Microstructure evolution of 6061 O Al alloy during ultrasonic consolidation:An insight from electron backscatter diffraction

6061 O Al alloy foils were welded to form monolithic and SiC fibre-embedded samples using the ultrasonic consolidation (UC) process. Contact pressures of 135, 155 and 175 MPa were investigated at 20 kHz frequency, 50% of the oscillation amplitude, 34.5 mm s sonotrode velocity and 20 °C. Deformed microstructures were analysed using electron backscatter diffraction (EBSD). At all contact pressures deformation occurs by non-steady state dislocation glide. Dynamic recovery is active in the upper and lower foils. Friction at the welding interface, instantaneous internal temperatures (0.5-0.8 of the melting temperature, T), contact pressure and fast strain rates result in transient microstructures and grain size reduction by continuous dynamic recrystallization (CDRX) within the bonding zone. Bonding occurs by local grain boundary migration, which allows diffusion and atom interlocking across the contact between two clean surfaces. Textures weaken with increasing contact pressure due to increased strain hardening and different grain rotation rates. High contact pressures enhance dynamic recovery and CDRX. Deformation around the fibre is intense within 50 μm and extends to 450 μm from it. © 2009 Acta Materialia Inc.

Microstructure and microtexture evolution of aluminum alloy 3003 under ultrasonic welding process for embedding SiC fibre

Ultrasonic welding process can be used for bonding metal foils which is the fundament of ultrasonic consolidation (UC). UC process can be used to embed reinforcement fibres such as SiC fibres within an aluminum matrix materials. In this research we are investigating the phenomena occurring in the microstructure of the parts during ultrasonic welding process to obtain better understanding about how and why the process works. High-resolution electron backscatter diffraction (EBSD) is used to study the effects of the vibration on the evolution of microstructure in AA3003. The inverse pole figures (IPF) and the correlated misorientation angle distribution of the mentioned samples are obtained. The characteristics of the crystallographic orientation, the grain structure and the grain boundary are analyzed to find the effect of ultrasonic vibration on the microstructure and microtexture of the bond. The ultrasonic vibration will lead to exceptional refinement of grains to a micron level along the bond area and affect the crystallographic orientation. Ultrasonic vibration results in a very weak texture. Plastic flow occurs in the grain after welding process and there is additional plastic flow around the fibre which leads to the fibre embedding. © 2009 Editorial Board of CHINA WELDING.

Microstrcutural evolution of SiC fibre embedded AA6061 matrix induced by ultrasonic consolidation

Ultrasonic consolidation (UC) uses high frequency (20-40KHz) mechanical vibrations to produce a solid-state metallurgical bond (weld) between metal foils. UC as a novel layered manufacturing technique is used in this research to embed reinforcing members such as silicon carbide fibers into the aluminium alloy 6061's matrices. It is known that UC induce volume and surface effect in the material it is acting on. Both effects are employed in embedding active/passive elements in the metal matrix. Whilst the process and the two effects are used and identified at macro level, what is happening at micro level is unknown and hardly studied. In this research we are investigating the phenomena occurring in the microstructure of the parts during UC process to obtain better understanding about how and why the process works. In this research, high-resolution electron backscatter diffraction is used to study the effects of the UC process on the evolution of microstructure in AA6061 with and without fibre elements. The inverse pole figures (IPF), pole figures (PF) and the correlated misorientation angle distribution of the mentioned samples are obtained. The characteristics of the crystallographic orientation, the grain structure and the grain boundary are analysed to find the effect of ultrasonic vibration and embedding fibre on the microstructure and texture of the bond. The ultrasonic vibration will lead to exceptional refinement of grains to a micron level along the bond area and affect the crystallographic orientation. Additional plastic flow occurs around the fibre which leads to the fibre embedding. © 2008 Materials Research Society.

