超声化学制备单分散金属纳米钯

A simple sonochemical technique is used to synthesize palladium nanoparticles in a poly(ethylene glycol) (PEG) solvent at room temperature. The reaction based on chemical reduction of PdCl₂ by ascorbic acid (AA). The as prepared Pd nanoparticles are highly dispersed and uniform in size (with average size of ～20nm). The products were characterized by X-ray powder diffraction (XRD) and transmission electron microscopy (TEM).     

羧基功能化离子液体修饰Pd纳米微粒的制备及结构表征

1-methyl-3-(ω-carboxyl)decyl imidazolium bromine ([C₁₁OOHmim]Br) ionic liquid was synthesized and [C₁₁OOHmim]Br modified Pd nanoparticles were prepared in solution. The morphology and structure of Pd nanoparticles were investigated by IR, TEM, XRD, XPS. The results indicated that the Pd nanoparticles were face-centered cubic structure and the diameter was between 10～30 nm. [C₁₁OOHmim]Br was connected to the surface of Pd nanoparticles by carboxyl and Pd nanoparticles with different sizes could be obtained by varying the amount of the modifier.     

Sonochemical Synthesis of Three-dimensional Aggregates of Pd Nanoparticles with High Electrocatalytic Activity Towards Ethanol Oxidation

Flower-like aggregates composed of （4.0±0.8） nm palladium（Pd） nanoparticles were prepared via ultrasonics in the palladium（Ⅱ） chloride（PdCl2） H2O/EtOH（5/1,volume ratio） solution with the addition of a quantity of poly（vinyl pyrrolidone）（PVP） and sodium dodecyl sulfonate（SDS）.The morphologies,crystal structures and the optical properties of the flower-like Pd nanostructures were characterized by X-ray diffraction（XRD）,X-ray photoelectron spectroscopy（XPS）,scanning electron microscopy（SEM）,transmission electron microscopy（TEM）,selected area electron diffraction（SAED） and UV-visible absorption spectroscopy,respectively.The mechanism of sonochemical reduction of Pd（Ⅱ） ions was also investigated.The results show that the molar ratio of PVP to SDS affected the formation of the flower-like aggregates of Pd nanoparticles.Moreover,the electrocatalytic properties of Pd aggregates modified glassy carbon electrode for ethanol oxidation were also investigated by cyclic voltammetry（CV）.This material exhibits remarkable electrocatalytic activity for ethanol oxidation in 1 mol/L KOH and appears as a promising candidate to be applied in direct ethanol fuel cells.     

Co-modified Pd/CeO2-ZrO2 catalysts for methanol decomposition

Pd/Ce0.8Zr0.2O2 catalysts modified by cobalt were prepared by a sequential impregnation method and characterized by X-ray powder diffraction(XRD), N2adsorption/desorption(Brunauer-Emmet-Teller), oxygen storage capacity(OSC), CO-chemisorption, H2-temperature-programmed reduction(H2-TPR) and X-ray photoelectron spectroscopy(XPS). The effect of Co on the performance of methanol decomposition was evaluated at a fixed-bed microreactor. The results showed that the addition of Co can improve the oxygen storage capacity of the catalyst and the dispersion of Pd. XPS results indicated that Pd was in a partly oxidized(Pdδ+, 1δ2) state and Co2+was present in Pd catalysts modified by Co. A 90% conversion of methanol was achieved at around 280°C over Pd-Co/Ce0.8Zr0.2O2 catalyst which was 20°C lower than that over Pd/Ce0.8Zr0.2O2, indicating that both Pdδ+and Co2+play an important role in improving the catalytic activity of methanol decomposition.     

Co-modified Pd/CeO_2-ZrO_2 catalysts for methanol decomposition

Pd/Ce0.8Zr0.2O2 catalysts modified by cobalt were prepared by a sequential impregnation method and characterized by X-ray powder diffraction(XRD), N2adsorption/desorption(Brunauer-Emmet-Teller), oxygen storage capacity(OSC), CO-chemisorption, H2-temperature-programmed reduction(H2-TPR) and X-ray photoelectron spectroscopy(XPS). The effect of Co on the performance of methanol decomposition was evaluated at a fixed-bed microreactor. The results showed that the addition of Co can improve the oxygen storage capacity of the catalyst and the dispersion of Pd. XPS results indicated that Pd was in a partly oxidized(Pdδ+, 1δ2) state and Co2+was present in Pd catalysts modified by Co. A 90% conversion of methanol was achieved at around 280°C over Pd-Co/Ce0.8Zr0.2O2 catalyst which was 20°C lower than that over Pd/Ce0.8Zr0.2O2, indicating that both Pdδ+and Co2+play an important role in improving the catalytic activity of methanol decomposition.     

