Formation of aggregated nanoparticle spheres through femtosecond laser surface processing

A detailed structural and chemical analysis of a class of self-organized surface structures, termed aggregated nanoparticle spheres (AN-spheres), created using femtosecond laser surface processing (FLSP) on silicon, silicon carbide, and aluminum is reported in this paper. AN-spheres are spherical microstructures that are 20–100 μm in diameter and are composed entirely of nanoparticles produced during femtosecond laser ablation of material. AN-spheres have an onion-like layered morphology resulting from the build-up of nanoparticle layers over multiple passes of the laser beam. The material properties and chemical composition of the AN-spheres are presented in this paper based on scanning electron microscopy (SEM), focused ion beam (FIB) milling, transmission electron microscopy (TEM), and energy dispersive x-ray spectroscopy (EDX) analysis. There is a distinct difference in the density of nanoparticles between concentric rings of the onion-like morphology of the AN-sphere. Layers of high-density form when the laser sinters nanoparticles together and low-density layers form when nanoparticles redeposit while the laser ablates areas surrounding the AN-sphere. The dynamic nature of femtosecond laser ablation creates a variety of nanoparticles that make-up the AN-spheres including Si/C core-shell, nanoparticles that directly fragmented from the base material, nanoparticles with carbon shells that retarded oxidation, and amorphous, fully oxidized nanoparticles

Micro/nanostructures formation by femtosecond laser surface processing on amorphous and polycrystalline Ni60Nb40

Femtosecond laser surface processing is a technology that can be used to functionalize many surfaces, imparting specialized properties such as increased broadband optical absorption or superhydrophilicity/superhydrophobicity. In this study, two unique classes of surface structures, below surface growth (BSG) and above surface growth (ASG) mounds, were formed by femtosecond laser surface processing on amorphous and polycrystalline Ni60Nb40 with two different grain sizes. Cross sectional imaging of these mounds revealed thermal evidence of the unique formation processes for each class of surface structure. BSG mounds formed on all three substrates using the same laser parameters had similar surface morphology. The microstructures in the mounds were unaltered compared with the substrate before laser processing, suggesting their formation was dominated by preferential valley ablation. ASG mounds had similar morphology when formed on the polycrystalline Ni60Nb40 substrates with 100 nm and 2 [H9262]m grain size. However, the ASG mounds had significantly wider diameter and higher peak-to-valley heights when the substrate was amorphous Ni60Nb40. Hydrodynamic melting was primarily responsible for ASG mound formation. On amorphous Ni60Nb40 substrates, the ASG mounds are most likely larger due to lower thermal diffusivity. There was clear difference in growth mechanism of femtosecond laser processed BSG and ASG mounds, and grain size does not appear to be a factor

Microstructure and Phase Analysis in Mn-Al and Zr-Co Permanent Magnets

In America’s search for energy independence, the development of rare-earth free permanent magnets is one hurdle that still stands in the way. Permanent magnet motors provide a higher efficiency than induction motors in applications such as hybrid vehicles and wind turbines. This thesis investigates the ability of two materials, Mn-Al and Zr-Co, to fill this need for a permanent magnet material whose components are readily available within the U.S. and whose supply chain is more stable than that of the rare-earth materials. This thesis focuses on the creation and optimization of these two materials to later be used as the hard phase in nanocomposites with high energy products (greater than 10 MGOe). Mn-Al is capable of forming the pure L10 structure at a composition of Mn54Al43C3. When Mn is replaced by Fe or Cu using the formula Mn48Al43C3T6 the anisotropy constant is lowered from 1.3∙107 ergs/cm3 to 1.0∙107 ergs/cm3 and 0.8∙107 ergs/cm3 respectively. Previous studies have reported a loss in magnetization in Mn-Al alloys during mechanical milling. The reason for this loss in magnetization was investigated and found to be due to the formation of the equilibrium β-Mn phase of the composition Mn3Al2 and not due to oxidation or site disorder. It was also shown that fully dense Mn-Al permanent magnets can be created at hot pressing temperatures at or above 700oC and that the ε-phase to τ-phase transition and consolidation can be combined into a single processing step. The addition of small amounts of Cu to the alloy, 3% atomic, can increase the compaction density allowing high densities to be achieved at lower pressing temperatures. While the structure is still under debate, alloys at the composition Zr2Co11 in the Zr-Co system have been shown to have hard magnetic properties. This thesis shows that multiple structures exist at this Zr2Co11 composition and that altering the cooling rate during solidification of the alloy affects the ratio of the phase composition and therefore affects the magnetic properties. Phase diagrams for the Zr-Co system show that the Zr2Co11 phase is stable to a temperature of 1272oC, at which point the Zr6Co23 phase is the most favorable. However, this thesis shows that the Zr6Co23 phase forms at room temperature during high energy mechanical milling and at annealing temperatures as low as 600oC. Since high energy mechanical milling was not a potential method to creating single crystalline particles, hydrogen embrittlement was investigated. Hydrochloric acid was used to induce hydrogen embrittlement in the Zr2Co11 alloy, modifying the fracture characteristics of the alloy causing it to occur primarily along grain boundaries resulting in single crystalline particles with remanent magnetization enhancement. Adviser: Jeffrey E. Shiel

