The aims of the current study were to synthesize new responsive polymeric microgels with embedded silver nanoparticles and then to employ these particles as catalyst for reduction reactions. To these ends, stimuli‐responsive microgels from PNIPAAm and the chitosan derivative were firstly synthesized by free radical precipitation polymerization. Then, silver nanoparticles were synthesized inside these microgel networks by in situ reduction of AgNO3. These microgels were temperature/pH sensitive with a phase transition temperature of 32–35 °C in water at pH = 3 and 8, respectively. The catalytic activity of the Ag nanoparticles for the reduction of 4‐nitrophenol can be tuned through the swelling or collapse of the responsive microgel network hosting the active nanoparticles.
The CO 2 laser vaporization (LAVA) method was used to prepare titania nanopowders. Because this versatile method does not require special precursors, a coarse anatase raw powder was applied as starting material. Powder samples produced under varied process parameters were characterized by transmission electron microscopy (TEM), X-ray diffraction measurements, and Brunauer-Emmett-Teller surface area measurements. The laser-generated powders consist of spherical, single crystalline and pure anatase nanoparticles, merely softly agglomerated by weak van der Waals forces. Using TEM analysis, the influence of the process parameters on the resulting particle size distribution was investigated. The results are discussed with respect to the particle formation by gas phase condensation. The potential of a process integrated, i.e. in situ, coating procedure for the surface modification of the anatase nanoparticles is demonstrated. As an exemplary representative of organic layer materials stearic acid was chosen. The organic coating was characterized by TEM and Raman spectrometry. Because of the unavoidable soft agglomeration the coating covers entire agglomerates rather than individual primary particles. Thus, the influence of the LAVA process parameters on the agglomerate sizes was systematically studied using a scanning mobility particle sizer.
Crystalline magnetic iron oxide nanopowders are prepared by CO 2 laser vaporization (LAVA) of a hematite (α-Fe 2 O 3 ) raw powder. Condensation at normal pressure leads to maghemite (γ-Fe 2 O 3 ) as the main phase in the nanopowders. With an increasing oxygen partial pressure in the zone of condensation, an increasing amount of Fe 2 O 3 polymorph ε-Fe 2 O 3 is found. The LAVA-prepared Fe 2 O 3 nanopowders are characterized by X-ray diffraction, transmission electron microscopy, and chemical analysis and with respect to their magnetic properties. A mechanism for the initial nucleation is proposed to explain the formation of ε-Fe 2 O 3 with an increasing oxygen content in the condensation atmosphere. The model is based on the evidence of ozone in oxygen-rich condensation atmospheres. Density functional theory calculations indicate that ozone facilitates the formation of 6-fold oxygen-coordinated Fe ions acting as building units for the emerging crystal structure during the solidification of the nanoparticles. This insight into early nucleation stages will be useful for the functional design and crystal engineering of either isostructural materials like alumina (Al 2 O 3 ) or, more generally, vapor phase synthetic routes for ceramic materials.
Spherical, softly agglomerated and superparamagnetic nanoparticles (NPs) consisting of maghemite (γ-Fe2O3) and amorphous silica (SiO2) were prepared by CO2 laser co-vaporization (CoLAVA) of hematite powder (α-Fe2O3) and quartz sand (SiO2). The α-Fe2O3 portion of the homogeneous starting mixtures was gradually increased (15 mass%-95 mass%). It was found that (i) with increasing iron oxide content the NPs' morphology changes from a nanoscale SiO2 matrix with multiple γ-Fe2O3 inclusions to Janus NPs consisting of a γ-Fe2O3 and a SiO2 hemisphere to γ-Fe2O3 NPs each carrying one small SiO2 lens on its surface, (ii) the multiple γ-Fe2O3 inclusions accumulate at the NPs' inner surfaces, and (iii) all composite NPs are covered by a thin layer of amorphous SiO2. These morphological characteristics are attributed to (i) the phase segregation of iron oxide and silica within the condensed Fe2O3-SiO2 droplets, (ii) the temperature gradient within these droplets which arises during rapid cooling in the CoLAVA process, and (iii) the significantly lower surface energy of silica when compared to iron oxide. The proposed growth mechanism of these Fe2O3-SiO2 composite NPs during gas phase condensation can be transferred to other systems comprising a glass-network former and another component that is insoluble in the regarding glass. Thus, our model will facilitate the development of novel functional composite NPs for applications in biomedicine, optics, electronics, or catalysis.
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