液相分散法制备硬脂酸修饰铋纳米微粒

金属纳米微粒由于具有不同于普通材料的光、电、磁、热力学和化学反应等性能,在催化、信息存储、光电、微电子以及润滑等领域中有着广阔的应用前景。金属纳米微粒这些特殊的物理化学性能主要取决于制备工艺和具体的反应条件,因此研究具有特定性能的金属纳米微粒一直是纳米技术领域中的一个研究热点犤1,2犦,目前制备金属纳米微粒最常用的方法是液相法,它是通过在含有表面修饰剂的溶剂中还原相应的金属盐犤3,4犦或有机金属化合物热分解犤5,6犦来制备表面修饰的金属纳米微粒。虽然这种方法能够制备出多种具有特定性能的金属纳米微粒,但是这种方…     

超声电化学制备PbSe纳米枝晶

近年来，纳米晶态半导体粒子因其具有大的表面体积比、高的活性、特殊的电学性质和独特的光学性质引起了科学界的广泛关注犤１，２犦。基于半导体纳米粒子的量子尺寸效应和表面效应，半导体纳米粒子在发光材料犤３犦、非线性光学材料犤４犦、光敏传感器材料犤５犦、光催化材料犤６犦等方面具有广阔的应用前景。如何实现对半导体纳米粒子的尺寸大小、粒度分布以及形状和表面修饰的控制，寻找更简便的合成方法以及改善制备环境等是半导体纳米粒子研究的关键。超声电化学是结合了电化学和超声辐照而建立起来的一种新方法，它显示了两者的优点犤…     

纳米AgBr乳剂的制备及其紫外吸收光谱的研究

通常人们把粒径1~100 nm之间的金属、半导体、氧化物及各种化合物的粒子或者粒子的集合体称为纳米粒子。近年来的纳米粒子化学和物理的迅速发展已经证实:随着原子或分子簇尺寸的减小,表面原子的比例逐渐增大,粒子表现了与块状材料不同的特性,其粒子显示出以“量子尺寸效应”为主的特点,特性表现出种种异常^[1,2]。     

介电限域效应对SnO_2纳米微粒光学特性的影响

半导体纳米微粒作为一种新兴材料，在声、光、电、磁、热及催化等方面显示出全新的异于体相材料和分子或原子的特性，在理论和实验上已引起。们极大的兴趣I‘，’］．当纳米微粒的尺寸接近或小于激于玻尔半径时，表现出明显的量子尺寸效应，其表现光学能隙变大，一些半导体粒子如CdS，Cdse等纳米微粒的量予尺寸效应已经被人们利用有效质量近似模型做了定性解释。八但是，由于纳米微粒尺寸小，具有相对大的表面积，因而粒子周围的介质可以强烈地影响它们的光学性质【’，‘1．我们采用胶体化学方法，对SnO。阶电常数为13）半导体纳米微粒…     

钛氧有机化合物常压低温液相合成纳米二氧化钛晶体的研究

二氧化钛晶体有三种晶型，锐钛矿型、金红石型和板钛矿型，每一种晶型都表现出不同的性质，如光折射指数、化学反应性和光催化活性。锐钛矿和金红石型纳米二氧化钛在催化剂犤１，２犦、太阳能转化犤３～６犦、功能陶瓷犤７～９犦、湿度和高温氧气的敏感元件犤１０犦、化妆品犤１１犦和无机膜犤１２犦等许多方面都有广泛的应用前景。金红石型TiO２比锐钛矿型稳定，有较高的硬度、密度、介电常数和折射率，因此在高级涂料、化妆品和电子陶瓷等方面有着更重要的应用价值。锐钛矿型纳米TiO２晶体已发展的制备法主要有Sol－Gel法犤１３，１４…     

氧化锌-银复合纳米粒子的制备：吸收光谱和荧光光谱

金属和半导体纳米粒子的制备及性质的研究是当今材料科学和物理化学的热门课题［1－6］．在利用太阳能光降解环境污染物、生物传感器以及光生物等方面这些纳米粒子都具有实际应用的可能性．对纳米粒子表面进行修饰而形成的复合纳米粒子可以有效地调整单一颗粒的表面性质甚至颗粒的稳定性．另外，复合纳米粒子的制备对研究纳米粒子的尺寸量子化效应、非线性光学性质及其它光电性质都有重要的意义．人们已成功地制备了许多复合金属－金属纳米粒子，如Cu－Ag［7］，Ag-Pd［8］及Ag－Pt［9］等．关于复合半导体－半导作纳米粒子也有报导，如C…     

Zn(Oxin)2·2H2O纳米晶的固相化学反应合成及表征

随着纳米微粒研究的深入,对纳米超细微粒提出了不同的物理、化学特性需求,制备高纯、超细、均匀的纳米微粒,发展新型的纳米材料,就显得非常重要,而解决问题的关键在于研究、发展新的合成技术.通常,纳米微粒制备的要求是:表面洁净;粒子形状及粒径、粒度分布可控,防止粒子团聚;易于收集;有较好的稳定性;产率高.     