Formation of aggregated nanoparticle spheres through femtosecond laser surface processing

A detailed structural and chemical analysis of a class of self-organized surface structures, termed aggregated nanoparticle spheres (AN-spheres), created using femtosecond laser surface processing (FLSP) on silicon, silicon carbide, and aluminum is reported in this paper. AN-spheres are spherical microstructures that are 20–100 μm in diameter and are composed entirely of nanoparticles produced during femtosecond laser ablation of material. AN-spheres have an onion-like layered morphology resulting from the build-up of nanoparticle layers over multiple passes of the laser beam. The material properties and chemical composition of the AN-spheres are presented in this paper based on scanning electron microscopy (SEM), focused ion beam (FIB) milling, transmission electron microscopy (TEM), and energy dispersive x-ray spectroscopy (EDX) analysis. There is a distinct difference in the density of nanoparticles between concentric rings of the onion-like morphology of the AN-sphere. Layers of high-density form when the laser sinters nanoparticles together and low-density layers form when nanoparticles redeposit while the laser ablates areas surrounding the AN-sphere. The dynamic nature of femtosecond laser ablation creates a variety of nanoparticles that make-up the AN-spheres including Si/C core-shell, nanoparticles that directly fragmented from the base material, nanoparticles with carbon shells that retarded oxidation, and amorphous, fully oxidized nanoparticles

Phase Transitions in Mechanically Milled Mn-Al-C Permanent Magnets

Mn-Al powders were prepared by rapid solidification followed by high-energy mechanical milling. The rapid solidification resulted in single-phase ε. The milling was performed in both the ε phase and the τ phase, with the τ-phase formation accomplished through a heat treatment at 500 °C for 10 min. For the ε-milled samples, the conversion of the ε to the τ phase was accomplished after milling via the same heat treatment. Mechanical milling induced a significant increase in coercivity in both cases, reaching 4.5 kOe and 4.1 kOe, respectively, followed by a decrease upon further milling. The increase in coercivity was the result of grain refinement induced by the high-energy mechanical milling. Additionally, in both cases a loss in magnetization was observed. Milling in the ε phase showed a smaller decrease in the magnetization due to a higher content of the τ phase. The loss in magnetization was attributed to a stress-induced transition to the equilibrium phases, as no site disorder or oxidation was observed. Surfactant-assisted milling in oleic acid also improved coercivity, but in this case values reached >4 kOe and remained stable at least through 32 h of milling

Experimental explanation of the formation mechanism of surface mound-structures by femtosecond laser on polycrystalline Ni\u3csub\u3e60\u3c/sub\u3eNb\u3csub\u3e40\u3c/sub\u3e

Femtosecond laser surface processing (FLSP) is an emerging technique for creating functionalized surfaces with specialized properties, such as broadband optical absorption or superhydrophobicity/ superhydrophilicity. It has been demonstrated in the past that FLSP can be used to form two distinct classes of mound-like, self-organized micro/nanostructures on the surfaces of various metals. Here, the formation mechanisms of below surface growth (BSG) and above surface growth (ASG) mounds on polycrystalline Ni60Nb40 are studied. Cross-sectional imaging of these mounds by focused ion beam milling and subsequent scanning electron microscopy revealed evidence of the unique formation processes for each class of microstructure. BSG-mound formation during FLSP did not alter the microstructure of the base material, indicating preferential valley ablation as the primary formation mechanism. For ASG-mounds, the microstructure at the peaks of the mounds was clearly different from the base material. Transmission electron microscopy revealed that hydrodynamic melting of the surface occurred during FLSP under ASG-mound forming conditions. Thus, there is a clear difference in the formation mechanisms of ASG- and BSG-mounds during FLSP

Micro/nanostructures formation by femtosecond laser surface processing on amorphous and polycrystalline Ni60Nb40

Femtosecond laser surface processing is a technology that can be used to functionalize many surfaces, imparting specialized properties such as increased broadband optical absorption or superhydrophilicity/superhydrophobicity. In this study, two unique classes of surface structures, below surface growth (BSG) and above surface growth (ASG) mounds, were formed by femtosecond laser surface processing on amorphous and polycrystalline Ni60Nb40 with two different grain sizes. Cross sectional imaging of these mounds revealed thermal evidence of the unique formation processes for each class of surface structure. BSG mounds formed on all three substrates using the same laser parameters had similar surface morphology. The microstructures in the mounds were unaltered compared with the substrate before laser processing, suggesting their formation was dominated by preferential valley ablation. ASG mounds had similar morphology when formed on the polycrystalline Ni60Nb40 substrates with 100 nm and 2 [H9262]m grain size. However, the ASG mounds had significantly wider diameter and higher peak-to-valley heights when the substrate was amorphous Ni60Nb40. Hydrodynamic melting was primarily responsible for ASG mound formation. On amorphous Ni60Nb40 substrates, the ASG mounds are most likely larger due to lower thermal diffusivity. There was clear difference in growth mechanism of femtosecond laser processed BSG and ASG mounds, and grain size does not appear to be a factor