油相稳定分散Fe3O4纳米粒子的制备研究

分别采用热分解法及共沉淀油酸同步修饰法制备了2种可以在油相稳定分散的Fe3O4纳米粒子,并对热分解法制备Fe3O4纳米粒子的反应条件进行了优化,考察了热分解温度、熟化时间对颗粒粒径、形貌及磁性能的影响。通过TEM、VSM和FTIR等表征手段对2种方法制备的Fe3O4纳米粒子的油相分散稳定性、颗粒形貌及粒径、比饱和磁化强度及表面性质进行了比较。结果表明:热分解法制备的Fe3O4纳米粒子表现出更好的油相分散稳定性,共沉淀油酸同步修饰法制备的Fe3O4纳米粒子则表现出更好的磁响应性。     

静电纺丝技术制备LaF3/LaOF复合纳米纤维与表征

采用静电纺丝技术,以硝酸镧、氟化铵、PVP和无水乙醇为原料,制备了LaF3/LaOF复合纳米纤维。用X射线衍射、扫描电镜等分析手段对制得的复合纳米纤维进行了表征。结果表明：所得产物为LaF3/LaOF复合纳米纤维,平均直径为150nm,长度〉50μm。对LaF3/LaOF复合纳米纤维的形成机理进行了讨论。     

多元醇还原法制备FePt纳米颗粒

以乙酰丙酮铁和氯铂酸作为Fe源和Pt源,1,2-十二烷二醇为还原剂,通过多元醇还原法制备出单分散的FePt纳米颗粒,研究了表面活性剂油酸和油胺对FePt纳米颗粒形貌和分散性的影响。结果显示,未使用表面活性剂制得的FePt纳米颗粒粒度范围是1.0～6.0 nm,平均粒径为3.4 nm;使用油酸和油胺制得的FePt纳米颗粒粒度范围是2.5～5.5 nm,平均粒径4.1 nm。通过XRD、TEM和VSM分析表明,油酸和油胺修饰的FePt纳米颗粒为面心立方结构,形状近似球形,分散性良好,粒径分布较未使用表面活性剂时变窄;VSM显示其矫顽力趋近于0,呈现超顺磁性。     

表面活性剂在FePt纳米颗粒形貌控制中的应用

采用湿化学还原法制备FePt纳米颗粒,选择复配型表面活性剂柠檬酸和聚乙二醇(PEG)、油酸和油胺,以及单一型表面活性剂十二烷基苯磺酸钠对FePt纳米颗粒进行修饰,比较了三者在FePt纳米颗粒形貌及磁性能上的作用区别。XRD、TEM以及振动样品磁强计表征结果显示,表面活性剂的选择对制备FePt纳米颗粒的结构没有影响,均显示化学无序的面心立方结构;复配型表面活性剂有利于诱导生成各向异性纳米结构,聚合物表面活性剂PEG诱导生成了棒状和米粒状纳米结构;室温下颗粒均显示超顺磁性,但饱和磁化强度M s差别很大,球形颗粒M s相对最大,而棒状颗粒M s相对较小。     

膜控制扩散制备纳米镧化合物及其摩擦学性能

通过石蜡膜控制沉淀离子扩散速率,采用尿素水解制备镧化合物,对其进行热重分析确定焙烧温度,运用XRD、TEM等表征手段对其进行表征,物相分析表明焙烧产物主要成分为La5O7NO3,粒径约为40 nm。合成两性表面活性剂对纳米镧化合物进行表面修饰,使其能稳定分散于液体石蜡基础油中。以液体石蜡为润滑油基础油,添加基础油质量0.5%的表面活性剂修饰后的纳米镧极压抗磨剂,结果表明,极压性提高33.33%、磨损性减小20%左右。     

制备表面修饰油酸的CeO2纳米粒子

以具有不饱和双键的油酸为表面活性剂,对水溶胶中的CeO2纳米粒子进行表面修饰.TEM分析表明,经表面修饰的CeO2纳米粒子基本呈球形,粒径约为3 nm,分布均匀,并且表面包覆油酸的CeO2纳米粒子易溶于弱极性溶剂,不易溶于极性溶剂.     

