Fe3O4磁性纳米颗粒的合成及其调控

利用水解共沉淀法制备了Fe3O4纳米颗粒,研究了温度和pH值对Fe3O4纳米颗粒粒径、形貌的影响关系。研究结果表明,反应温度从30℃升高到90℃,Fe3O4颗粒的粒径从6～8nm增大到10～12nm;同时,Fe3O4颗粒的饱和磁矩也随着Fe3O4颗粒粒径的增加而升高。溶液pH值会影响Fe3O4纳米颗粒的形状,高pH值易使合成的Fe3O4纳米颗粒为四方形,随着pH值的降低,Fe3O4纳米颗粒向球形转变。Fe3O4纳米颗粒的粒径和形状的可控性为进一步合成、调控Fe3O4电磁功能复合材料奠定了良好基础。     

Synthesis and magnetic properties of Fe3O4 nanoparticles

Ferromagnetic Fe₃O₄ nanoparticles with diameter of ∼27 nm were prepared by a hydrothermal route in the presence of a surfactant, sodium bis(2-ethylhexyl)sulfosuccinate (AOT). The as-synthesized product was characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM) and high-resolution transmission electron microscopy (HRTEM). The hysteresis loops of the iron oxide nanoparticles were measured using a physical property measuring system (PPMS), and the results showed a superparamagnetic behavior at room temperature.     

纳米Fe3O4颗粒及磁性液体的制备

用低温相转化法制备了小粒径的Fe3O4纳米颗粒,用油酸对纳米颗粒进行了表面处理,溶液pH为6．90,80℃下恒温反应50～60min时磁性粉体颗粒的改性效果较好。然后将包覆颗粒分散到载液中制得磁性液体。实验中用XRD、TEM、VSM、IR光谱等对所制的样品进行了相应表征,并将UV光谱分析方法用于油酸包覆的定量评估,从而建立了磁性颗粒表面修饰的表征方法。     

单分散Fe3O4纳米粒子的合成、表征及其自组装

采用高温有机前驱体分解法,以Fe(acac)3为前驱体制备出单分散性较好的Fe3O4纳米粒子,粒径为(6.4±0.90)nm.利用TEM、XRD、HPPS、FTIR等手段对粒子的形貌及性质进行了研究,证实得到的是Fe3O4单晶,粒子表层的铁原子通过共价键和油酸分子中-COO的两个氧原子结合在一起.通过对自组装过程的初步研究表明随磁性纳米粒子浓度的增加,粒子排布逐渐由零星的无规排列变为规整的单层和多层有序结构.     

Fe3O4／羧甲基化壳聚糖纳米粒子的制备与表征

磁性壳聚糖纳米粒子可用于药物载体及废水处理吸附剂。以化学共沉淀法制备Fe3O4纳米粒子，壳聚糖先进行羧甲基化改性，再经碳二亚胺活化，包履在Fe3O4颗粒表面,透射电镜（TEM）表明，Fe3O4纳米粒子被CMC包履，粒径约10nm；X射线衍射（XRD）分析表明复合纳米粒子中磁性物质为Fe3O4；傅立叶红外光谱（FTIR）表明壳聚糖发生羧甲基反应；磁性测试表明，Fe3O4／CMC具有超顺磁性，饱和磁化强度25.73emu／g，且有良好的磁稳定性。     

化学还原法制备Fe3O4纳米颗粒及其性能研究

采用化学还原法制备得到了Fe3O4纳米颗粒,并用XRD对制备条件:分散剂种类、分散剂用量、煅烧温度、煅烧时间进行了研究。研究结果表明,当选用PEG(6000)做分散剂,PEG用量为50g/L,煅烧温度为700℃,煅烧时间为120min时,制备得到的Fe3O4纳米颗粒已经具有晶型完整的反尖晶石结构。将该样品做VSM分析,分析结果表明样品饱和磁化强度可达85A.m2/kg,并且矫顽力趋近于0,呈现出良好的顺磁性。     