DOMINANCE OF SHORT-RANGE-ORDER EFFECTS IN LOW-ENERGY ELECTRON-DIFFRACTION INTENSITY SPECTRA

Using low-energy electron-diffraction (LEED) formalism, we demonstrate theoretically that LEED I-V spectra are characterized mainly by short-range order. We also show experimentally that diffuse LEED (DLEED) I-V spectra can be accurately measured from a disordered system using a video-LEED system even at very low coverage. These spectra demonstrate that experimental DLEED I-V spectra from disordered systems may be used to determine local structures. As an example, it is shown that experimental DLEED I-V spectra from K/Co {1010BAR} at potassium coverages of 0.07, 0.1, and 0.13 monolayer closely resemble calculated and experimental LEED I-V spectra for a well-ordered Co{1010BAR}-c(2X2)-K superstructure, leading to the conclusion that at low coverages, potassium atoms are located in the fourfold-hollow sites and that there is no large bond-length change with coverage.

A STUDY ON THE HOLOGRAPHIC TRANSFORM FOR ELECTRON-DIFFRACTION FROM SURFACES

We break down photoelectron diffraction intensities into four terms in analogy to optical holography and discuss the effect of each term on reconstructed images. The second term involving products of scattered waves SIGMA-SIGMA-O(i)O(j)*, is in this case not structure-less. Theoretical analysis and simulations demonstrate that this term may lead to spurious features in real space images in holographic transforms of medium energy electron diffraction patterns. If it is small enough the problem may be overcome by an iterative correction process.

Scanning electron microscopy study of microstructural evolution of electroless nickel-phosphorus deposits with heat treatment

This paper follows previous X-ray diffraction work on crystallisation and phase transformation of electroless nickel–phosphorus deposits, concentrating on microstructural changes. Amorphous or nanocrystalline coatings, depending on their phosphorus content, were heat treated at temperatures between 100 and 500 °C for 1 h. Changes in microstructure after the heat treatment were examined using high-resolution field emission scanning electron microscope. Crystallisation and grain growth effects are observed, as well as some inherent defect structures in the coatings and their changes. These are compared with the previous X-ray diffraction work and in general, good agreement is observed. The complementary strength and weakness of the different characterisation techniques are discussed.

Alkynyl-Bridged Ruthenium(II) 4 '-Diferroceny1-2,2 ':6 ',2 ''-terpyridine Electron Transfer Complexes: Synthesis, Structures, and Electrochemical and Spectroscopic Studiese

The novel ligand 4'-diferrocenylallcyne-2,2':6',2 ''-terpyridine (7; Fc-C C-Fc-tpy; tpy = terpyridyl; Fc = ferrocenyl) and its Ru2+ complexes 8-10 have been synthesized and characterized by single-crystal X-ray diffraction, cyclic voltammetry, and UV-vis and luminescence spectroscopy. Electrochemical data and UV absorption and emission spectra indicate that the insertion of an ethynyl group causes delocalization of electrons in the extended pi* orbitals. Cyclic voltammetric measurements of 7 show two successive reversible one-electron-oxidation processes with half-wave potentials of 0.53 and 0.78 V. The small variations of the E-1/2 values for the Fe2+/Fe3+ redox couples after the coordination of the Ru2+ ion suggest a weak interaction between the Ru2+ and Fe2+ centers. After insertion of an ethynyl group, UV-vis absorption spectra show a red shift of the absorption peak of the (1)[(d(pi)(Fe))(6)]->(1)[(d(pi)(Fe))(5)(pi*(Ru)(tpy))(1)] MMLCT of the Ru2+ complexes. The Ru2+ complex 8 exhibits the strongest luminescence intensity (lambda(em)(max) 712 nm, Phi(em) = 2.63 x 10(-4), tau = 323 ns) relative to analogous ferrocene-based terpyridine Ru(II) complexes in H2O/CH3CN (4/1 v/v) solution.