纳米Fe3O4/聚苯乙烯复合材料结构与性能

以化学共沉淀法制备Fe3O4纳米颗粒,以油酸为表面活性剂、苯乙烯为负载液制备可聚合磁流体,再经自由基聚合制备出了纳米Fe3O4/聚苯乙烯复合材料.TEM测试结果表明,表面处理的Fe3O4颗粒在聚苯乙烯基质中分散均匀,不发生团聚.DSC和TGA研究结果表明,虽然Fe3O4/聚苯乙烯均匀分散体系的玻璃化转变温度比聚苯乙烯的低,但少量Fe3O4纳米颗粒的存在使聚苯乙烯的起始、终止和最大热分解温度都有明显的提高.     

硬脂酸修饰纳米Fe_3O_4的制备及摩擦学性能的研究

通过微波水热法制备了表面修饰硬脂酸的纳米Fe3O4颗粒。运用红外光谱对其结构进行了分析,该添加剂具有较好的分散性与稳定性。经四球长磨实验表明,当表面修饰硬脂酸的纳米Fe3O4颗粒在液体石蜡油中的添加量为1.00%时,摩擦系数降至0.025,磨斑直径为0.47。     

油酸包覆的机油基Fe3 O4磁流体的制备及表征

首先利用化学共沉淀法制备了具有超顺磁性的纳米Fe3O4颗粒,然后用油酸对其进行包覆,得到稳定的Fe3O4机油基磁流体。分别用XRD、IR、TEM、VSM和TGA对所制备的产物进行表征,探讨了油酸包覆Fe3O4纳米颗粒的形成机理。研究表明,所得磁流体具有高的饱和磁化强度和稳定性,制备的纳米Fe3O4颗粒的饱和磁化强度为79.886emu/g,用油酸包覆后的颗粒的饱和磁化强度达到73.991emu/g,油酸的包覆使得Fe3O4颗粒的饱和磁化强度有所降低。     

纳米LaF3的介电性能

采用水溶液沉淀法制备了平均粒径17纳米的LaF3粉体,通过真空压结成形法制备了纳米LaF3块体,通过测量复阻抗谱研究了纳米LaF3块体材料的介电性能。     

Enhanced emission of ultra-small-sized LaF(3):RE(3+) (RE = Eu, Tb) nanoparticles through 1,2,4,5-benzenetetracarboxylic acid sensitization

Uniform, ultra-small-sized and well-water-dispersible LaF(3) nanoparticles doped with trivalent rare earth (RE) ions (Eu(3+) or Tb(3+)) have been synthesized by a simple, low temperature synthesis route. The nanoparticles, with sizes of about 3.2 nm (for those doped with Eu(3+)) and 3.0 nm (for those doped with Tb(3+)), are roughly spherical and monodisperse. 1,2,4,5-Benzenetetracarboxylic acid (labeled as BA) as sensitizer has been bonded to the surface of the nanoparticles, which can sensitize the emission of RE(3+) in the LaF(3) nanoparticles. The BA-LaF(3):RE(3+) (RE = Eu or Tb) nanoparticles have a broad absorption band in the UV domain, and show enhanced luminescence of RE(3+) based on an energy transfer from BA ligands to RE(3+) ions (i.e. the so-called "antenna effect"). Due to the dual protection of organic ligands (BA) and inorganic matrices (LaF(3)), BA-LaF(3):RE(3+) (RE = Eu or Tb) nanoparticles have longer excited state lifetimes than LaF(3):RE(3+) (RE = Eu or Tb) nanoparticles as well as lanthanide coordination polymers of BA.     

The unexpected structures of "core-shell" and "alloy" LnF3 nanoparticles as examined by variable energy X-ray photo-electron spectroscopy

Lanthanide fluoride nanoparticles were synthesized in aqueous media using procedures intended for a core-shell structure of Ln((1))F(3)-Ln((2))F(3), its reverse architecture, and an alloy structure. Their structures were examined by variable photon energy photo-electron spectroscopy using synchrotron radiation, along with X-ray powder diffractometry, transmission electron microscopy, energy dispersive X-ray spectroscopy, and luminescence spectroscopy. The results show that the nanoparticles intended for a core-shell structure do not have a core-shell structure, and that nanoparticles intended for an alloy structure do not always have an alloy structure. A possible explanation for this is cation exchange, a phenomenon that occurs when LnF(3) nanoparticles are exposed to another Ln(3+) ion in aqueous media, resulting in Ln(3+) ions in nanoparticles being quickly replaced by Ln(3+) ions in solution. This cation exchange effectively competes with the precipitation of LnF(3), which leads to a concentration gradient in the case of the combination of LaF(3) and GdF(3), and to nearly an alloy structure (isotropic mixture of all the ions) in the case of the combination of LaF(3) and NdF(3), regardless of the procedure used. Finally, the intended "core-shell" nanoparticles were doped with Eu(3+) to show that a non-core-shell structure can also give rise to the improvement of optical properties as compared with the corresponding core nanoparticles. These results suggest that conclusions in the literature that a core-shell structure was obtained as inferred by TEM or enhanced luminescence may not be correct.     

