Decomposition Of Metalorganic Precursors Research Articles

Preparation and Investigation of Pd and Bimetallic Pd-Sn Nanocrystals on γ-Al2O3

One of the key factors for producing highly dispersed controlled nanoparticles is the method used for metal deposition. The decomposition of metal-organic precursors is a good method for deposition of metal nanoparticles with very small sizes and narrow size distributions on the surface of various supports. The preparation process of Pd and bimetallic Pd-Sn nanoparticles supported onto γ-Al2O3 is considered. The samples were prepared by diffusional co-impregnation of the γ-Al2O3 support by using organometallic Pd(acac)2 and Sn(acac)2Cl2 precursors. To achieve the formation of Pd and bimetallic Pd-Sn nanoparticles on the support surface, the synthesized samples were then subjected to thermal decomposition under Ar (to decompose the organometallic bound to the surface while keeping the formed nanoparticles small) followed by an oxidation in O2 (to eliminate the organic compounds remaining on the surface) and a reduction in H2 (to reduce the nanoparticles oxidized during the previous step). A combination of methods (ICP-OES, TPR-H2, XPS, TEM/EDX) was used to compare the physical-chemical properties of the synthesized Pd and bimetallic Pd-Sn nanoparticles supported on the γ-Al2O3. The three samples exhibit narrow size distribution with a majority on nanoparticles between 3 and 5 nm. Local EDX measurements clearly showed that the nanoparticles are bimetallic with the expected chemical composition and the measured global composition by ICP-OES. The surface composition and electronic properties of Pd and Sn on the γ-Al2O3 support were investigated by XPS, in particular the chemical state of palladium and tin after each step of thermal decomposition treatments (oxidation, reduction) by the XPS method has been carried out. The reducibility of the prepared bimetallic nanoparticles was measured by hydrogen temperature programmed reduction (TPR-H2). The temperature programmed reduction TPR-H2 experiments have confirmed the existence of strong surface interactions between Pd and Sn, as evidenced by hydrogen spillover of Pd to Sn (Pd-assisted reduction of oxygen precovered Sn). These results lead us to propose a mechanism for the formation of the bimetallic nanoparticles.

GaAs nanowires grown by Ga-assisted chemical beam epitaxy: Substrate preparation and growth kinetics

Growth kinetics of GaAs nanowires (NWs) on Si(111) substrates by Ga-assisted chemical beam epitaxy is studied as a function of growth conditions such as substrate temperature (Ts), V/III flux ratio and catalyst dimension. The preparation method for Si(111) substrates is optimized in order to obtain a thin surface oxide with a thickness around 0.5nm, allowing both the decomposition of metalorganic precursors and GaAs nucleation at oxide pinholes. The use of thinner oxides enables the growth of a GaAs layer whereas the utilization of thicker oxides could even inhibit GaAs nucleation. The successful self-formation of Ga droplets over this slightly oxidized Si surface has been observed by scanning electron microscopy (SEM), whose initial size is demonstrated to affect both the NW growth rate and the resultant NW aspect ratio. The formation of these droplets is crucial to enable the catalytic growth of NWs whose morphology is thoroughly analyzed by SEM, showing a self-organized array of vertically aligned match shaped GaAs NWs with a hexagonal footprint. In addition, the crystalline structure of NWs is monitored in-situ by reflection high energy diffraction, showing pure zincblende phase along the whole NW stem.In terms of better NW aspect ratio, higher crystalline quality and faster growth rates, the best NW growth conditions are found at Ts=580°C, using an effective flux ratio V/III≈0.8. Moreover, NW growth kinetics is demonstrated to be improved when using a pre-deposited Ga coverage of 7.5 monolayers, stabilized for 90s prior to the NW growth.

Influence of metal organic and inorganic precursors on spray pyrolyzed ceramic MgO (2 0 0) thin films for epitaxial over layers

The MgO (2 0 0) surface is widely used as a substrate for epitaxial growth of superconducting and ferro-electric films. Highly oriented, single crystalline, extremely flat and transparent MgO films have been successfully deposited on quartz substrates by the chemical spray pyrolysis technique using economically viable metal organic and inorganic precursors under optimized conditions at the substrate temperature of 600 °C. Thermal analysis (TGA/DTA) in the temperature range 30–600 °C with the heating rate of 10 °C/min revealed the decomposition behavior of the precursors and confirmed the suitable substrate temperature range for film processing. The heat of reaction, Δ H due to decomposition of metal organic precursor contributed additional heat energy to the substrate for better crystallization. The intensity of the (2 0 0) peak in X-ray diffraction (XRD) measurements and the smooth surface profiles revealed the dependency of precursor on film formation. The compositional purity and the metal–oxide bond formation were tested for all the films. UV–Vis–NIR optical absorption in the 200–1500 nm range revealed an optical transmittance above 80% and the absorption edge at about 238 nm corresponding to an optical band gap E g = 5.25 eV. Scanning electron microscopy (SEM) and atomic force microscopy (AFM) micrographs of MgO films confirmed better crystallinity with larger grain size (0.85 μm) and reduced surface roughness (26 nm), respectively.

A thermal analysis evaluation of the low temperature synthesis of BaBiO3

Thermal decomposition of metal-organic precursors for the mixed oxide BaBiO3 was studied using TG and EGA. Precursors produced by polyesterification of bifunctional acids with ethylene glycol (Pechini process) decomposed about 100°C higher than those without the diol. BaCO3 was identified by IR and XRD as a reaction intermediate. EGA proved that the amount of BaCO3 was below 10% of the total barium, and that the barium exists mainly as a nitro-compound up to 650°C. Phase-pure BaBiO3 with a moderately high surface area (1.4 m2/g) could be synthesised from a citrate precursor by the Pechini process at around 850°C.