solar cell with undesirable microstructural features. Such a system, when fully operational, will provide the means for the identification of special regions from where samples for TEM analysis can be obtained using the FIB technique to study specifically the defects responsible for local variations in solar cell properties.
Show less - Date Issued
- 2006
- Identifier
- CFE0001022, ucf:46807
- Format
- Document (PDF)
- PURL
- http://purl.flvc.org/ucf/fd/CFE0001022
- Title
- SYNTHESIS AND CHARACTERIZATION OF STABLE AND METASTABLE PHASES IN Ni- AND Fe-BASED ALLOY SYSTEMS BY MECHANICAL ALLOYING.
- Creator
-
Al-Joubori, Ahmed, Challapalli, Suryanarayana, Vaidyanathan, Raj, Gou, Jihua, Bai, Yuanli, Lin, Kuo-Chi, University of Central Florida
- Abstract / Description
-
Mechanical Alloying (MA) is a process that involves repeated cold welding, fracturing and rewelding of powder particles in a high-energy ball mill and has been used extensively to synthesize both stable (equilibrium) and metastable phases in a number of alloy systems. This is due to its ability to achieve many effects simultaneously, viz., reduction in grain size, introduction of a variety of crystal defects, disordering of the lattice, and modifying the crystal structures of materials; all...
Show moreMechanical Alloying (MA) is a process that involves repeated cold welding, fracturing and rewelding of powder particles in a high-energy ball mill and has been used extensively to synthesize both stable (equilibrium) and metastable phases in a number of alloy systems. This is due to its ability to achieve many effects simultaneously, viz., reduction in grain size, introduction of a variety of crystal defects, disordering of the lattice, and modifying the crystal structures of materials; all these allowing alloying and phase transformations to occur in powders. In this Dissertation, we have synthesized a number of different alloy phases in Ni- and Fe-based alloy systems using MA.The as-received, blended, and milled powders were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), and transmission electron microscopy techniques to obtain information about the overall microstructure and chemical compositions. The NiX2 (X = Ge and Si) phases were synthesized in the Ni-Ge and Ni-Si systems. MA of Ni-Ge powder blends was investigated to study phase evolution as a function of milling time. On milling the powders for 5 h, the equilibrium NiGe phase started to form, and its amount in the powder increased with increasing milling time. On milling for about 60 h, the equilibrium intermetallic NiGe and Ge powder particles reacted to form the metastable NiGe2 phase. However, on milling for a longer time (75 h), the metastable phase transformed back to the equilibrium NiGe phase.Synthesis of the NiSi2 intermetallic phase depended on the Si content in the initial powder blend. For example, while in the Ni-60 at.% Si powder blend, only the NiSi phase was present homogeneously, the powder blend of the Ni-67 at.% Si composition contained the NiSi phase along with a small amount of unreacted Si. But in the Ni-75 at.% Si and Ni-80 at% compositions, the NiSi phase that had formed earlier (after 2 h of milling) and the remaining free Si powder reacted to form the equilibrium intermetallic NiSi2 phase. This constitution in the milled powder has been attributed to a partial loss of Si content during MA. Formation of Ni(Si) solid solutions with a solubility of about 18.2 at.% and 20.6 at.% for the Ni-75 at.% Si and Ni-80 at.% Si powder blends, respectively, was also achieved in the early stages of MA.In the Fe-C system, we were able to synthesize ferrite, cementite, and mixtures of the two phases. We were able to obtain the Fe-C solid solution phase (ferrite) with a BCC structure and the cementite phase with an orthorhombic structure in the eutectoid Fe-0.8 wt. % C composition, while a homogeneous cementite phase had formed at the higher carbon content of Fe-7.0 wt. % C after 30 h of milling time.In the case of the Fe-18Cr-xNi (x = 8, 12, and 20) system, the current investigation showed that the phase constitution depended significantly on the Ni content in the powder blend. Whereas mostly the martensite or the ferrite and austenite phase mixture was present at lower Ni contents, a completely homogeneous austenite phase was present in the alloy with 20% Ni.
Show less - Date Issued
- 2016
- Identifier
- CFE0006244, ucf:51059
- Format
- Document (PDF)
- PURL
- http://purl.flvc.org/ucf/fd/CFE0006244
- Title
- STRUCTURAL CHARACTERIZATION OF SPUTTER-DEPOSITED SS304+XAL (X = 0, 4, 7 AND 10 WT.%) COATINGS AND MECHANICALLY MILLED TI, ZR AND HF POWDERS.
- Creator
-
Seelam, Uma Maheswara, Suryanarayana, Challapalli, University of Central Florida
- Abstract / Description
-
Study of the metastable phases obtained by non-equilibrium processing techniques has come a long way during the past five decades. New metastable phases have often given new perspectives to the research on synthesis of novel materials systems. Metastable materials produced by two non-equilibrium processing methods were studied for this dissertation- 304-type austenitic stainless steel (SS304 or Fe-18Cr-8Ni)+aluminum coatings produced by plasma enhanced magnetron sputter-deposition (PEMS) and...
Show moreStudy of the metastable phases obtained by non-equilibrium processing techniques has come a long way during the past five decades. New metastable phases have often given new perspectives to the research on synthesis of novel materials systems. Metastable materials produced by two non-equilibrium processing methods were studied for this dissertation- 304-type austenitic stainless steel (SS304 or Fe-18Cr-8Ni)+aluminum coatings produced by plasma enhanced magnetron sputter-deposition (PEMS) and nanocrystalline Ti, Zr and Hf powders processed by mechanical milling (MM). The objective of the study was to understand the crystallographic and microstructural aspects of these materials. Four SS304+Al coatings with a nominal Al percentages of 0, 4, 7 and 10 wt.% in the coatings were deposited on an SS304 substrate by PEMS using SS304 and Al targets. The as-deposited coatings were characterized by x-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and three-dimensional atom probe microscopy (3DAP). Surface morphology and chemical analysis were studied by SEM. Phase identification was carried out by XRD and TEM. The microstructural features of all the coatings, as observed in the TEM, consisted of columnar grains with the columnar grain width (a measure of grain size) increasing with an increase in the Al content. The coatings had grains with average grain sizes of about 100, 290, 320 and 980 nm, respectively for 0, 4, 7 and 10 wt.% Al. The observed grain structures and increase in grain size were related to substrate temperature during deposition. XRD results indicated that the Al-free coating consisted of the non-equilibrium ferrite and sigma phases. In the 4Al, 7Al and 10Al coatings, equilibrium ferrite and B2 phases were observed but no sigma phase was found. In 10Al coating, we were able to demonstrate experimentally using 3DAP studies that NiAl phase formation is preferred over the FeAl phase at nano scale. During mechanical milling of the hexagonal close packed (HCP) metals Hf, Ti and Zr powders, unknown nanocrystalline phases with face centered cubic (FCC) structure were found. The FCC phases could be either allotropes of the respective metals or impurity stabilized phases. However, upon MM under high purity conditions, it was revealed that the FCC phases were impurity stabilized. The decrease in crystallite size down to nanometer levels, an increase in atomic volume, lattice strain, and possible contamination were the factors responsible for the transformation.
Show less - Date Issued
- 2010
- Identifier
- CFE0003161, ucf:48595
- Format
- Document (PDF)
- PURL
- http://purl.flvc.org/ucf/fd/CFE0003161