Plasmonic Effects of Infiltrated Silver Nanoparticles Inside TiO2 Film: Enhanced Photovoltaic Performance in DSSCs

The plasmonic effects of infiltrated silver (Ag) nanoparticles, with different contents, inside a nanostructured TiO₂ film on the photovoltaic performance of dye‐sensitized solar cells (DSSCs) are explored. The synthesized Ag nanoparticles are immobilized onto deposited TiO₂ nanoparticles by a new strategy using 3‐mercaptopropionic acid (MPA), a bifunctional linker molecule. Transmission electron microscope (TEM) images show that monodispersed Ag and polydispersed TiO₂ nanoparticles have an average diameter of 12 ± 3 nm and 5 ± 1 nm, respectively. Moreover, Fourier transform infrared spectroscopy (FTIR) analysis reveals that Ag nanoparticles were successfully functionalized and capped with MPA. Optical studies on the MPA‐capped Ag nanoparticles inside TiO₂ film show an increase in the total absorbance of the electrode. Moreover, EIS measurements confirm that MPA‐capped Ag nanoparticles inhibit the charge recombination and improve the stability of nanoparticles in I₃^?/I^? electrolyte. The DSSC assembled with optimal content of MPA‐capped Ag nanoparticles demonstrated an enhanced power conversion efficiency (8.82% ± 0.07%) compared with the pure TiO₂ (7.30% ± 0.05%). The increase in cell efficiency was attributed to the enhanced dye light absorption in strength and spectral range due to the surface plasmon resonance of MPA‐capped Ag nanoparticles in the photoanode.     

LaF3和YF3对偏高岭石基地聚物力学性能和结构的影响

地聚物由于其优异的力学和耐久性能,成为近年来国际上的研究热点.通过在高岭土中掺入不同量的LaF3和YF3合成地聚物,测试不同龄期地聚物的抗压强度,并对其力学性能进行评价,探究了LaF3和YF3对地聚物力学强度和结构的影响.采用X射线衍射(XRD)、扫描电镜(SEM)、能谱(EDS)红外光谱(FTIR)和核磁共振(MAS-NMR)对地聚物的物相和微观结构进行了分析.结果表明:LaF3和YF3的掺入导致地聚物的抗压强度明显下降,并随掺量增加抗压强度逐渐降低,且掺量相同时,掺入YF3的地聚物抗压强度的降幅更明显.红外光谱(FTIR)分析发现掺入LaF3和YF3的地聚物在950～1250cm-1的弯曲振动峰明显向高波速移动,说明地聚物中聚合Al-O-Si键数量减少,地聚物缩聚反应趋向不完全,27Al核磁共振(MAS-NMR)结果表明地聚物中Al配位数位没有发生变化.物相分析显示稀土氟化物经煅烧后转变成了稀土氟氧化物.通过扫描电镜(SEM)和能谱分析发现稀土氟氧化物在断面裂痕处发生偏聚现象,应力集中于两相晶界处,使其出现力学弱点,是导致掺入稀土氟化物的地聚物抗压强度明显下降的主要原因.     

表面修饰氧化亚铅纳米颗粒的制备及其抗磨性能研究

以硬脂酸铅为单源前驱体,成功制备出硬脂酸修饰的氧化亚铅纳米颗粒,用透射电子显微镜、X-射线粉末衍射仪、红外光谱仪等仪器对其进行了结构表征,并在四球摩擦试验机上测试了其抗磨性能。结果表明:所制备的Pb2O纳米颗粒大小均匀,表面修饰层与纳米颗粒表面之间发生化学键合作用,其作为润滑油添加剂具有良好的抗磨能力。     

