磁性纳米钌催化剂的制备及对聚苯乙烯催化加氢的催化性能

通过化学共沉淀法制备了Fe3O4,利用硅酸钠水解、缩合制备了具有核壳结构SiO2/Fe3O4复合纳米粒子。利用红外光谱(FT-IR)、扫描电镜(SEM)、X射线衍射(XRD)以及振动样品磁强计(VSM)技术对其进行了表征。将所得的磁性纳米SiO2/Fe3O4用有机硅改性的聚乙烯吡咯烷酮进行表面修饰,利用原位还原RuCl3的方法将金属Ru负载到磁性载体上,制备了磁性纳米催化剂Ru/PVP/SiO2/Fe3O4。探讨了所得催化剂对聚苯乙烯氢化反应的催化性能,考察了反应压力、温度、时间以及溶剂等对催化性能的影响。结果表明,随着反应温度的升高、压力的增加,催化活性提高;当反应温度为393K、氢气压力为8 MPa、反应时间为5 h时,聚苯乙烯氢化度可以达到90%以上。     

Magnetic Fe3O4@chitosan nanoparticle: synthesis, characterization and application as catalyst carrier

A novel method was developed to prepare Fe3O4@CS beads with core-shell structure using a double-crosslinking process. Before the coating process, an unique crosslinking agent, glutaraldehyde (GA), was adsorbed onto the surface of Fe3O4 in advance, so the subsequent CS can uniformly coat around the magnetic core processed from the strong interaction between GA and CS, forming a perfect core-shell structure. The obtained Fe3O4@CS beads were followed by the Pd deposition through in-situ reduction method, and the prepared composite catalyst was applied exemplarily in synthesizing nabumetone to check its reusing property. The nanoparticles were characterized by transmission electron microscopy (TEM), X-ray powder diffraction (XRD), Fourier transformation infrared spectroscopy (FTIR), X-ray photoelectron spectroscopy (XPS), and the magnetic hysteresis loop determination method. This novel composite catalyst showed admirable potential in reusable catalysis.     

Synthesis of magnetic nanocomposites and alloys from platinum-iron oxide core-shell nanoparticles

This paper presents a systematic study on the generation of iron platinum-containing magnetic nanocomposites and alloys from Pt@Fe(2)O(3) core-shell nanoparticle precursors. These core-shell nanoparticles were made using a sequential synthetic approach. They could form FePt alloys and alloy-containing nanocomposites through a solid-state reaction at >400?°C. The chemical compositions of FePt alloys were controllable by using Pt@Fe(2)O(3) core-shell nanoparticles that had the designed Pt core diameter and iron oxide shell thickness. We show that face-centred tetragonal (fct) FePt@Fe core-shell nanoparticles could be made from Pt@Fe(2)O(3) core-shell nanoparticles with?5% hydrogen in argon (v/v). Furthermore, various FePt alloys and alloy-containing nanocomposites including metastable intermediate phases could be obtained. The materials were characterized by high resolution scanning transmission electron microscopy (HR-STEM), energy dispersive x-ray (EDX) spectroscopy, powder x-ray diffraction (PXRD), parallel electron energy loss spectroscopy (PEELS), and superconducting quantum interference device (SQUID) magnetometry. These materials could have potential applications as permanent hard magnets and data storage media.     

聚乙二醇法在温和条件下制备不同结构的磁性Fe3O4纳米晶

以Fe（acac）3为原料,乙二醇、聚乙二醇1000和聚乙二醇5000为还原剂和溶剂,在温和的溶剂热的条件下制备了不同尺寸的顺磁性Fe3O4纳米颗粒.利用X射线衍射（XRD）、光电子能谱（XPS）、透射电子显微镜（TEM）和磁性测量技术对制备的Fe3O4纳米颗粒的结构、形貌、磁性能进行了表征测试.结果发现,聚乙二醇分子链的长度对Fe3O4纳米颗粒的平均粒径大小、结晶度和饱和磁化强度均有重要影响.以乙二醇、聚乙二醇1000和聚乙二醇5000为还原剂制备的Fe3O4纳米颗粒的尺寸分别为2～3nm、5nm和7～8nm;相应的纳米Fe3O4颗粒饱和磁化强度分别为55.2、61.5和81.3emu/g;同时结晶度也随分子链的增加而增加.随分子链长度的增加,还原剂还原性的逐渐增加是导致Fe3O4纳米颗粒平均粒径大小、结晶度和饱和磁化强度逐渐增大的重要因素.     