石墨烯负载的金属氧化物纳米颗粒的可控制备及催化性能

采用直接浸渍法、过氧化氢均相氧化沉积法和氨水催化水解法制备了石墨烯负载的铁、钴、镍金属氧化物纳米颗粒.研究了三种沉积方法对颗粒尺寸分布的影响;采用透射电子显微镜、傅里叶变换红外光谱、X射线衍射和X射线光电子能谱表征了催化剂的形貌与结构.用过氧化氢均相氧化沉淀法可制得粒径分布最均匀的纳米颗粒.过氧化氢的氧化作用可使石墨烯表面的氧化基团含量最大化,为纳米颗粒提供了足够的吸附与成核点.氨水加速了金属离子的水解与成核,导致纳米颗粒的粒径增大与不均.以苯甲醇氧化为探针反应考察了催化剂的性能.催化剂的活性按以下顺序逐渐下降:过氧化氢辅助沉积法>直接浸渍法>氨水催化水解法,与纳米颗粒尺寸增长趋势一致.纳米催化剂颗粒尺寸与其活性的良好关联性显示,发展石墨烯负载尺寸可控的纳米催化剂的方法具有重要意义.     

ITO/TiO2表面电沉积CdS纳米粒子及其薄膜的光电性能

采用阴极恒电位沉积方法, 在TiO2表面沉积制备出CdS纳米粒子. XRD和SEM测试结果表明, CdS粒子的结构以六方晶相为主, 粒径分布均匀, 表面形貌呈菜花状. 通过调节沉积电位和沉积时间等因素在一定程度上可以控制CdS纳米粒子的生长. 随着沉积电位变负, CdS粒子的粒径逐渐减小. 沉积时间越短, 粒子粒径越小. 紫外-可见吸收光谱测试结果表明, 不同条件下制备出来的CdS粒子表现出一定的量子尺寸效应. 此外, 沉积条件也会影响ITO/TiO2/CdS复合半导体薄膜的光电性能.     

甲醛在PtAuPd纳米合金/巯基功能化离子液体修饰电极上的电催化氧化

近年来,金属纳米粒子在催化、电学和光学等领域引起了人们的广泛兴趣~([1]).与单一金属纳米粒子相比,合金纳米粒子常常具有更多、更好的性能.制备粒径小且分布均匀的合金纳米粒子是开展相关研究应用的重要环节.     

Preparation of Au Nanoparticles on Surface of Two Supports by Adsorption Phase Synthesis

By utilizing adsorption phase synthesis (APS), Au nanoparticles were prepared on the surface of SiO₂ with or without modification by Ni(OH)₂. TEM, XRD, and UV‐vis were employed to characterize the morphology of Au particles on the surface of two kinds of supports. The results showed that the average size of Au particles on the SiO₂ surface modified by Ni(OH)₂ was less than 5 nm. Due to high surface isoelectric point, Au particles formed in the adsorption layer were prone to distribute on the surface of SiO₂ modified by Ni(OH)₂. With content of Ni(OH)₂ in samples increasing, more Au particles with small size appeared on the support surface.     

α-Al2O3纳米粒子对Co-Ni合金异常共沉积电化学行为的影响

为了研究在电化学复合共沉积过程中,惰性纳米粒子和金属离子、电极表面的相互作用,以及由此产生的对合金电化学共沉积行为的影响.本文从两个吸附过程出发: 电解液中的金属离子和H＋在纳米粒子表面的吸附；纳米粒子迁移到阴极表面,在电极表面的吸附.采用Zeta电势和稳态极化以及电化学交流阻抗（EIS）研究了纳米Al2O3粒子和电解液中的金属离子，和电极表面的相互作用,进而分析了纳米粒子对Co2＋和Ni2＋还原沉积的影响规律.通过对阻抗数据的拟合,讨论了Al2O3纳米粒子对等效电路中各物理参数的影响.在H＋和不同金属离子在纳米粒子上发生竞争吸附的基础上,提出了纳米粒子和合金共沉积的可能反应历程.     

