碳负载尺寸可控的铂纳米粒子微波合成和表征

分别以XC-72碳和碳纳米管为载体,H₂PtCl₆为前驱体,用微波辐射加热的方法合成了碳负载的铂纳米粒子,并对其进行了EDX、TEM和XRD表征.研究了H₂PtCl₆乙二醇溶液的pH值对微波合成铂纳米粒子的大小、均匀性及其在碳载体上分散程度的影响.研究结果发现对于Pt/XC-72碳,随着pH值从3.4增加到9.5,铂纳米粒子的平均粒径从5.5nm减小到2.7nm;对于Pt/CNTs,随着pH值从3.5增加到9.4,铂纳米粒子的平均粒径从5.3nm减小到2.8nm.另外,随着pH值的增加,铂纳米粒子的尺寸均匀性及其在碳载体表面的分散程度得到改善.     

Synthesis of noble metal/carbon nanotube composites in supercritical methanol

A simple and efficient route has been employed to deposit noble metal nanoparticles (Pt, Ru, Pt-Ru, Rh, Ru-Sn) onto carbon nanotubes (CNTs) in supercritical methanol solution. In this method, the inorganic metallic salts acted as metal precursors, and methanol as solvent as well as reductant for the precursors. The as-prepared nanocomposites were structurally and morphologically characterized by X-ray diffraction spectroscopy, transmission electron microscopy (TEM), scanning electron microscopy, and X-ray photoelectron spectroscopy analyses. It was demonstrated that the CNTs were decorated by crystalline metal nanoparticles with uniform sizes and a narrow particle size distribution. The size and loading content of the nanoparticles on CNTs could be tuned by manipulating reaction parameters. Furthermore, the formation mechanism of the composites was also discussed.     

Precise control of the Pt nanoparticle size by seeded growth using EO13PO30EO13 triblock copolymers as protective agents

Here, we report an efficient way to produce homogeneous Pt nanoparticles within a well-defined size range (3.5-6.6 nm) as a result of the seeded growth procedure using Pluronic L64 polymer capping agent. First, small seeds (3.5 nm) were prepared by the reduction of H2PtCl6.6H2O in water with NaBH4 in the presence of the capping poly(ethylene oxide)13-poly(propylene oxide)30-poly(ethylene oxide)13 triblock copolymer at room temperature. Additional anionic Pt salt was then introduced under flowing H2 to obtain larger nanoparticles.     

Preparation of platinum nanoparticle and its catalytic activity for toluene oxidation

Colloidal Pt nanoparticles are prepared using H2PtCl6 as a precursor, polyvinylpyrrolidone (PVP: molecular weight = 10,000 and 40,000) and hydrogen as a stabilizing agent and a reducing agent, respectively. The amounts of the precursor and the stabilizing agent and the molecular weight of PVP have an effect on the formation of Pt nanoparticles. Supported Pt catalyst (CSPt) is prepared from colloidal Pt nanoparticles and y-Al2O3. Another supported Pt catalyst (ISPt) is prepared by using the conventional incipient wetness impregnation method with an aqueous H2PtCl6 solution and gamma-Al2O3. The catalytic activities of CSPt and ISPt catalysts are compared for VOC (toluene) oxidation. Transmission Electron Microscopy (TEM), UV-vis, X-ray diffraction (XRD) and temperature programmed reduction (TPR) are used to characterize CSPt and ISPt catalysts. The experimental results reveal that the catalytic activity of CSPt is superior to that of ISPT.     

Pt nanoparticles: Heat treatment-based preparation and Ru(bpy)(3)2+-mediated formation of aggregates that can form stable films on bare solid electrode surfaces for solid-state electrochemiluminescence detection

A simple thermal process for the preparation of small Pt nanoparticles is presented, carried out by heating a H2PtCl6/3-thiophenemalonic acid aqueous solution. The following treatment of such colloidal Pt solution with Ru(bpy)(3)2+ causes the assembly of Pt nanoparticles into aggregates. Most importantly, directly placing such aggregates on bare solid electrode surfaces can produce very stable films exhibiting excellent electrochemiluminescence behaviors.     

