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1.  Nanostructured, mesoporous Au/TiO2 model catalysts – structure, stability and catalytic properties 
Aiming at model systems with close-to-realistic transport properties, we have prepared and studied planar Au/TiO2 thin-film model catalysts consisting of a thin mesoporous TiO2 film of 200–400 nm thickness with Au nanoparticles, with a mean particle size of ~2 nm diameter, homogeneously distributed therein. The systems were prepared by spin-coating of a mesoporous TiO2 film from solutions of ethanolic titanium tetraisopropoxide and Pluronic P123 on planar Si(100) substrates, calcination at 350 °C and subsequent Au loading by a deposition–precipitation procedure, followed by a final calcination step for catalyst activation. The structural and chemical properties of these model systems were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), N2 adsorption, inductively coupled plasma ionization spectroscopy (ICP–OES) and X-ray photoelectron spectroscopy (XPS). The catalytic properties were evaluated through the oxidation of CO as a test reaction, and reactivities were measured directly above the film with a scanning mass spectrometer. We can demonstrate that the thin-film model catalysts closely resemble dispersed Au/TiO2 supported catalysts in their characteristic structural and catalytic properties, and hence can be considered as suitable for catalytic model studies. The linear increase of the catalytic activity with film thickness indicates that transport limitations inside the Au/TiO2 film catalyst are negligible, i.e., below the detection limit.
PMCID: PMC3190629  PMID: 22003465
Au catalysis; Au/TiO2; CO oxidation; gold nanoparticles; model catalysts; thin-film catalyst
2.  Nanoscaled alloy formation from self-assembled elemental Co nanoparticles on top of Pt films 
The thermally activated formation of nanoscale CoPt alloys was investigated, after deposition of self-assembled Co nanoparticles on textured Pt(111) and epitaxial Pt(100) films on MgO(100) and SrTiO3(100) substrates, respectively. For this purpose, metallic Co nanoparticles (diameter 7 nm) were prepared with a spacing of 100 nm by deposition of precursor-loaded reverse micelles, subsequent plasma etching and reduction on flat Pt surfaces. The samples were then annealed at successively higher temperatures under a H2 atmosphere, and the resulting variations of their structure, morphology and magnetic properties were characterized. We observed pronounced differences in the diffusion and alloying of Co nanoparticles on Pt films with different orientations and microstructures. On textured Pt(111) films exhibiting grain sizes (20–30 nm) smaller than the particle spacing (100 nm), the formation of local nanoalloys at the surface is strongly suppressed and Co incorporation into the film via grain boundaries is favoured. In contrast, due to the absence of grain boundaries on high quality epitaxial Pt(100) films with micron-sized grains, local alloying at the film surface was established. Signatures of alloy formation were evident from magnetic investigations. Upon annealing to temperatures up to 380 °C, we found an increase both of the coercive field and of the Co orbital magnetic moment, indicating the formation of a CoPt phase with strongly increased magnetic anisotropy compared to pure Co. At higher temperatures, however, the Co atoms diffuse into a nearby surface region where Pt-rich compounds are formed, as shown by element-specific microscopy.
PMCID: PMC3190617  PMID: 22003453
alloy; Co; CoPt; epitaxy; HRTEM; magnetometry; nanoparticles; Pt; XMCD
3.  Platinum nanoparticles from size adjusted functional colloidal particles generated by a seeded emulsion polymerization process 
The benefits of miniemulsion and emulsion polymerization are combined in a seeded emulsion polymerization process with functional seed particles synthesized by miniemulsion polymerization. A systematic study on the influence of different reaction parameters on the reaction pathway is conducted, including variations of the amount of monomer fed, the ratio of initiator to monomer and the choice of surfactant and composition of the continuous phase. Critical parameters affecting the control of the reaction are determined. If carefully controlled, the seeded emulsion polymerization with functional seed particles yields monodisperse particles with adjustable size and functionalities. Size-adjusted platinum-acetylacetonate containing latex particles with identical seed particles and varied shell thicknesses are used to produce arrays of highly ordered platinum nanoparticles with different interparticle distances but identical particle sizes. For that, a self-assembled monolayer of functional colloids is prepared on a solid substrate and subsequently treated by oxygen plasma processing in order to remove the organic constituents. This step, however, leads to a saturated state of a residual mix of materials. In order to determine parameters influencing this saturation state, the type of surfactant, the amount of precursor loading and the size of the colloids are varied. By short annealing at high temperatures platinum nanoparticles are generated from the saturated state particles. Typically, the present fabrication method delivers a maximum interparticle distance of about 260 nm for well-defined crystalline platinum nanoparticles limited by deformation processes due to softening of the organic material during the plasma applications.
PMCID: PMC3190616  PMID: 22003452
colloid lithography; functional colloids; miniemulsion polymerization; nanoparticles; seeded emulsion polymerization
4.  Preparation and characterization of supported magnetic nanoparticles prepared by reverse micelles 
Monatomic (Fe, Co) and bimetallic (FePt and CoPt) nanoparticles were prepared by exploiting the self-organization of precursor loaded reverse micelles. Achievements and limitations of the preparation approach are critically discussed. We show that self-assembled metallic nanoparticles can be prepared with diameters d = 2–12 nm and interparticle distances D = 20–140 nm on various substrates. Structural, electronic and magnetic properties of the particle arrays were characterized by several techniques to give a comprehensive view of the high quality of the method. For Co nanoparticles, it is demonstrated that magnetostatic interactions can be neglected for distances which are at least 6 times larger than the particle diameter. Focus is placed on FePt alloy nanoparticles which show a huge magnetic anisotropy in the L10 phase, however, this is still less by a factor of 3–4 when compared to the anisotropy of the bulk counterpart. A similar observation was also found for CoPt nanoparticles (NPs). These results are related to imperfect crystal structures as revealed by HRTEM as well as to compositional distributions of the prepared particles. Interestingly, the results demonstrate that the averaged effective magnetic anisotropy of FePt nanoparticles does not strongly depend on size. Consequently, magnetization stability should scale linearly with the volume of the NPs and give rise to a critical value for stability at ambient temperature. Indeed, for diameters above 6 nm such stability is observed for the current FePt and CoPt NPs. Finally, the long-term conservation of nanoparticles by Au photoseeding is presented.
PMCID: PMC3045932  PMID: 21977392
Co; CoPt; core–shell particles; FePt; magnetic anisotropy; magnetic particles; plasma etching; reverse micelles; self-assembly

Results 1-4 (4)