Ni doped Fe3O4 magnetic nanoparticles

In this work, the effect of nickel doping on the structural and magnetic properties of Fe3O4 nanoparticles is analysed. Ni(x)Fe(3-x)O4 nanoparticles (x = 0, 0.04, 0.06 and 0.11) were obtained by chemical co-precipitation method, starting from a mixture of FeCl2 x 4H2O and Ni(AcO)2 x 4H2O salts. The analysis of the structure and composition of the synthesized nanoparticles confirms their nanometer size (main sizes around 10 nm) and the inclusion of the Ni atoms in the characteristic spinel structure of the magnetite Fe3O4 phase. In order to characterize in detail the structure of the samples, X-ray absorption (XANES) measurements were performed on the Ni and Fe K-edges. The results indicate the oxidation of the Ni atoms to the 2+ state and the location of the Ni2+ cations in the Fe2+ octahedral sites. With respect to the magnetic properties, the samples display the characteristic superparamagnetic behaviour, with anhysteretic magnetic response at room temperature. The estimated magnetic moment confirms the partial substitution of the Fe2+ cations by Ni2+ atoms in the octahedral sites of the spinel structure.     

Synthesis and characterization of Piperidine-4-carboxylic acid functionalized Fe3O4 nanoparticles as a magnetic catalyst for Knoevenagel reaction

Piperidine-4-carboxylic acid (PPCA) functionalized Fe₃O₄ nanoparticles as a novel organic–inorganic hybrid heterogeneous catalyst was fabricated and characterized by XRD, FT-IR, TGA, TEM and VSM techniques. Composition was determined as Fe₃O₄, while particles were observed to have spherical morphology. Size estimations using X-ray line profile fitting (10 nm), TEM (11 nm) and magnetization fitting (9 nm) agree well, revealing nearly single crystalline character of Fe₃O₄ nanoparticles. Magnetization measurements reveal that PPCA functionalized Fe₃O₄ NPs have superparamagnetic features, namely immeasurable coercivity and absence of saturation. Small coercivity is established at low temperatures. The catalytic activity of Fe₃O₄–PPCA was probed through one-pot synthesis of nitro alkenes through Knoevenagel reaction in CH₂Cl₂ at room temperature. The heterogeneous catalyst showed very high conversion rates (97%) and could be recovered easily and reused many times without significant loss of its catalytic activity.     

Green fabrication of agar-conjugated Fe3O4 magnetic nanoparticles

Magnetic nanoparticles are of great interest both for fundamental research and emerging applications. In the biomedical field, magnetite (Fe(3)O(4)) has shown promise as a hyperthermia-based tumor therapeutic. However, preparing suitable solubilized magnetite nanoparticles is challenging, primarily due to aggregation and poor biocompatibility. Thus methods for coating Fe(3)O(4) NPs with biocompatible stabilizers are required. We report a new method for preparing Fe(3)O(4) nanoparticles by co-precipitation within the pores of agar gel samples. Permeated agar gels were then dried and ground into a powder, yielding agar-conjugated Fe(3)O(4) nanoparticles. Samples were characterized using XRD, FTIR, TGA, TEM and SQUID. This method for preparing agar-coated Fe(3)O(4) nanoparticles is environmentally friendly, inexpensive and scalable.     

共沉淀制备不同粒径Fe3O4纳米颗粒及磁性能的研究

以氯化铁(FeCl3·6H2O)和氯化亚铁(FeCl2·4H2O)为原料,氢氧化钠(NaOH)为沉淀剂,在无表面活性剂作用下共沉淀制备出了不同粒径的Fe3O4纳米颗粒.采用X射线衍射(XRD)、透射电子显微镜(TEM)和振动样品磁强计(VSM)对产物的晶体结构、形貌、粒径及磁性能进行了表征.实验结果表明,n(Fe2+)...     

Synthesis of size-controlled Fe3O4@SiO2 magnetic nanoparticles for nucleic acid analysis

