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.
The iron crosslinked chitosan (Ch-Fe-CL) and N-carboxylmethyl chitosan (N-CM-Ch-Fe) complexes were studied by complementary techniques: structurally sensitive Mössbauer and X-ray absorption methods, as well as static magnetic measurements. A detailed and consistent description of these complexes including, besides the overall magnetic behavior, the spin ordering and local atomic structure around Fe ions is presented. Fe atoms in the investigated samples are mostly penta-coordinated and appear in a high spin Fe (3+) ionic state. In Ch-Fe-CL, two kinds of Fe near neighbors are equally probable and several Fe atoms are situated in the second coordination sphere. The magnetic interactions between these Fe ions lead to a sperimagnetic-like ordering. In N-CM-Ch-Fe, only one Fe neighborhood was found. Other Fe atoms were identified neither in the first nor in the second coordination sphere, but the third coordination sphere indicates the presence of Fe atoms. The magnetic coupling between these atoms is antiferromagnetic, but the dominant part of Fe in this sample remains in a paramagnetic state.
Changes of the local structure around Mn atoms in (Ga, Mn)As layers after high temperature annealing were determined by x-ray absorption spectroscopy (EXAFS) and high-resolution x-ray diffraction (HRXRD) measurements, and related to their magnetic properties. X-ray absorption is known to be able to detect crystalline structure changes occurring around investigated atoms. The qualitative and quantitative analysis of EXAFS spectra gives unambiguous evidence for the transition from a cubic to a hexagonal phase around Mn atoms as a result of annealing at temperatures of 500 and 600• C. The performed HRXRD investigation indicated a relaxation of the GaAs matrix during annealing, from highly to slightly compressively strained, and finally, after the formation of inclusions of hexagonal MnAs, to slightly tensile strained. The sample with hexagonal MnAs inclusions exhibits ferromagnetic properties up to room temperature with almost all Mn atoms being in a ferromagnetic phase.
In this work we adapt rare-earth-ion-doped NaYF4 nanoparticles coated with a silicon oxide shell (NaYF4:20%Yb,0.2%Tm@SiO2) for biological and medical applications (for example, imaging of cancer cells and therapy at the nano level). The wide upconversion emission range under 980 nm excitation allows one to use the nanoparticles for cancer cell (4T1) photodynamic therapy (PDT) without a photosensitizer. The reactive oxygen species (ROS) are generated by Tm/Yb ion upconversion emission (blue and UV light). The in vitro PDT was tested on 4T1 cells incubated with NaYF4:20%Yb,0.2%Tm@SiO2 nanoparticles and irradiated with NIR light. After 24 h, cell viability decreased to below 10%, demonstrating very good treatment efficiency. High modification susceptibility of the SiO2 shell allows for attachment of biological molecules (specific antibodies). In this work we attached the anti-human IgG antibody to silane-PEG-NHS-modified NaYF4:20%Yb,0.2%Tm@SiO2 nanoparticles and a specifically marked membrane model by bio-conjugation. Thus, it was possible to perform a selective search (a high-quality optical method with a very low-level organic background) and eventually damage the targeted cancer cells. The study focuses on therapeutic properties of NaYF4:20%Yb,0.2%Tm@SiO2 nanoparticles and demonstrates, upon biological functionalization, their potential for targeted therapy.
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