Non-aqueous synthesis of water-dispersible Fe3O4-Ca3(PO4)2 core-shell nanoparticles

The Fe(3)O(4)-Ca(3)(PO(4))(2) core-shell nanoparticles were prepared by one-pot non-aqueous nanoemulsion with the assistance of a biocompatible triblock copolymer, poly(ethylene glycol)-block-poly(propylene glycol)-block-poly(ethylene glycol) (PEO-PPO-PEO), integrating the magnetic properties of Fe(3)O(4) and the bioactive functions of Ca(3)(PO(4))(2) into single entities. The Fe(3)O(4) nanoparticles were pre-formed first by thermal reduction of Fe(acac)(3) and then the Ca(3)(PO(4))(2) layer was coated by simultaneous deposition of Ca(2+) and PO(4)(3-). The characterization shows that the combination of the two materials into a core-shell nanostructure retains the magnetic properties and the Ca(3)(PO(4))(2) shell forms an hcp phase (a = 7.490 ?, c = 9.534 ?) on the Fe(3)O(4) surface. The magnetic hysteresis curves of the nanoparticles were further elucidated by the Langevin equation, giving an estimation of the effective magnetic dimension of the nanoparticles and reflecting the enhanced susceptibility response as a result of the surface covering. Fourier transform infrared (FTIR) analysis provides the characteristic vibrations of Ca(3)(PO(4))(2) and the presence of the polymer surfactant on the nanoparticle surface. Moreover, the nanoparticles could be directly transferred to water and the aqueous dispersion-collection process of the nanoparticles was demonstrated for application readiness of such core-shell nanostructures in an aqueous medium. Thus, the construction of Fe(3)O(4) and Ca(3)(PO(4))(2) in the core-shell nanostructure has conspicuously led to enhanced performance and multi-functionalities, offering various possible applications of the nanoparticles.     

Synthesis of Fe3O4@PbS hybrid nanoparticles through the combination of surface-initiated atom transfer radical polymerization and acidolysis by H2S

A versatile approach to fabricate nanoparticles with multiple functionalities through the combined use of both surface-initiated ATRP and acidolysis by H2S techniques was demonstrated. The hybrid nanoparticles exhibited the core-shell structure having the magnetite nanoparticles as the core and the polymethacrylate as the shell with PbS nanoparticles distributing in the shell. The structure and morphology of the synthesized nanoparticles were characterized using Fourier transform infrared spectroscopy (FTIR), X-ray photoelectron spectroscopy (XPS), X-ray diffraction (XRD) and transmission electron microscopy (TEM). The optical and magnetic properties of the nanoparticles were investigated by UV-Vis spectroscopy, photoluminescence spectroscopy and vibrating sample magnetometer (VSM), respectively. It is observed that the absorption and emission behaviors of the Fe3O4@PbS hybrid nanoparticles were seriously influenced by the ATRP time and the reaction time with H2S. The saturated magnetization (Ms) decreased with the increase of ATRP time due to the formation of thicker shells coating on the surfaces of magnetite nanoparticles.     

Poly(n-isopropylacrylamide)-based hydrogel coatings on magnetite nanoparticles via atom transfer radical polymerization

Core magnetite (Fe(3)O(4)) nanoparticles have been functionalized with a model intelligent hydrogel system based on the temperature responsive polymer poly(n-isopropyl acrylamide) (PNIPAAm) to obtain magnetically responsive core-shell nanocomposites. Fe(3)O(4) nanoparticles were obtained from a one-pot co-precipitation method which provided either oleic acid (hydrophobic) or citric acid (hydrophilic) coated nanoparticles. Subsequent ligand exchange of these coatings with various bromine alkyl halides and a bromo silane provided initiating sites for functionalization with NIPAAm using atom transfer radical polymerization (ATRP). The bromine alkyl halides that were used were 2-bromo-2-methyl propionic acid (BMPA) and 2-bromopropionyl bromide (BPB). The bromo silane that was used was 3-bromopropyl trimethoxysilane (BPTS). The intelligent polymeric shell consists of NIPAAm crosslinked with poly(ethylene glycol) 400 dimethacrylate (PEG400DMA). Fourier transform infrared (FTIR) spectroscopy, thermogravimetric analysis (TGA), and transmission electron microscopy (TEM) were used to confirm the presence of the polymeric shell. Dynamic light scattering (DLS) was used to characterize the nanocomposites for particle size changes with temperature. Their magnetic and temperature responsiveness show great promise for further biomedical applications. This platform for functionalizing magnetic nanoparticles with intelligent hydrogels promises to impact a wide range of medical and biological applications of magnetic nanoparticles.     