Ruthenium(II) bis(terpyridine) electron transfer complexes with alkynyl-ferrocenyl bridges: synthesis, structures, and electrochemical and spectroscopic studies

Two novel alkynyl-bridged symmetric bis-tridentate ligands 1,2-bis(1'-[4'-(2,2':6', 2 ''-terpyridinyl)]-ferrocenyl)ethyne (3a; tpy-Fc-C C-Fc-tpy; Fc = ferrocenyl; tpy = terpyridyl) and 1,4-bis(1'-[4'-(2,2':6', 2 ''-terpyridinyl)]ferrocenyl)-1,3-butadiyne (3b; tpy-Fc-C C-C C-Fc-tpy) and their Ru2+ complexes 6a and 6b have been synthesized and characterized by cyclic voltammetry, UV-vis and luminescence spectroscopy, and in the case of 3b by single-crystal X-ray diffraction. Cyclic voltammograms of both compounds, 3a and 3b, display two severely overlapping ferrocene-based oxidative peaks with only one reductive peak. The redox behavior of 6a and 6b is dominated by the Ru2+/Ru3+ redox couple (E-1/2 from 1.33 to 1.34 V), the Fe2+/Fe3+ redox couples (E-1/2 from 0.46 to 0.80 V), and the tpy/tpy(-)/tpy(2-)redox couples (E-1/2 from -1.19 to -1.48 V). The UV-vis spectra of 6a and 6b show absorption bands assigned to the (1)[(d(pi)(Fe))(6)] -> (1)[(d(pi)(Fe))(5)(pi*(Ru)(tpy))(1)] MMLCT transition at similar to 555 nm. Complexes 6a and 6b are luminescent in H2O-CH3CN (4 : 1, v/v) solution at room temperature, and 6b exhibits the strongest luminescence intensity (lambda(em)(max): 710 nm, Phi(em): 2.28 x 10(-4), tau: 358 ns) relative to analogous ferrocene-based bis(terpyridine) Ru(II) complexes reported so far.

Orientation effects in copper phthalocyanine films studied by electron paramagnetic resonance spectroscopy

The metallo-phthalocyanines (MPcs) are an interesting group of organic semiconductor materials for applications such as large area solar cells due to their optoelectronic properties coupled with the possibility of easily and cheaply fabricating thin films of MPcs [1, 2]. As for organic semiconductors in general, many of the interesting properties of the MPcs such as magnetism, light absorption and charge transport, are highly anisotropic [2, 3]. To maximise the efficiency of a device based on these materials it is therefore important to study their molecular orientation in films and to assess the influence of different growth conditions and substrate treatments.
X-ray diffraction is a well established and powerful technique for studying texture (and hence molecular orientation) in crystalline materials, but it cannot provide any information about amorphous or nanocrystalline films. In electron paramagnetic resonance (EPR) spectroscopy the signal comes from the spin of unpaired electrons in the material. This technique therefore does not require the sample to be crystalline. It works for any sample with paramagnetic centres such as the MPcs where the unpaired electrons are contributed by the metal. In this paper we present a continuous-wave X-band EPR study using the anisotropy of the EPR spectrum of CuPc [4] to determine the orientation effects in different types of CuPc films. From these measurements we gain insight into the molecular arrangement of films with different spin concentrations, and apply our technique to the study of molecular orientation in photovoltaic cells.

High-resolution electron energy-loss spectroscopy of Ba Ti O 3∕ Sr Ti O 3 multilayers

The dielectric properties of BaTiO3 thin films and multilayers are different from bulk materials because of nanoscale dimensions, interfaces, and stress-strain conditions. In this study, BaTiO3/SrTiO3 multilayers deposited on SrTiO3 substrates by pulsed laser deposition have been investigated by high-energy-resolution electron energy-loss spectroscopy. The fine structures in the spectra are discussed in terms of crystal-field splitting and the internal strain. The crystal-field splitting of the BaTiO3 thin layer is found to be a little larger than that of bulk BaTiO3, which has been interpreted by the presence of the internal strain induced by the misfit at the interface. This finding is consistent with the lattice parameters of the BaTiO3 thin layer determined by the selected area diffraction pattern. The near-edge structure of the oxygen K edge in BaTiO3 thin layers and in bulk BaTiO3 are simulated by first-principle self-consistent full multiple-scattering calculations. The results of the simulations are in a good agreement with the experimental results. Moreover, the aggregation of oxygen vacancies at the rough BaTiO3/SrTiO3 interface is indicated by the increased [Ti]/[O] element ratio, which dominates the difference of dielectric properties between BaTiO3 layer and bulk materials.