Facile synthesis of Pt multipods nanocrystals

A facile and efficient seeded growth approach was used to fabricate single-crystal Pt multipods nanocrystals, which were intensively characterized by TEM, ED, HRTEM, XRD, EDX, and XPS. The size and shape of Pt multipod nanocrystals can be easily controlled by varying the ratio of Pt seeds to H2PtCl6. The catalytic performance of these nanocrystals as heterogeneous catalysts was examined using the hydrogenation of cyclohexene as a model reaction in a biphasic system. These Pt nanocrystals should have potential applications as catalysts in organic synthesis, electronics, sensors, and other devices.     

可见光响应型Pt/GaP纳米粉体的光催化性质

利用水合肼液相还原法在纳米磷化镓(GaP)粉体表面沉积贵金属铂(Pt), 制备低Pt担载量Pt(0.80 wt%)/GaP和高Pt担载量Pt(4.2 wt%)/GaP纳米粉体样品. 在可见光照射条件下, 分别以GaP和Pt/GaP纳米粉体作为光催化剂, 对结晶紫水溶液进行光催化降解. 实验结果表明, GaP和Pt/GaP两种纳米粉体皆具有可见光响应光催化性能; Pt担载量对Pt/GaP纳米粉体的光催化性能有着较大的影响, 低Pt担载量Pt(0.80 wt%)/GaP纳米粉体的结晶紫光催化脱色率高于GaP纳米粉体, 而高Pt担载量Pt(4.2 wt%)/GaP粉体的结晶紫光催化脱色率则低于GaP纳米粉体.     

Rapid synthesis of cubic Pt nanoparticles and their use for the preparation of Pt nanoagglomerates

We report the synthesis of hexadecyltrimethylammonium bromide (CTAB)-stabilized cubic Pt nanoparticles by NaBH4 reduction of H2PtCl6 in aqueous CTAB solution. These Pt nanoparticles (average size of 7 nm) were well dispersed in aqueous solution and stable at least for 2 months. Addition of a trace amount of AgNO3 can alter the morphology of these Pt nanoparticles. More interestingly, the as-prepared uniform Pt nanoparticles were further developed into bigger Pt nanoagglomerates (approximately 20 to 47 nm) by a seed-mediate growth process. Dentritic and spherical Pt nanoagglomerates can be synthesized by altering the incubation time and their size can be tuned by controlling the amount of the seeds added.     

Facile synthesis of highly faceted multioctahedral Pt nanocrystals through controlled overgrowth

Highly faceted Pt nanocrystals with a large number of interconnected arms in a quasi-octahedral shape were synthesized simply by reducing H2PtCl6 precursor with poly(vinyl pyrrolidone) in aqueous solutions containing a trace amount of FeCl3. The iron species (Fe(3+) or Fe(2+)) play a key role in inducing the formation of the multioctahedral structure by decreasing the concentration of Pt atoms and keeping a low concentration for the Pt seeds during the reaction. This condition favors the overgrowth of Pt seeds along their corners and thus the formation of multiarmed nanocrystals. Electron microscopy studies revealed that the multioctahedral Pt nanocrystals exhibit a large number of edge, corner, and surface step atoms. The size of the multioctahedral Pt nanocrystals can be controlled by varying the concentration of FeCl3 added to the reaction and/or the reaction temperature. These multioctahedral Pt nanocrystals were tested as electrocatalysts for the oxygen reduction reaction in a proton exchange membrane fuel cell and exhibited improved specific activity and durability compared to commercial Pt/C catalyst.     

一步法制备L10相FePt纳米颗粒

以乙酰丙酮铁(Fe(acac)3)和氯铂酸(H2PtCl6.6H2O)分别作Fe源和Pt源,三缩四乙二醇(TEG)作溶剂和还原剂,聚乙烯基吡咯烷酮(PVP)作表面活性剂,通过多元醇还原法制备出单分散的FePt纳米颗粒。通过X射线衍射仪(XRD)及透射电子显微镜(TEM)分析表明,所制备的FePt纳米颗粒形状近似球形,分散性较好,平均颗粒粒径约为5.5nm。通过振动样品磁强计(VSM)分析显示所制备FePt纳米颗粒矫顽力为37.64kA/m,这意味着FePt纳米颗粒部分转变为面心四方相(L10相)。     

Tuning of catalytic CO oxidation by changing composition of Rh-Pt bimetallic nanoparticles

Recent breakthroughs in synthesis in nanoscience have achieved control of size and composition of nanoparticles that are relevant for catalyst design. Here, we show that the catalytic activity of CO oxidation by Rh/Pt bimetallic nanoparticles can be changed by varying the composition at a constant size (9+/-1 nm). Two-dimensional Rh/Pt bimetallic nanoparticle arrays were formed on a silicon surface via the Langmuir-Blodgett technique. Composition analysis with X-ray photoelectron spectroscopy agrees with the reaction stoichiometry of Rh/(Pt+Rh). CO oxidation rates that exhibit a 20-fold increase from pure Pt to pure Rh show a nonlinear increase with surface composition of the bimetallic nanoparticles that is consistent with the surface segregation of Pt. The results demonstrate the possibility of controlling catalytic activity in metal nanoparticle-oxide systems via tuning the composition of nanoparticles with potential applications for nanoscale design of industrial catalysts.     