Au/Fe3O4磁性纳米粒子的合成及表征

报道了一种合成具有巯基官能团修饰的Au/Fe_3O_4磁性纳米粒子的新方法。采用共沉淀法制备Fe_3O_4磁性纳米颗粒,并在此基础上用聚(烯丙胺)溶液还原HAuCl4,制得Au/Fe_3O_4磁性核壳纳米颗粒,再用3-巯基-1-丙磺酸钠修饰Au/Fe_3O_4磁性纳米粒子,最后得到具有巯基官能团稳定的Au/Fe_3O_4磁性纳米粒子。通过扫描电子显微镜(SEM)、透射电子显微镜(TEM)、X射线能谱仪(EDS)、X射线衍射仪(XRD)、X射线光电子能谱(XPS)、振动样品磁强计(VSM)分别对产物的微观结构及磁性特征进行表征。     

单相Bi0.95Eu0.05Fe0.95Co0.05O3纳米颗粒的结构及其铁磁特性

采用溶胶-凝胶法制备了单相Bi0.95 Eu0.05Fe0.95 Co0.05 O3纳米粉末。用X射线衍射仪(XRD)和扫描电子显微镜(SEM)测量分析了其结构和形貌,结果表明样品仍为钙钛矿菱方结构。样品Fe2p的X射线吸收谱(XAS)表明样品中Fe的价态处于Fe2+和Fe3+的混合态。利用振动样品磁强计(VSM)测量样品的磁性特征,结果表明样品具有完整闭合的磁滞回线,表现出室温的铁磁性,相比BiFeO3样品磁性得到明显增强。     

微波辐射乳液聚合制备聚氰基丙烯酸正丁酯磁性微球

通过化学共沉淀法制备Fe3O4纳米粒子,再用油酸钠和十二烷基磺酸钠(SDS)对Fe3O4进行改性,制得稳定的水基磁流体。在自制的磁流体存在下,以氰基丙烯酸正丁酯(BCA)为单体,用微波辐射乳液聚合的方法制备了Fe3O4/聚氰基丙烯酸正丁酯磁性微球。并用X射线衍射仪(XRD),透射电子显微镜(TEM),傅立叶红外光谱仪(FT-IR),振动样品磁强计(VSM)对制备的磁性高分子微球的结构形貌和磁性能进行表征测试。结果表明,在适当的pH值条件下,得到了粒径为150 nm~200 nm,饱和磁化强度为20.23 emμ/g,粒径均一的聚氰基丙烯酸正丁酯磁性微球。     

磁性核壳Fe3O4/P(GMA-DVB)-SH-Au复合催化剂的制备及催化性能

首先通过水热法合成了单分散空心Fe3O4磁球,之后利用蒸馏沉淀聚合将P(GMA-DVB)聚合物层包覆在Fe3O4磁球表面形成Fe3O4/P(GMA-DVB)核壳结构,巯基化处理后吸附Au纳米粒子,得到磁性核壳Fe3O4/P(GMA-DVB)-SH-Au复合催化剂。利用TEM,SEM,FTIR,XRD,TGA,VSM及UV-vis对其进行表征,并考察该催化剂在催化还原4-硝基苯酚反应中的催化性能。结果表明合成的材料粒径均匀,球形度规整,核壳结构明显,在催化反应中,Fe3O4/P(GMA-DVB)-SH-Au表现出优异的催化性能,而且经过连续8次循环使用后,催化效率仍可保持80%以上。     

Fe@Ag core-shell nanoparticles with both sensitive plasmonic properties and tunable magnetism

Monodisperse Fe@Ag core-shell nanoparticles with relatively uniform Fe cores and Ag shells have been successfully fabricated by a seed mediated method in a two-step reducing process, and then characterized by electron microscopy techniques (HRTEM, EDX), X-ray diffraction (XRD), UV-vis spectroscopy,and magnetometry. The results demonstrate unique optical and magnetic properties for Fe@Ag core-shell nanoparticles. The surface plasmon resonance of Fe@Ag core-shell nanoparticles is red shifted as compared with that of pure colloidal nano-silver, while the plasmon band of Fe@Ag core-shell nanoparticles with thinner Ag shells is shifted to a longer wavelength. Fe@Ag core-shell nanoparticles have a narrow plasmon band and therefore sensitive plasmonic properties. The magnetism of Fe@Ag nanoparticles can be tuned from superparamagnetic to ferromagnetic by modifying the proportion between Fe and Ag contents. The multifunctional Fe@Ag core-shell nanoparticles have potential in optoelectronic, spintronic, and biomedicine applications.     