溶剂热制备条件对镍晶体结构的影响

Nickel powders were obtained after chemical reduction of nickel chloride by KBH₄ using absolute ethylenediamine as solvent in a stainless autoclave. The product was characterized by X-ray powder diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). XRD results show that the as-prepared sample have different crystal structures at different reaction temperatures. It was face-centered cubic (fcc) nickel under 200 ℃, and there was only hexagonal close-packed (hcp) Ni above 300 ℃. At 250 ℃, the patterns indicate that both fcc and hcp phases of Ni coexist in the as-prepared sample. When the ethylenediamine was respectively substituted by benzene and toluene, only fcc phase nickel was obtained. SEM and TEM indicate that the fcc Ni is nano-particles with about 100 nm in diameter, and hcp nickel is nano-crystalline clusters.     

羟基功能化离子液体中Pd纳米微粒制备与结构表征

1-Ethoxyl-3-methyl imidazolium tetrafluoroborate ([C₂OHmim]BF₄)， 1-(4′-hydroxyl)-butyl-3-methyl imidazolium tetrafluoroborate ([C₄OHmim]BF₄) and 1-(6′-hydroxyl)-hexyl-3-methyl imidazolium tetrafluoroborate([C₆OHmim]BF₄) were synthesized and then Pd nanoparticles were prepareds in these ionic liquids .The structure and shape of Pd nanoparticles were investigated by XRD and TEM. The results indicate that the Pd nanoparticles are fcc structure and there are some differences in the diameter of Pd nanoparticles prepared in different ionic liquids， i.e. 150 nm， 30 nm， 10 nm， respectively. The formation mechanism of nanoparticles is proposed.     

Pt3Co核-Pt壳型纳米粒子的制备及磁性

Pt₃Co alloy nanoparticles were prepared by the reduction of H₂PtCl₆ and Co(OOCCH₃)₂ using NaBH₄ as a reducing agent. The Pt₃Co core-Pt shell nanoparticles (Pt₃Co@Pt) were synthesized using hydrogen absorption reduction and characterized by plasma-atomic emission spectrometry (ICP), transmission electron microscopy (TEM), X-ray diffraction (XRD) and SQUID magnetometer. The results show that average size of Pt₃Co@Pt nanoparticles is 3.6 nm with a standard deviation of 0.9 nm. Heating Pt₃Co nanoparticles in air at 700 ℃ for 1 h, Co in Pt₃Co nanoparticles was oxidized to Co₃O₄ and CoO; while no oxidation tendency was detected for Pt₃Co@Pt nanoparticles. The crystallize structure of Pt₃Co@Pt changed from the face centered cube (fcc) to the face centered tetragonal (fct) after the heating treatment. The coercivity of the heated Pt₃Co@Pt reached to 276 Oe at room temperature.     

TiSe2纳米管的制备和表征

The ball-milled mixture of Ti and Se powders was carried out a solid-phase reaction at 600℃.The asprepared sample had been characterized by X-ray diffraction(XRD),scanning electron microscopy(SEM),transmission electron microscopy(TEM)and high-resolution transmission electron microscopy(HRT EM).The result shows that the products are multiwalled TiSe₂ nanotubes with open-ended tips,which are about 15nm in outer diameter,several micron in lengths,and 0.6nm of interlayer spacing.     

PEG还原Cu(Ⅱ)制备Cu2O纳米立方晶

Cuprous oxide (Cu₂O) nanocubes have successfully been prepared through a simple and novel method by heating Cu(ethyl acetoacetate)₂ (Cu(EAC)₂) and poly(ethyleneglycol) (PEG) in the absence of other chemicals. The PEG acted as the reducing agent as well as the stabilizer. The XRD results indicated that no metal Cu or CuO developed in the preparation process, and only Cu₂O nanoparticles with the cuprous structure were produced. The TEM images revealed that all the Cu₂O nanoparticles were cubic-shaped or square-shaped particles. The size and shape of Cu₂O nanocubes were dependent on concentrations of the Cu(Ⅱ) precursor, reactant temperatures, and chain length of PEGs. It is interesting that the reducing reactivity of PEG was sensitive to its chain length, and the reduction reaction activity was drastically dropped with the decreasing of polymer′s chain length.