We present a systematic study on the preparation, characteration and potential application of Fe3O4 and Fe3O4@SiO2 nanoparticles. Fe3O4 nanoparticles of controllable diameters were successfully synthesized by solvothermal system with tuning pH. The magnetic properties of nanoparticles were measured by vibration sample magnetometer. Fe3O4@ SiO2 nanoparticles were obtained via classic St?ber process. Streptavidin coated Fe3O4@SiO2 nanoparticles were prepared by covalent interaction. The quantity of streptavidin bound to nanoparticles was determined by UV-Vis spectrometer. To evaluate the binding efficiency and capacity of nucleic acid on nanoparticles, the capture of biotinylated oligonucleotide on streptavidin coated Fe3O4@SiO2 nanoparticles at different concentration was estimated by fluorescence detection. Both Fe3O4 and Fe3O4@SiO2 nanoparticles exhibited well crystallization and magnetic properties. The maximal amount of streptavidin immobilized onto the Fe3O4@SiO2 nanoparticles was 29.3 microg/mg. The saturation ratio of biotinylated oligonucleotides captured on streptavidin coated Fe3O4@SiO2 nanoparticles was 5 microM/mg within 20 minutes, indicating that FeO4@SiO2 nanoparticles immobilized by streptavidin were excellent carriers in nucleic acid analysis due to their convenient magnetic-separation property. Therefore, the synthesized Fe3O4 and Fe3O4@SiO2 nanoparticles with controllable size and high magnetic saturation have shown great application potentials in nucleic acid research.     

氧化硅-磁性Fe3O4复合纳米粒子的制备及应用

采用溶胶-凝胶法通过正硅酸四乙酯（TEOS）碱催化水解,在Fe₃O₄纳米粒子表面包裹氧化硅。利用生物倒置显微镜、场发射透射电镜、X射线衍射仪、激光粒度仪、振动样品磁强计对氧化硅/Fe₃O₄复合粒子的外貌、粒径及粒径分布、饱和磁化强度、化学成分进行了表征。结果表明,所制得的复合粒子性能良好,粒径在15 nm左右,饱和磁化强度为109 emu/g。用该磁性纳米复合粒子提取质粒DNA和基因组DNA取得良好的效果,可用于食品中致病菌的分析判定和疾病的基因诊断分析。     

Preparation,characterization and application of Fe3O4/ZnO core/shell magnetic nanoparticles

Fe₃O₄ magnetic nanoparticles (MNPs) were synthesized by a co-precipitation method. The phase purity was confirmed by X-ray powder diffraction (XRD) analysis. The crystal size was found to be 10 nm from transmission electron microscopy (TEM). It is evidenced that the surface of Fe₃O₄ MNPs was modified by sodium citrate. The Fe₃O₄/ZnO core/shell MNPs were obtained by coating the MNPs with direct precipitation using zinc acetate and ammonium carbonate. The precursor was firstly dried and then calcined at 350 °C. The antioxidation tests indicated that the core/shell MNPs give better antioxidation than that of the Fe₃O₄ MNPs. The photocatalytic degradation of methyl orange revealed that the core/shell MNPs have higher photocatalytic activity than that of the ZnO nanoparticles. Separation of the core/shell MNPs from the aqueous suspension using a magnet provides an easy way to recycle the core/shell MNPs. After four-time recycling, the photocatalytic degradation percentage of the core/shell MNPs is about 70%.     

Synthesis and characterization of SiO2/(PMMA/Fe3O4) magnetic nanocomposites

Magnetic silica nanocomposites (magnetic nanoparticles core coated by silica shell) have the wide promising applications in the biomedical field and usually been prepared based on the famous St?ber process. However, the flocculation of Fe3O4 nanoparticles easily occurs during the silica coating, which limits the amount of magnetic silica particles produced in the St?ber process. In this paper, PMMA/Fe3O4 nanoparticles were used in the St?ber process instead of the "nude" Fe3O4 nanoparticles. And coating Fe3O4 with PMMA polymer beforehand can prevent magnetic nanoparticles from the aggregation that usually comes from the increasing of ionic strength during the hydrolyzation of tetraethoxysilane (TEOS) by the steric hindrance. The results show that the critical concentration of magnetic nanoparticles can increase from 12 mg/L for "nude" Fe3O4 nanoparticles to 3 g/L for PMMA/Fe3O4 nanoparticles during the St?ber process. And before the deposition of silica shell, the surface of PMMA/FeO4 nanoparticles had to be further modified by hydrolyzing them in CH3OH/NH3 x H2O mixture solution, which provides the carboxyl groups on their surface to react further with the silanol groups of silicic acid.     