The grafting and release behavior of doxorubincin from Fe(3)O(4)@SiO(2) core-shell structure nanoparticles via an acid cleaving amide bond: the potential for magnetic targeting drug delivery

Fe(3)O(4)@SiO(2) core-shell structure nanoparticles were first prepared and characterized by TEM, FTIR, XPS and XRD. Subsequently the widely used anticancer agent doxorubincin (DOX) was successfully grafted to the surface of the core-shell nanoparticles via an amide bond with the aid of a spacer arm we synthesized. The spacer arm met two needs: one end can couple to the core-shell nanoparticles' surface while the other end was the active?-COOH group, which can react with the?-NH(2) group of DOX molecules. The synthesized spacer arm and the conjugation of the drug with nanoparticles through amidation were confirmed by FTIR. The DOX-loading efficiency determined by UV-vis spectrometer was 86.5%. Drug release experiments displayed a pH-dependent behavior that DOX was cleaved from the nanoparticles easily under low pH conditions in the presence of protease and that most of the conjugated doxorubincin were released within the first 12?h. The prepared DOX-grafted Fe(3)O(4)@SiO(2) core-shell structure nanoparticles showed a superparamagnetic property with a saturation magnetization value of 49.3?emu?g(-1), indicating a great potential application in the treatment of cancer using magnetic targeting drug-delivery technology.     

磁性羧甲基化壳聚糖纳米粒子的制备与表征

以化学共沉淀法制备了Fe3O4纳米粒子,壳聚糖经羧甲基化改性后接枝在Fe3O4颗粒表面,得到了磁性羧甲基化壳聚糖(Fe3O4/CMC)纳米粒子.利用透射电镜(TEM)、X射线衍射(XRD)、傅立叶红外光谱(FT-IR)及磁性测试对产物进行了表征.TEM表明Fe3O4纳米粒子被CMC包覆,粒径约10 nm;XRD分析表明复合纳米粒子中磁性物质为Fe3O4;FT-IR表明壳聚糖发生羧甲基反应以及在Fe3O4表面的接枝反应.Fe3O4/CMC纳米粒子具有超顺磁性,比饱和磁化强度25.73 emu/g,有良好的磁稳定性.     

Fe3O4／Ag复合纳米材料的制备及SERS研究

采用乙酰丙酮铁作为有机前驱体盐,在二苄基醚溶液中,以油酸、油胺为表面活性剂,十六醇作为“分解促进剂”,分解前驱体乙酰丙酮铁,制备四氧化三铁纳米颗粒。以四氧化三铁纳米颗粒为“种子”,加入醋酸银,以油胺为还原剂,制备Fe3O4/Ag复合磁性纳米材料。利用透射电子显微镜对纳米材料的形貌进行了表征,通过紫外～可见吸收光谱和拉曼光谱仪对纳米材料的表面增强拉曼散射光谱进行表研究,采用铷硼磁铁对磁性纳米材料的磁性进行初步研究。实验结果表明：FelO2／Ag复合磁性纳米颗粒既具有磁性又具有贵金属光谱特性;相对Fe304而言,Fe3O4/Ag复合纳米粒子具有更好的s隙S增强效果。     

静电纺丝法制备PAN/Fe3O4磁性纳米纤维

采用化学共沉淀法制备纳米四氧化三铁,选用曲拉通X-100为分散剂,利用静电纺丝法制备PAN/Fe3O4磁性纳米复合材料。X射线衍射仪(XRD)验证了四氧化三铁在复合纳米纤维中的存在。同时使用扫描电镜(SEM)和透射电镜(TEM)对复合纳米纤维的微观形貌和Fe3O4在纤维中的分布进行了观察,利用热重(TGA)对纳米复合材料的热稳定性进行分析;通过磁性实验分析了纳米复合材料的磁性性能。结果表明,所制备PAN/Fe3O4磁性纳米纤维成型良好,且Fe3O4磁性颗粒在纤维中分散均匀,其与PAN是物理复合。纳米复合材料具有一定磁性,并可由磁性颗粒的加入量进行控制。     

Synthesis of SiO2-coated ZnMnFe2O4 nanospheres with improved magnetic properties

A core-shell structured composite, SiO2 coated ZnMnFe2O4 spinel ferrite nanoparticles (average diameter of approximately 80 nm), was prepared by hydrolysis of tetraethyl orthosilicate (TEOS) in the presence of ZnMnFe2O4 nanoparticles (average diameter of approximately 10 nm) synthesized by a hydrothermal method. The obtained samples were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), and field emission scanning electron microscopy (FESEM). The magnetic measurements were carried out on a vibrating sample magnetometer (VSM), and the measurement results indicate that the core-shell samples possess better magnetic properties at room temperature, compared with paramagnetic colloids with a magnetic core by a coprecipitation method. These core-shell nanospherical particles with self-assembly under additional magnetic fields could have potential application in biomedical systems.     

