Herein, a novel method for the in situ growth of single gold nanoparticles (AuNPs) in microgel (MG) networks is presented. The key feature in this approach is the localization of β‐diketone groups capable of both complexation and reduction of aurate ions in the MGs’ core, which allows localization of the nucleation and growth of single AuNPs. The MG synthesis is carried out via precipitation polymerization in water with N‐vinylcaprolactam as the main monomer and with the two comonomers acetoacetoxyethyl methacrylate (AAEM) and acrylic acid (AAc), where AAEM is mainly located in the MGs’ core and AAc in their shell. For the synthesis of AuNPs, a certain amount of chloroauric acid (HAuCl4) is added to the dispersion, followed by fast reduction with sodium borohydride (NaBH4). In situ synthesized AuNPs in MGs possess a spherical shape, with a diameter of 8.1 ± 0.8 nm, being localized in the center of every MG. In addition, these AuNPs embedded into MG networks can be used as seeds that grow in their size after the addition of HAuCl4 up to 46.0 ± 9.5 nm under mild reaction conditions (room temperature, aqueous dispersion) and without the use of any additional reducing and stabilizing agents.
The compound IrGa3 was synthesized by direct reaction
of the elements. It is formed as a high-temperature phase in the Ir-Ga
system. Single-crystal X-ray diffraction analysis confirms the tetragonal
symmetry (space group P42
/mnm, No. 136) with a = 6.4623(1) Å and c = 6.5688(2) Å and reveals strong disorder in the
crystal structure, reflected in the huge values and anisotropy of
the atomic displacement parameters. A model for the real crystal structure
of ht-IrGa3 is derived by the split-position
approach from the single-crystal X-ray diffraction data and confirmed
by an atomic-resolution transmission electron microscopy study. Temperature-dependent
electrical resistivity measurements evidence semiconductor behavior
with a band gap of 30 meV. A thermoelectric characterization was performed
for ht-IrGa3 and for the solid solution
IrGa3–x
Zn
x
.
The kinetics of formation of silver nanoparticles consisting of nearly 300 metal atoms is investigated, which were prepared by reduction of silver nitrate with hydrazine in ethylene glycol at 25 • C without any stabilizer other than the glycol solvent. The resulting sigmoidal kinetic curves are analyzed by using the 1997 Finke-Watzky two-step mechanism of slow continuous nucleation with subsequent fast autocatalytic surface growth. The kinetics of homogeneous nucleation of metal nanoparticles was analyzed using the assumption about the stepwise adjunction of precursor and the quasi steadystate approximation. The equations were proposed to calculate the concentration of the formed metal nanoparticles and their mean size from the experimentally determined values of the Finke-Watzky rate constants. It is shown that a stepwise nucleation process can be described in the terms of the catalytically effective nucleus concept and that the number of atoms in the catalytically effective nucleus can be estimated.
K E Y W O R D Scatalytically effective nucleus concept, homogeneous nucleation, kinetics, silver nanoparticles 266
The influence of Al incorporation on the heavy fermion superconductor UBe13 was investigated to explain the sample dependence of physical properties. Clear evidence for incorporated Al in flux-grown UBe13 single crystals is presented by results from X-ray diffraction, nuclear magnetic resonance and X-ray spectroscopy. The increase of the lattice parameter and the concomitant change of the superconducting properties are caused by substitution of Be in the compound by 1–2 at.% Al. The minute amounts of Al in the structure were located by atomic resolution transmission electron microscopy. Specific heat measurements reveal the strong influence of incorporated Al on the physical properties of UBe13. Upon long-term annealing, Al incorporated in single crystals can leave the structure, restoring properties of Al-free polycrystalline UBe13.
Lead chalcogenides are known for their thermoelectric properties since the first work of Thomas Seebeck on the discovery of this phenomenon. Yet, the electronic properties of lead telluride are still of interest due to the incomplete understanding of the metal-to-semiconductor transition at temperatures around 230 °C. Here, a temperature-dependent atomic-resolution transmission electron microscopy study performed on a single crystal of lead telluride reveals structural reasons for this electronic transition. Below the transition temperature, the formation of a dislocation network due to shifts of the NaCl-like atomic slabs perpendicular to {100} was observed. The local structure modification leads to the appearance of in-gap electronic states and causes metal-like electronic transport behavior. The dislocation network disappears with increasing temperature, yielding semiconductor-like electrical conductivity, and re-appears after cooling to room temperature restoring the metal-like behavior. The structural defects coupled to the ordering of stereochemically active lone pairs of lead atoms are discussed in the context of dislocations' formation.
Nano-scaled thermoelectric materials attract significant interest due to their improved physical properties as compared to bulk materials. Well-shaped nanoparticles such as nano-bars and nano-cubes were observed in the known thermoelectric material PbTe. Their extended two-dimensional nano-layer arrangements form directly in situ through electron-beam treatment in the transmission electron microscope. The experiments show the atomistic depletion mechanism of the initial crystal and the recrystallization of PbTe nanoparticles out of the microparticles due to the local atomic-scale transport via the gas phase beyond a threshold current density of the beam.
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