Fe3O4/石墨烯复合材料的制备及表征

采用液相还原的方法,在碱性环境下使用FeCl2.4H2O和氧化石墨作为前驱体,制备Fe3O4微球附载的石墨烯复合材料。通过调节氧化石墨和铁盐的质量比制备得到不同组分的Fe3O4/石墨烯复合粉体。使用场发射电子扫描显微镜(FESEM)、X射线衍射仪(XRD)、振动样品磁强计(VSM)和四探针电阻仪等仪器分析了产物的形貌、物相、磁性能和导电性能。结果表明Fe3O4/石墨烯复合粉体中Fe3O4微球在石墨烯表面分散均匀,且Fe3O4结晶良好,为立方晶系的尖晶石型。该复合粉体具有高的磁性能和良好的导电性能,饱和磁化强度和电导率分别达到72emu/g和0.53S/cm。     

Size and surface effects on magnetic properties of Fe3O4 nanoparticles

In this study, size and surface effects on temperature and frequency dependent magnetic properties of superparamagnetic Fe3O4 nanoparticles in a size range of 1.1-11 nm are investigated by SPR technique. We used a theoretical formalism based on a distribution of diameters or volumes of the nanoparticles following lognormal proposed by Berger et al. The nanoparticles are considered as single magnetic domains with random orientations of magnetic moments and thermal fluctuations of anisotropic axes. The individual line shape function is derived from the damped precession equation of Landau-Lifshitz. Magnetic properties of the samples were strongly temperature and size dependent. The increase in SPR line width, the decrease in the resonance field and also increase in anisotropy filed by decreasing the temperature core-shell type structure of the nanoparticles and disordered magnetic structure (spin-glass like phase) of the particle surface. A linear microwave frequency dependence of the resonance field and the increase in the blocking temperature of the particles by the particle size were also observed.     

Synthesis,characterization and microwave absorption properties of Fe3O4/Co core/shell-type nanoparticles

Co coated Fe₃O₄ core/shell-type nanoparticles were fabricated by hydrothermal technique and electroless plating process. X-ray powder diffraction (XRD), X-ray fluorescence spectrometer (XRF) and transmission electron microscope (TEM) were employed to investigate the crystal structure, element composition and morphology of the prepared nanoparticles. Vibrating sample magnetometer (VSM) and vector network analyzer were used to measure the magnetic properties and electromagnetic parameters of pure Fe₃O₄ and Fe₃O₄/Co core/shell-type nanoparticles, then reflection losses (RL(dB)) were calculated in the frequency range of 2–18 GHz. Magnetic studies revealed typical ferromagnetic behavior for the pure Fe₃O₄ and Fe₃O₄/Co core/shell-type nanoparticles with their saturation magnetization (M_s = 63.1 and 72.4 emu/g) and coercivity (H_c = 99.5, and 165.4 Oe), respectively. Due to the existence of the core/shell structure, the electromagnetic characteristic of the Fe₃O₄/Co nanoparticles exhibit better microwave absorption performance than the pure Fe₃O₄ in the range of 2–18 GHz, such as more powerful absorbing property and wider frequency band of microwave absorption.     

O-羧甲基化壳聚糖修饰磁性Fe3O4纳米粒子及其生物应用

采用共沉淀法制备Fe3O4纳米粒子,用XRD测定粒子成分,用透射电镜和显微镜观测粒子形貌,用震动样品磁场计测定Fe3O4粉末饱和磁化强度,再以O-羧甲基化壳聚糖修饰后,用红外光谱检测粒子成分.粒子性能良好,能很好的应用于生物分离,连接等.     

Synthesis and conductivity studies of piperidine-4-carboxylic acid functionalized Fe3O4 nanoparticles

Piperidine-4-carboxylic acid (PPCA) functionalized Fe₃O₄ nanoparticles as a novel organic–inorganic hybrid was fabricated and characterized by XRD, FT-IR, VSM, and TEM techniques. Its detailed electrical properties are also presented. Composition was determined as Fe₃O₄, while particles were observed to have spherical morphology. VSM measurement proved the super-paramagnetic property of the as synthesized nanocomposite. ac and dc conductivity measurements indicated semiconductor characteristics and changing trends with temperature because of reorganization of the nanocomposite. dc conductivity is strongly temperature dependent and is classified into three regions. Analysis of the real and imaginary parts of the permittivity of nanocomposite showed the ionic polarization mechanism consisting of ionic conductivity and interfacial polarization.