乙二醇还原Ru／CNTs的制备及催化氨分解性能研究

为获得高分散的Ru负载催化剂,采用乙二醇液相化学还原沉积法制备Ru／CNTs,TEM、XRD、H2-TPD表征,结果表明,乙二醇液相还原法可以制备金属粒径小（2—4nm）而均匀的高分散度的钌修饰CNTs,其表面存在较高稳态浓度吸附氢。以氨分解制氢作探针反应,实验结果表明,在相同反应条件下,经乙二醇油浴液相还原沉积制备的Ru／CNTs催化剂上氨转化率约为浸渍法制得相应催化剂上的1．6倍,同时发现钌微晶粒径在3—4nm范围的Ru／CNTs对氨分解制氢的催化性能最佳,钌微晶粒径≤2nm时氨分解转化率明显下降。     

Controlled silver delivery by silver-cellulose nanocomposites prepared by a one-pot green synthesis assisted by microwaves

Controlled silver release from cellulosic nanocomposites was achieved by synthesizing silver nanoparticles, under microwave heating for 1-15 min, in a one-pot, versatile and sustainable process in which microcrystalline cellulose simultaneously functions as reducing, stabilizing and supporting agent in water; chitin, starch and other cellulose derivatives could also be used as reducing, stabilizing and supporting agents for silver nanoparticles and the method was also found to be extensible to the preparation of noble metal (Au, Pt) and metal oxide nanoparticle (ZnO, Cu, CuO and Cu(2)O) nanocomposites.     

Single-step high-speed nanogranulation of metal alloy around carbon nanotubes by flash light irradiation

We demonstrate to decorate carbon nanotubes (CNTs) with metal alloy nanoparticles by flash light from a xenon lamp highlighting dramatically simplified process and ultrafast speed of millisecond. By managing the pulse energy of the irradiation, we customize the nucleation and growth rates of homogeneous binary and ternary nanoparticles with Pt–Ru and Pt–Ru–Mo thin layers that are e-beam deposited onto CNTs. No damage of CNTs during the light-induced nanogranulation is guaranteed by the rapid and surface-localized heating mechanism. The fabricated nanoparticle/CNT nanostructures are characterized using variety of microscopic and spectroscopic techniques such as SEM, TEM and Raman spectroscopy.     

Fabrication of PtNi bimetallic nanoparticles supported on multi-walled carbon nanotubes

Platinum/nickel bimetallic nanoparticles supported on multi-walled carbon nanotubes (xPtNi/CNTs) were synthesised. The fabrication process includes the chemical modification on the graphene surface of CNTs by acid treatment and the subsequent deposition of Pt or PtNi bimetallic nanoparticles with different compositions of Pt (x = 100, 90, 80 and 70 wt%). The deposition was carried out using ethylene glycol as a reducing agent in the polyol method or using poly(amidoamine) dendrimer as a platform and sodium borohydride as a reducing agent to load the metal nanoparticles on the CNT surface. The structures of the produced PtNi/CNT nanoparticles were investigated by ultraviolet absorption spectra, X-ray diffraction (XRD) and the composite ratio consisting of 70 wt% of metal content and 30 wt% of CNTs was confirmed by the thermogravimetric analysis. The morphology and the phase identification of the produced PtNi/CNT nanoparticles were investigated by high-resolution scanning electron microscope, transmission electron microscope and XRD measurements. It was observed that the deposited Pt and PtNi bimetallic nanoparticles on the surface of CNTs had average particle sizes of 2–16 nm, when they were prepared from the polyol method. On the other hand, the PtNi/CNT nanoparticles prepared by using a dendrimer as an intermediate had a smaller particle size and more uniform size distribution of the quantum dot size ranged from 2 to 4 nm.     

