SummaryZinc oxide nanopowders doped with 1–15 mol % cobalt were produced by the microwave solvothermal synthesis (MSS) technique. The obtained nanoparticles were annealed at 800 °C in nitrogen (99.999%) and in synthetic air. The material nanostructure was investigated by means of the following techniques: X-ray diffraction (XRD), helium pycnometry density, specific surface area (SSA), inductively coupled plasma optical emission spectrometry (ICP-OES), extended X-ray absorption fine structure (EXAFS) spectroscopy, scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDS) and with magnetometry using superconducting quantum interference device (SQUID). Irrespective of the Co content, nanoparticles in their initial state present a similar morphology. They are composed of loosely agglomerated spherical particles with wurtzite-type crystal structure with crystallites of a mean size of 30 nm. Annealing to temperatures of up to 800 °C induced the growth of crystallites up to a maximum of 2 μm in diameter. For samples annealed in high purity nitrogen, the precipitation of metallic α-Co was detected for a Co content of 5 mol % or more. For samples annealed in synthetic air, no change of phase structure was detected, except for precipitation of Co3O4 for a Co content of 15 mol %. The results of the magentometry investigation indicated that all as-synthesized samples displayed paramagnetic properties with a contribution of anti-ferromagnetic coupling of Co–Co pairs. After annealing in synthetic air, the samples remained paramagnetic and samples annealed under nitrogen flow showed a magnetic response under the influences of a magnetic field, likely related to the precipitation of metallic Co in nanoparticles.
A series of (Zn,Co)O layers with Co contents x up to 40% grown by atomic layer deposition have been investigated. All structures deposited at 160 • C show magnetic properties specific to II-VI dilute magnetic semiconductors with localized spins S = 3/2 coupled by strong but short-range antiferromagnetic interactions resulting in low-temperature spin-glass freezing for x = 0.16 and 0.4. At higher growth temperature (200 • C) metallic Co nanocrystals precipitate in two locations giving rise to two different magnetic responses: (i) a superparamagnetic contribution coming from volume disperse nanocrystals; (ii) a ferromagneticlike behavior brought about by nanocrystals residing at the (Zn,Co)O/substrate interface. It is shown that the dipolar coupling within the interfacial two-dimensional dense dispersion of nanocrystals is responsible for the ferromagneticlike behavior.
The local order around Mn atoms in the Mn-implanted Si samples, with ferromagnetic properties, has been investigated by use of x-ray-absorption spectroscopy techniques. Analysis of both extended x-ray-absorption fine structure and x-ray absorption near-edge structure spectra clearly indicates that Mn ions are located neither in the substitutional nor in the interstitial position in the Si lattice, but depending on how the samples were prepared, they have five to eight near neighbors.
X-ray Free Electron Lasers (XFELs) have the potential to contribute to many fields of science and to enable many new avenues of research, in large part due to their orders of magnitude higher peak brilliance than existing and future synchrotrons. To best exploit this peak brilliance, these XFEL beams need to be focused to appropriate spot sizes. However, the survivability of X-ray optical components in these intense, femtosecond radiation conditions is not guaranteed. As mirror optics are routinely used at XFEL facilities, a physical understanding of the interaction between intense X-ray pulses and grazing incidence X-ray optics is desirable. We conducted single shot damage threshold fluence measurements on grazing incidence X-ray optics, with coatings of ruthenium and boron carbide, at the SPring-8 Angstrom compact free electron laser facility using 7 and 12 keV photon energies. The damage threshold dose limits were found to be orders of magnitude higher than would naively be expected. The incorporation of energy transport and dissipation via keV level energetic photoelectrons accounts for the observed damage threshold.
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