Preparation and characterization of Ni-nitrilotriacetic acid bearing poly(methacrylic acid) coated superparamagnetic magnetite nanoparticles

Stable superparamagnetic magnetite (Fe3O4) nanoparticles were synthesized via co-precipitation in the presence of poly(methacrylic acid) (PMAA) in aqueous solution. The polymer coated Fe3O4 nanoparticles were characterized using transmission electron microscopy (TEM), Fourier transform infrared spectroscopy (FTIR), X-ray diffraction, thermal analysis, and vibrating sample magnetometry (VSM) techniques. These measurements reveal the presence of magnetite nanoparticles with a size of approximately 8 nm inside the PMAA matrix. The magnetization value of these superparamagnetic nanoparticles at room temperarure and 7 T was measured as about 40 emu/g. PMAA-coated Fe3O4 nanoparticles were further assembled with Ni-chelate through a reaction between a primary amine-bearing NTA (nitrilotriacetic acid) ligand and carboxy-functional groups of PMAA. NTA-PMAA-coated magnetite nanoparticles were then loaded with nickel ions and characterized using FTIR. The average amount of binded Ni on the surface of the NTA-modified PMAA coated Fe3O4 was calculated as 1.65 +/- 0.3 x 10(-6) mol nickel(II) ions per g of the magnetic particles from the inductively coupled plasma optical emission spectroscopy (ICP-OES) measurements.     

Synthesis of alpha-Fe nanoparticles by solventless thermal decomposition

A new preparation for highly crystalline and monodisperse Fe3O4 nanoparticle is reported. This synthesis requires the use of rather complicated procedures including delicate control of surfactants ratios and inert reaction conditions due to the toxic and unstable nature of the precursors none the less because thermal decomposition methods were tried to synthesize monodispersed inorganic nanocrystallites until very recently. The synthesis of Fe3O4 nanocrystallites by using Fe(+2)-oleate2 complex was studied. The Fe(+2)-oleate2 complex was prepared from the reaction of iron chloride and sodium oleate in water. The thermal decomposition of the complex at the reduced pressure (0.3 torr) and about 300 degrees was done without any solvent. We demonstrated that a new solventless synthesis of size- and shape-monodisperse Fe3O4 nanoparticles depends on the amount of Na-oleate. And it is possible to remove the oleate ligand using reduction process. We confirmed that the nanoparticles changed from Fe3O4 to alpha-Fe phase obtained higher magnetic properties and crystallites by a vibrating sample magnetometer (VSM) and x-ray powder diffraction (XRD). Removal of the organic surfactant and other volatile components surrounding Fe3O4 nanoparticles was detected by fourier transform infrared spectroscopy (FT-IR).     

Preparation of SiO2/(PMMA/Fe3O4) nanoparticles using linolenic acid as crosslink agent for nucleic acid detection using chemiluminescent method

Usually, magnetic nanoparticles (MNPs) are prepared based on the famous St?ber process in which divinylbenzene (DVA) is often used as a crosslink agent to synthesize SiO2/(PMMA/Fe3O4) nanoparticles. Compared with DVA, linolenic acid (LNA) is innoxious and can polymerize more easily for it has three unsaturated double bonds. In this paper, LNA was used as a new crosslink agent instead of DVA to synthesize the SiO2/(PMMA/Fe3O4) nanoparticles. The results showed that the core-shell structure could be observed obviously. The sizes of nanoparticles with core-shell structure range from 200 to 500 nm. The DNA probes which was immobilized on the surface of MNPs were used to capture the biotin modified complementary sequence of the probe, and the formed complexes were bonded with streptavidin-modified alkaline phosphatase (SA-AP). Finally the chemiluminescent signals were detected by adding 3-(2'-spiroadamantane)-4-methoxy-4-(3"-phosphoryloxy) phenyl-1, 2-dioxetane (AMPPD) which was the substrate reagent of AP. The specificity and sensitivity of this approach were investigated in this paper.