The strength of polycrystalline materials increases with decreasing grain size. The increase of strength is usually associated with deterioration of ductility, especially for materials having sub-micrometer or nanometer in grain size. It has bee suggested that the ductility of submicro- or nano- grained materials can be improved significantly by introducing a bimodal distribution of grain sizes. The purpose of the present study aims at clarifying the microstructural parameters of the bimodal distribution, such as area ratio and size difference, on the strength and ductility of pure nickel and nickel-cobalt specimens produced by electrodeposition. The microstructural parameters were determined from orientation imaging mapping technique using electron backscatter diffraction. Results indicated that the yield strength is mainly determined by the average size of the fine grains, whereas the tensile strength has a good relation with the average grain size in total. Moreover, it was showed that samples having a area ratio of the fine grains lower than 30% or higher than 70% possess a better ductility. The possible mechanism is discussed in detail.

We deposited CuInSe2 or CuIn1-xGaxSe2 on the substrate of bi-layer Mo by electrodeposition. Besides, we deposited bi-layer Mo by RF sputtering on soda-lime glass. First, we discussed the characteristic of Mo metal, and how can we have a good adhesion and a low resistivity simultaneously. Then, we deposited CuInSe2 and CuIn1-xGaxSe2 thin film by electrodeposition, and discussed the effect of depositing time, pH value in depositing solution, depositing current and different concentration ions respectively.

The strength of the ultrafine-grained materials is increased with grain refinement, but it will also reduce the ductility. In the previous study, there are higher strength and better ductility for the copper with bimodal distribution of grain size. In this study, Ni with lamellar structure is fabricated by electrodeposition in order to explore the mechanical properties of the materials with bimodal distribution of grain size, which is obtained by controlling the grain size. From the result of EBSD analysis, it shows that the area ratio of coarse grains and fine grains is from 0.3 to 3 by changing the plating parameters. The average grain size of fine grains is about 0.5 £gm, and the maximum average grain size of coarse grains is up to 6.0 £gm. From the result of tensile test, the materials with 35% of micro-grains embedded regularly inside a matrix of ultrafine grains have better strength and ductility. When the area ratio of micro-grains is up to 62.5%, there is no difference in mechanical properties between the general electrodeposited materials and ones with bimodal distribution of grain size. For pure Ni, the enhancement of ductility for bimodal distribution of grain size is only in post uniform elongation. Otherwise, it is found that the strength and ductility of the material with lamellar structure are increased through the heat treatmeant under the appropriate temperature.

Three illustrative cases involving the electrodeposition of ultrathin metal films of varying reactivities onto noble-metal substrates were investigated: (i) Pd on Pt(111), a noble admetal on a noble-metal surface; (ii) Bi on Pd(111), a less noble admetal on a noble-metal surface; and (iii) Co on polycrystalline Pd and Pd(111), a reactive metal on a noble-metal surface. The interfacial electrochemistry of these prototypical systems was characterized using a combination of electrochemical methods (voltammetry and coulometry) and ultrahigh vacuum electron spectroscopies (Auger electron spectroscopy, AES; low energy electron diffraction, LEED; and X-ray photoelectron spectroscopy, XPS). Potential-controlled adsorption-desorption cycles of aqueous bromide exerted surface smoothening effects on ultrathin Pd films with defect sites (steps). This procedure, dubbed as electrochemical (EC) annealing, constituted a nonthermal analogue to conventional annealing. EC-annealed ultrathin Pd films exhibited long-range surface order and remained free of oxygen adspecies. Pdadatoms occupying step-sites were selectively dissolved and/or rearranged to assume equilibrium positions in a well-ordered (1x1) film. Electrodeposition of Co was found to be highly surface-structuresensitive. While virtually no Co electrodeposition transpired on a clean Pd(111) surface, Co was voltammetrically deposited on (i) a Pd(111) electrode roughened by oxidation-reduction cycles; and (ii) thermally annealed polycrystalline Pd, which is a composite of the (111) and (100) facets. Electrodeposition of Co was also observed to be kinetically hindered and slow potential scan rates (0.1 mV/s) were required. Well-defined ultrathin Bi films were potentiostatically electrodeposited onto Pd(111); a Stranski-Krastanov growth mode was indicated. The electrochemical reactivity of ultrathin Bi films was characterized using two surface probes: aqueous iodide and D-glucose. (i) Exposure of the prepared Bi adlayers (ΘBi 0.33) to aqueous iodide gave rise to (√3x√7) I-on-Bi superlattice. The same superlattice was obtained if Bi was electrodeposited onto Pd(111)(√3x√3)R30o-I. (ii) With respect to electrooxidation of D-glucose on Pd(111), the presence of Bi adlayers inhibited the by-product-induced "surface poisoning" of Pd(111) but reduced its electrocatalytic efficiency.