磁流体制备中表面活性剂的选择及其包裹条件的影响

讨论了表面活性剂对磁性颗粒的包裹以及pH值、温度、表面活性剂的用量和搅拌速度等包裹条件对磁性颗粒的影响。应用磁天平、粒度测试仪对磁性颗粒的粒径和磁化率进行了测定。结果表明,在十二烷基苯磺酸钠、油酸钠和乙二醇3种不同的表面活性剂中,选用油酸钠效果最好。当pH=5,温度为80℃,搅拌速度为200 r/min,油酸钠的用量大约为Fe2+的0.4~0.5倍时,包裹效果最好,得到的磁性颗粒小、磁性强。     

Size controlled synthesis of well-distributed nano-silver on hydroxyapatite using alkanolamine compounds

A well-distributed nano-silver hydroxyapatite composite has been successfully prepared by a one-pot synthesis method. Hydroxyapatite was separately synthesized by a sol-gel method, then impregnated with silver nanoparticles with the mediation of Uncaria gambir Roxb. leaf extract in the presence of three kinds of alkanolamine compound; monoethanolamine (MEA), diethanolamine (DEA), and triethanolamine (TEA) as capping agents. The effect of different capping agents on the properties of the silver nanoparticles and the nano-silver hydroxyapatite composite were studied. UV–visible spectrophotometer analysis exhibited absorbance peaks at 402–439 nm which specifically corresponds to spherical silver nanoparticles. Higher optical absorbance was observed in TEA-capped silver nanoparticles, than in DEA and MEA-capped ones. X-ray diffraction (XRD) analysis showed a highly crystalline hexagonal structure for hydroxyapatite and no detected metallic silver. However, the presence of 1.65% silver was confirmed by energy dispersive x-ray (EDX) spectroscopy analysis. Transmission electron microscopy (TEM) analysis revealed spherical silver nanoparticles with a size range of 2–62 nm (smallest mean diameter of 2 nm) adhered to the hydroxyapatite surface. The TEA capped impregnated silver nanoparticles were the smallest, corresponding to the best capping performance, followed by those capped by DEA and MEA. Small-sized nanoparticles on hydroxyapatite are beneficial for highly antibacterial bone implants.     

Chitosan- and dehydroascorbic acid-coated Fe<Subscript>3</Subscript>O<Subscript>4</Subscript> nanoparticles: preparation,characterization and their potential as draw solute in forward osmosis process

Forward osmosis (FO) is a natural osmosis process that has attracted a significant attention due to its many advantages. However, the development of FO process depends on the development of proper draw solutions. In this work, chitosan (CS)-coated Fe₃O₄ nanoparticles and dehydroascorbic acid (DHAA)-coated Fe₃O₄ nanoparticles were successfully synthesized by co-precipitation method and their performance as draw solutes was investigated for application in FO systems. CS and DHAA could improve the surface hydrophilicity of the Fe₃O₄ nanoparticles. The synthesized nanoparticles were characterized by field emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM), X-ray diffractometry (XRD), Fourier transform infrared spectroscopy (FTIR) and vibrating sample magnetometry (VSM) which the results presented a small size, crystalline morphology and high magnetization value for their structure as well as a good dispersion in water. Cellulose triacetate/cellulose acetate (CTA/CA)-based membranes were also prepared by immersion precipitation and used as FO membranes. The synthesized FO membranes were characterized by FESEM. The performance evaluation of synthesized nanoparticles revealed that the water flux of Fe₃O₄ nanoparticles capped with DHAA was higher than that of the chitosan-coated Fe₃O₄ nanoparticles. At the end of the process, the Fe₃O₄ nanoparticles were easily separated from the diluted draw solution by applying the magnetic field.     

Evidence for high performances of low Pt loading electrodes based on capped platinum electrocatalyst and carbon nanotubes in fuel cell devices

Recently we reported the preparation and electrochemical behaviour of porous electrodes based on the controlled combination of carbon nanotubes and capped platinum nanoparticles towards oxygen reduction. Due to the organic crown of the nanoparticles, the electrodes exhibited low hydrogen underpotential deposition (H upd) electroactive surface areas but significant activity towards oxygen reduction was recorded down to very low platinum loadings of few μg/cm². While the presence of organic stabilizing material, at the surface of the electrocatalyst synthesized by wet chemistry, may be considered as a potential drawback in fuel cell community, we present in this paper results showing that our capped electrocatalyst associated with carbon nanotubes can be used without any pre-treatment and exhibit high performances in fuel cell devices, in spite of low platinum loadings. Beyond the practical interest of such capped nanoparticles in fuel cell technology demonstrated here, fundamental question related to the high performances of the capped electrocatalyst are still opened and are currently under investigation.