氧化锆改性的Ni/LaAl11O18用于CO甲烷化反应:催化剂结构对催化性能的影响

对于煤制天然气,CO甲烷化技术起着重要作用,其研究核心之一是高效催化剂的开发.目前,CO甲烷化催化剂主要采用金属Ni作为活性组分,但存在高温易烧结和易积炭等问题.因此,如何使其同时具有较高的催化活性和高温稳定性是亟待解决的问题.针对这些问题,本文以高热稳定性的六铝酸镧(LaAl11O18)为载体,采用浸渍法担载金属镍,制备了Ni/LaAl11O18催化剂;以高化学惰性的ZrO2为包覆层,采用改进的连续吸附反应法,将ZrO2前驱体液相沉积在Ni/LaAl11O18表面进行改性,制备了具有包覆结构的Ni/LaAl11O18@ZrO2甲烷化催化剂.探讨了ZrO2在Ni/LaAl11O18表面的分布形式以及不同沉积包覆量对催化剂结构、CO甲烷化催化剂活性和稳定性的影响.分别采用氮气物理吸附、X射线衍射、透射电镜、扫描电镜、氢气程序升温还原、氢气程序升温脱附、X射线光电子能谱、热重分析和电感耦合等离子体原子发射光谱法等手段对催化剂进行了系统表征.结果表明,ZrO2纳米粒子能够同时分布在催化剂活性组分和载体表面,增加了金属?载体间相互作用力,高温还原时可以有效抑制活性金属Ni的烧结,成功构筑了具有显著限域结构的包覆型催化剂.同时,ZrO2的包覆不利于金属的氢气化学吸附.在常压,260?600 oC和120 L g?1h?1条件下对催化剂进行了催化活性测试.结果显示,与未改性的催化剂相比,包覆后催化剂上CO转化率略有降低,但是其CH4选择性明显提高,适量的ZrO2包覆对CH4得率有较好的促进作用,但是过量的ZrO2包覆会因占据过多的金属镍表面使得CO转化率显著降低.在常压,550 oC和120 L g?1h?1空速的操作条件下所进行的107 h稳定性测试结果表明,包覆型Ni/LaAl11O18@ZrO2催化剂展示了良好的高温稳定性,具有优异的抗烧结和抗积碳性能.这主要是因为包覆型催化剂具有良好的"限域"效应,从而显著改善了催化剂的抗烧结性能;同时较强的金属?载体相互作用以及ZrO2助剂对CO2的活化提升了催化剂的消碳能力,增强了Ni/LaAl11O18@ZrO2催化剂的抗积碳能力.总之,本文构筑了一种高稳定性的包覆型催化剂Ni/LaAl11O18@ZrO2,可广泛应用到其他多种高温反应中.     

Monte Carlo simulations of segregation in Pt-Ni catalyst nanoparticles

We have investigated the segregation of Pt atoms in the surfaces of Pt-Ni nanoparticles, using modified embedded atom method potentials and the Monte Carlo method. The nanoparticles are constructed with disordered fcc configurations at two fixed overall concentrations (50 at. % Pt and 75 at. % Pt). We use octahedral and cubo-octahedral nanoparticles terminated by {111} and {100} facets to examine the extent of the Pt segregation to the nanoparticle surfaces at T=600 K. The model particles contain between 586 and 4033 atoms (particle size ranging from 2.5 to 5 nm). Our results imply that a complete {100}-facet reconstruction could make the cubo-octahendral Pt-Ni nanoparticles most energetically favorable. We predict that at 600 K due to segregation the equilibrium cubo-octahedral Pt50Ni50 nanoparticles with fewer than 1289 atoms and Pt75Ni25 nanoparticles with fewer than 4033 atoms would achieve a surface-sandwich structure, in which the Pt atoms are enriched in the outermost and third atomic shells while the Ni atoms are enriched in the second atomic shell. We also find that, due to an order-disorder transition, the Pt50Ni50 cubo-octahedral nanoparticles containing more than 2406 atoms would form a core-shell structure with a Pt-enriched surface and a Pt-deficient homogenous core.     

Electrophoretic deposition of nickel, iron and aluminum nanoparticles on carbon fibers

The electrophoretic deposition (EPD) of nickel (Ni), iron (Fe) and aluminum (Al) nanoparticles fabricated by an active hydrogen plasma evaporation method on the surface of carbon fibers was investigated, which will allow the obtained composites to be applied as practical catalysts or electrodes. SEM observations show that the Ni nanoparticles can build up a thick EPD coating with some cracks on the surface of carbon fibers, and the analyses of X-ray diffraction (XRD) and BET specific surface area indicate that fine particles from the as-received Ni powders were finally deposited after the EPD process without crystal growth. The surface oxidation of Fe and Al nanoparticles takes serious effect on the EPD process and the morphology of the as-prepared coatings.     