Zinc oxide (ZnO) has higher exiton binding energy (60 meV) and high band gap (~3.4 eV) that can provide efficient ultraviolet (UV) light at room temperature (RT). The easily etched in acids and alkalis that provides the fabrication of small-size ZnO-based devices. Electrodeposition is the growth method that can deposit high quality film and modify the characterizations of film by changing its deposition electrolyte concentration, temperature, and current density. Firstly, the ZnO is deposited on n-type Si substrate by electrodeposition by different deposited temperature, electrolyte concentration, and current density. The deposited films contain zinc nitrate, metal Zn, and ZnO while electrodeposited at various deposition parameters. For the deposited film contains only ZnO, no UV light is found measured by macroscopic photoluminescent analysis even annealed at different ambient and temperature. According to previous papers, an ideal UV light intensity can be obtained by thermal treated metal Zn or Zn ion implantation into oxide materials after annealing. Annealing the Zn-ZnO structure formed in 30oC by electrodeposition can observe intense UV light. This method improves the disadvantages of insufficient light intensity and no UV light observation from conventionally electrodeposited ZnO. The variation of UV light wavelength of ZnO oxidized from metal Zn is associated with the quantum-confinement effect that was discussed by previous papers. It is found that the size of ZnO is not small enough to realize the quantum-confinement effect, herein, we suggest that the variation of UV light wavelength is affected by the metal Zn resides in ZnO. Otherwise, the electrodeposition of ZnO is not easily performed on p-type substrate, an aluminum film on the back side of p-type Si can deposit ZnO by smaller potential, and different ZnO nanostructures are obtained by modifying the current density. Recently, different characteristics were found in nano-size noble metal crystals. In this thesis, the porous structure of Au-ZnO and Pt-ZnO were co-deposited by electrodeposition to enhance the photocatalytic activity. Si is the dominant material in semiconductor technology, but its indirect band gap property makes it not allowed in optoelectronics application. However, since 1990, the visible light is observed from porous Si fabricated by electrochemically etching of Si; though the light mechanism of porous Si is not clear, it can be divided into two parts, the quantum-confinement effect of Si nanocrystals and surface states on porous Si. Porous Si emits efficient visible light, but its light wavelength is readily influence by environment. We developed three methods, electrochemically etching the pre-treated Si substrate, adding chemical solution into electrolyte during etching process, and post-treatment of Si substrate after etching to prevent the emission of porous Si from being affected by environment.

In this thesis, manufacturing of microirradiators, electrodeposition of radioactive elements such as Ni-63, and applications of these radioactive sources are discussed. Ni-63 has a half life of 100 years and a low energy beta electron of 67 keV, ideal for low dose low linear energy transfer (LET) research. The main focus of the research is on the novel Ni-63 microirradiator. It contains a small amount of total activity of radiation but a large flux, allowing the user to safely handle the microirradiator without extensive shielding. This thesis is divided into nine chapters. Properties of microirradiators and various competing radioactive sources are compared in the introduction (chapter 1). Detailed description of manufacturing Ni-63 microirradiator using the microelectrode as the starting point is outlined in chapter 2. The microelectrode is a 25 µm in diameter Pt disk sealed in a pulled 1 mm diameter borosilicate capillary tube, as a protruding wire or recessed disk microelectrode. The electrochemically active surface area of each is verified by cyclic voltammetry. Electrodeposition of nickel with a detailed description of formulation of the electrochemical bath in a cold "non-radioactive setting" was optimized by using parameters as defined by pourbaix diagrams, radioactive electroplating of Ni-63, and incorporation of safety regulations into electrodeposition. Calibration and characterization of the Ni-63 microirradiators as protruding wire and recessed disk microirradiators is presented in chapter 3. In chapters 4 through 6, applications of the Ni-63 microirradiators and wire sources are presented. Chapter 4 provides a radiobiological application of the recessed disk microirradiator and a modified flush microirradiator with osteosarcoma cancer cells. Cells were irradiated with 2000 to 1 Bq, and real time observations of DNA double strand breaks were observed. A novel benchtop detection system for the microirradiators is presented in chapter 5. Ni-63 is most commonly measured by liquid scintillation counters, which are expensive and not easily accessible within a benchtop setting. Results show liquid scintillation measurements overestimates the amount of radiation coming from the recessed disk. A novel 10 µCi Ni-63 electrochemically deposited wire acting as an ambient chemical ionization source for pharmaceutical tablets in mass spectrometry is in chapter 6. Typically, larger radioactive sources (15 mCi) of Ni-63 have been used in an ambient ionization scenario. Additionally, this is the first application of using Ni-63 to ionize in atmosphere pharmaceutical tablets, leading to a possible field portable device. In the last chapters, chapters 7 through 8, previous microirradiator experiments and future work are summarized. Chapter 7 illustrates the prototype of the electrochemically deposited microirradiator, the Te-125 microirradiator. In conjunction with Oak Ridge National Laboratory, Te-125m is a low dose x-ray emitting element determined to be the best first prototype of an electrochemically deposited microirradiator. Manufacturing, characterization, and experiments that were not successful leading to the development of the Ni-63 microirradiator are discussed. In chapter 8, future work is entailed in continuing on with this thesis project. The work presented in the thesis is concluded in chapter 9.