微波辅助燃烧法制备镁铝尖晶石纳米粉体的研究

Stoichiometric MgAl2O4 spinel nanoparticles were synthesized by microwave assisted combustion reaction from aluminium nitrate nanohydrate(Al(NO3)3.9H2O) and Sol-Gel prepared magnesium hydroxide(Mg(OH)2) in the presence of urea((NH2)2CO) as a fuel,in about 20 min of irradiation.X-ray diffraction(XRD) studies reveal that mi-crowave assisted combustion synthesis route yields single-phase spinel nanoparticles with larger crystalline size(around 75 nm) than other conventional heating methods.Scanning electronic microscope(SEM) images show nanoparticles with spherical shape and homogenous morphology.The surface area measurements(SBET) show crystals with 2.11 m2/g and 0.0033 mL/g pore volume.     

One-pot synthesis of Pt/carbon nanotubes by self-regulated reduction for electrocatalysis

This paper describes a method for size-controlled synthesis of Pt nanoparticles and their attachment to the sidewalls of multiwall carbon nanotubes (CNTs) by self-regulated reduction of sodium n-dodecyl sulfate (SDS), without surface pretreatment. The size of the Pt nanoparticles is controlled by adjusting the concentration of SDS. When Pt/CNTs are heated to 500 degrees C in N2 atmosphere, Pt nanochains are formed on the CNTs; some of these nanochains contain small islands. Electrochemical measurements confirm that the electroactivities of the Pt/CNT nanocatalysts increase with a decrease in the size of the Pt nanoparticles. Additionally, comparing with the heated Pt/CNT nanocatalysts containing smooth Pt nanochains, the heated Pt/CNT nanocatalysts containing Pt nanochains with small Pt islands show higher electrocatalysis activities and stability.     

Preparation and catalytic activity of Pt/C materials via microwave irradiation

Microwave heating was employed to prepare highly dispersed Pt/C catalyst. Uniform platinum nanoparticles with average diameter of about 3.0-5.0 nm dispersed on carbon materials (XC-72) were synthesized using a domestic microwave oven. Synthesized Pt/C materials were characterized by X-ray diffraction and transmission electron microscopy. The particle size and size distribution of Pt nanoparticles greatly depend on microwave irradiation duration, where the heating temperature rises rapidly as the process proceeds. Cyclic voltammetry demonstrates that Pt/C catalysts derived from microwave irradiation for 90 s exhibits higher catalytic activity than a commercial Pt/C catalyst (E-Tek) at room temperature. The improvement in electrocatalytic activity of synthesized Pt/C materials is attributed to uniformity of particle size, well dispersion and high surface area, which is obtained around 175 °C and irradiation for 90 s.     

Grain size control of calcined SnO2 nanocrystals: Raman study and room temperature ethanol sensing properties

SnO2 nanoparticles were prepared via a sol-gel method by heating the mixture of hydrous SnO2 nanoparticles and SiO2 nanospheres at 600 degrees C. The average particle size of the obtained SnO2 nanoparticles is 3.3 nm, smaller than that of the SnO2 nanoparticles ( 6.4 nm) prepared by calcining the pure hydrous SnO2 at 600 degrees C. The restricting effect of SiO2 on the growth of SnO2 nanoparticles was discussed by Raman spectra. A blue shift of A1g ) and B2g Raman modes in SnO2/SiO2 composite was observed, and it was considered to be a compressive stress effect. The obtained SnO2 nanoparticles with a size of about 3.3 nm exhibit enhanced ethanol response at room temperature, and their recovery time is much shorter than that of the SnO2 nanocrystals with a size of about 6.4 nm.     

载体炭与Pt催化剂之间的相互作用及其引起的尺寸效应(英文)

通过乙二醇还原,在VulcanXC-72炭黑上负载了三种具有不同平均粒径(1.7nm,3.0nm和5.0nm)的Pt催化剂。利用透射电子显微镜,研究了载体炭黑表面的微孔与Pt催化剂之间的几何相互作用。结果表明:尺寸较小的Pt颗粒(平均粒径为1.7nm)通常被包含在载体表面的微孔中,表现为被一薄碳层所覆盖并嵌入炭黑基体。而尺寸较大的Pt颗粒(平均粒径为3.0nm和5.0nm)则不存在这种现象,往往显示出裸露的清洁表面。这种与载体表面微孔的不同相互作用引起了Pt颗粒在电化学活性比表面上的反常尺寸效应,进而影响了其催化甲醇氧化的质量比活性。