Composition-dependent sintering behaviour of chemically synthesised CuNi nanoparticles and their application in aerosol printing for preparation of conductive microstructures

Copper, nickel and copper–nickel nanoparticles were prepared by solution combustion method for use in direct write printing. Structural (X-ray diffraction) and morphological (transmission electron microscope) investigations showed that pure metal (Cu and Ni) and CuNi alloy particles with face-centred cubic crystal structure were formed. Atomic absorption spectrometer studies confirmed that the nanoparticle compositions corresponded to the initial Cu/Ni molar ratios selected for synthesis. Particle size and morphology were significantly influenced by composition, with high Cu content coinciding with small, spherical particles as opposed to larger, irregular shapes observed at high Ni concentrations. X-ray photoelectron spectroscopy measurements revealed that after the reduction process the surface of the alloy nanoparticles was partially oxidised in air and the amount of metallic surface species decreased, while the concentration of oxidic surface species and hydroxides increased with increasing Cu concentration (i.e. decreasing particle size). Dispersions of CuNi nanoparticles have been deposited by use of AerosolJet? and sintered under reducing atmosphere at 300–800?°C in order to prepare conductive structures. Resistivity measurements and microscopical studies (SEM-FIB) of printed and sintered CuNi structures showed that the sintering properties of nanoparticles were dependent on their chemical composition.     

Liquid-phase Reductive Deposition as Novel Preparation Method for Highly Dispersive Nickel Catalysts

We have been developing the selective deposition method onto TiO₂ nanoparticles, named as the liquid-phase selective-deposition method, where TiO₂ plays a role of formation center of Ni nanoparticles as well as protection from the aggregative growth of the particles. The concept of this method is to well disperse and stabilize Ni nanoparticles on TiO₂ surface by specific adsorption of Ni precursory complexes and then heterogeneous nucleation on the adsorption sites. The particle size was decreased with increasing the amount of Zn added, thus the catalytically active Ni surface area was increased. The selective deposition onto TiO₂ surface and addition of Zn to the nanoparticle promoted the catalytic activity of Ni–Zn nanoparticle, e.g. the catalytic activity of Ni–Zn/TiO₂ was ca. 10 times higher than that of the unsupported Ni nanoparticles. Ni in the nanocomposite was assigned as metallic, although their surface was oxidized under the atmospheric condition, but Zn and B were deposited as their oxide.     

SiC表面Ni沉积超疏水膜层的形成机理

前期采用环境友好方法制备的改性碳化硅颗粒,经较长时间放置,发现其由亲水性转变为超疏水性,接触角为156°。为解释这一新的现象,采用扫描电子显微镜、能谱、(高分辨)透射电子显微镜、X射线光电子能谱(XPS)对原粉碳化硅、改性后碳化硅及久置碳化硅进行了测试与分析。结果显示：改性后碳化硅经较长时间放置,表面胞状颗粒增大并出现凸起物,粗糙度增加,存在类似于荷叶的微纳米结构。改性后颗粒的主要成分为Ni、Si、O,其中凸起处Ni、O元素的含量明显高于凹陷处。Ni颗粒表面出现清晰的膜层,膜层厚度为2~3 nm,但结晶度偏低。XPS测试结果显示金属镍的特征峰正向移动近4eV,与镍的氧化态特征峰相一致,从而解释了颗粒表面形态发生细小改变,自发形成超疏水膜层的机理。     

SiC表面Ni沉积超疏水膜层的形成机理

前期采用环境友好方法制备的改性碳化硅颗粒,经较长时间放置,发现其由亲水性转变为超疏水性,接触角为156°。为解释这一新的现象,采用扫描电子显微镜、能谱、(高分辨)透射电子显微镜、X射线光电子能谱(XPS)对原粉碳化硅、改性后碳化硅及久置碳化硅进行了测试与分析。结果显示：改性后碳化硅经较长时间放置,表面胞状颗粒增大并出现凸起物,粗糙度增加,存在类似于荷叶的微纳米结构。改性后颗粒的主要成分为Ni、Si、O,其中凸起处Ni、O元素的含量明显高于凹陷处。Ni颗粒表面出现清晰的膜层,膜层厚度为2～3 nm,但结晶度偏低。XPS测试结果显示金属镍的特征峰正向移动近4 eV,与镍的氧化态特征峰相一致,从而解释了颗粒表面形态发生细小改变,自发形成超疏水膜层的机理。     

Simple and low-cost electrochemical sensor based on nickel nanoparticles for the determination of cabergoline

Cabergoline (CAB) is an ergot alkaloid derivative with dopamine agonist activity. In this work for the first time the electrocatalytic oxidation of CAB was carried out with nickel nanoparticles-modified carbon paste electrode using cyclic voltammetry, chronoamperometry, chronocoulometry and amperometry methods. At first, nickel nanoparticles were synthesized by non-aqueous polyol method and these nanoparticles were mixed with graphite powder to form modified carbon paste electrode. The resulting modified electrode was characterized by scanning electron microscope images. In the presence of 0.1 M NaOH a good redox behavior of the Ni(III)/Ni(II) couple at the surface of the electrode can be observed. CAB was successfully oxidized at the surface of the modified electrode. The electrocatalytic oxidation peak current of this drug was linearly dependent on its concentration. The proposed sensor exhibited a high sensitivity and was successfully applied for the determination of CAB in real samples.