Nanostructured materials have potential technological applications due to their characteristic dimensions. The material performance will depend on the atomic structure, and composition of these materials. This thesis focuses on proposing a reliable method for fabricating nanoporous alumina and palladium nanoparticles inside the templates.Palladium nanoparticles were synthesized in commercial porous alumina templates using electrodeposition. Pores within these nanoporous membranes act as templates for the synthesis of nanostructures of the desired material. Electrodeposition is achieved using a three-terminal set-up and a potentiostat. Different types of deposition techniques were investigated to improve the distribution of the deposit. The nanoparticles were characterized by SEM/EDX for composition. The commercial templates have high aspect ratio, but are not hexagonally ordered. Hence porous alumina was fabricated in the laboratory by anodization of aluminum.

Eisen-Gallium-Legierungen sind aufgrund ihrer hohen Magnetostriktion und ihrer hervorragenden mechanischen Eigenschaften sehr interessant für Anwendungen sowohl in Form von Sensoren als auch Aktoren. Die fortschreitende Miniaturisierung erfordert die Herstellung von Bauteilen in eindimensionaler Struktur und komplexen Geometrien. Beide Herausforderungen sind mit templatbasierter elektrochemischer Abscheidung zugänglich. Es konnte gezeigt werden, dass dünne Fe-Ga-Schichten schon aus einfachen wässrigen Elektrolyten abgeschieden werden können. Gallium kann nur in Anwesenheit von Fe induziert reduziert werden. Gleichzeitig konnte nachgewiesen werden, dass durch die Hydrolyseneigung der Ga-Ionen immer Hydroxide gebildet und in das Deposit eingebunden werden. Durch die Einführung einer alternierenden potentiostatischen Abscheidung mit einem Reduktions- und einem Relaxationsschritt können dennoch dichte und homogene Fe80Ga20-Schichten mit wenigen Defekten und einem vernachlässigbar kleinen Sauerstoffgehalt hergestellt werden. Die Übertragung der so gefundenen Abscheideparameter zur templatbasierten Nanodrahtherstellung ist nur bis zu einem Porendurchmesser von 100nm möglich. Wird der Durchmesser der Porenkanäle weiter verringert, führt aufgrund eingeschränkter Diffusionsvorgänge die Abscheidung zu segmentierten und sauerstoffreichen Depositen. Die Modifizierung des Elektrolyten durch Komplexierung der Metallionen verhindert die Bildung und Einbindung der Hydroxide. Damit können auch für Porendurchmesser kleiner 100nm Drähte in AAO-Template abgeschieden werden. Diese sind dicht, defektfrei und weisen keinen Zusammensetzungsgradienten entlang der Wachstumsrichtung auf. Detaillierte TEM-Untersuchungen konnten zeigen, dass die Herstellung durch ein einfacheres potentiostatisches Abscheideregime zu weniger verspannten und dennoch homogenen und defektfreien Drähten führt. Für die Herstellung von magnetisch aktiven Drähten sollte daher die potentiostatische der gepulsten Abscheidung vorgezogen werden.

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