柑橘皮提取液绿色合成纳米Fe3O4及其吸附水中孔雀石绿的性能研究

以柑橘皮提取液为还原剂和稳定剂,绿色合成Fe3O4纳米材料,利用扫描电子显微镜(SEM)、X射线衍射图谱(XRD)、傅立叶变换红外光谱(FT-IR)等手段对材料进行表征,并考察了其对孔雀石绿(MG)的吸附性能。结果表明:绿色合成纳米Fe3O4呈不规则圆球体,分散性和结晶度较好。在投加量为1.0 g/L、初始pH为4、温度为25℃、初始浓度为20 mg/L时,对孔雀石绿的吸附率达到95.33%。纳米Fe3O4对MG的吸附过程分别符合准二级动力学方程和Langmuir等温方程。热力学研究表明,纳米Fe3O4吸附MG是自发吸热过程。绿色合成纳米Fe3O4重复利用4次吸附率仍在70%以上。

Folate-conjugated Fe_3O_4 nanoparticles for in vivo tumor labeling

Highly biocompatible superparamagnetic Fe3O4 nanoparticles were synthesized by amide of folic acid （FA） ligands and the NH2-group onto the surface of Fe3O4 nanoparticles. The as-synthesized folate-conjugated Fe3O4 nanoparticles were characterized by X-ray diffraction diffractometer, transmission electron microscope, FT-IR spectrometer, vibrating sample magnetometer, and dynamic light scattering instrument. The in vivo labeling effect of folate-conjugated Fe3O4 nanoparticles on the hepatoma cells was investigated in tumor-bearing rat. The results demonstrate that the as-prepared nanoparticles have cubic structure of Fe3O4 with a particle size of about 8 nm and hydrated diameter of 25.7 nm at a saturation magnetization of 51 A·m2/kg. These nanoparticles possess good physiological stability, low cytotoxicity on human skin fibroblasts and negligible effect on Wistar rats at the concentration as high as 3 mg/kg body mass. The folate-conjugated Fe3O4 nanoparticles could be effectively mediated into the human hepatoma Bel 7402 cells through the binding of folate and folic acid receptor, enhancing the signal contrast of tumor tissue and surrounding normal tissue in MRI imaging. It is in favor of the tumor cells labeling, tracing, magnetic resonance imaging （MRI） target detection and magnetic hyperthermia.

Preparation and Analysis of Fe3O4 Magnetic Nanoparticles Used as Targeted-drug Carriers

Fe3O4 magnetic nanoparticles were prepared by the aqueous co-precipitation of FeCl3-6H2O and FeCl2-4H2O with addition of ammonium hydroxide. The conditions for the preparation of Fe3O4 magnetic nanoparticles were optimized, and Fe3O4 magnetic nanoparticles obtained were characterized systematically by means of transmission electron microscope （TEM）, dynamic laser scattering analyzer （DLS） and X-ray diffraction （XRD）. The results revealed that the magnetic nanoparticles were cubic shaped and dispersive, with narrow size distribution and average diameter of 11.4 nm. It was found that the homogeneous variation of pH value in the solution via the control on the dropping rate of aqueous ammonia played a critical role in size distribution. The magnetic response of the product in the magnetic field was also analyzed and evaluated carefully. A 32.6 mT magnetic field which is produced by four ferromagnets was found to be sufficient to excite the dipole moments of 0.05 g Fe3O4 powder 2 cm far away from the ferromagnets. In conclusion, the Fe3O4 magnetic nanoparticles with excellent properties were competent for the magnetic carders of targeted-drug in future application.

Size-dependent peroxidase-like catalytic activity of Fe_3O_4 nanoparticles

Peroxidase-like catalytic properties of Fe3O4 nanoparficles （NPs） with three different sizes, synthesized by chemical coprecipitation and sol-gel methods, were investigated by UV-vis spectrum analysis. By comparing Fe3O4 NPs with average diameters of 11, 20, and 150 nm, we found that the catalytic activity increases with the reduced nanoparticle size. The electrochemical method to characterize the catalytic activity of Fe3O4 NPs using the response currents of the reaction product and substrate was also developed.

Surface organic modification of Fe_3O_4 nanoparticles by silane-coupling agents

Fe3O4 nanoparticles were prepared by chemistry co-precipitation and the mean crystal size was 17.9 nm measured by XRD. After it had been treated by silane-coupling agents KH570, magnetic micro-spheres dispersed in organic medium glycol were gained and the mean size of Fe3O4 nanopowders was 33.7 nm. So it can be concluded that magnetic micro-sphere is made of a few Fe3O4 crystals. Many factors of modification were researched, such as the time of ball milling, the content of Fe3O4 and the content of KH570. The modification of Fe3O4 is relative to the time of ball milling, but the dominant function is affected by the content of Fe3O4 and KH570. When the content of Fe3O4 is known, there is a suitable content of KH570. Different content of Fe3O4 will make the different suitable content of KH570, but the range of latter is less than former, which is relative to the distribution of KH570 on Fe3O4 surface or in the solution.

Fabrication of Poly（y-glutamic acid）-coated Fe3O4 Magnetic Nanoparticles and Their Application in Heavy Metal Removal

In this study, poly（y-glutamic acid）-coated Fe3O4 magnetic nanoparticles （y-PGA/Fe304 MNPs） were successfully fabricated using the co-precipitation method. Fe3O4 MNPs were also prepared for comparison. The av erage size and specific surface area results reveal that 7-PGA/Fe304 MNPs （52.4 nm, 88.41 m2.g-1） have smaller particle size and larger specific surface area_ than Fe3O4 MNPs （62.0 nm, 76.83 mLg-1）. The y-PGA/Fe3O4 MNPs

Surface Organic Modification of Fe_3O_4 Magnetic Nanoparticles

The surface organic modification of Fe3O4 nanoparticles with silane coupling reagent KH570 was studied. The modified and unmodified nanoparticles were characterized by FT-IR, XPS and TEM. The spectra of FT-IR and XPS revealed that KH570 was coated onto the surface of Fe3O4 nanoparticles to get Fe-O- Si bond and an organic coating layer also was formed. Fe3O4 nanoparticles were spheres partly with mean size of 18,8 nm studied by TEM, which was consistent with the result 17.9 nm calculated by Scherrer＇s equation. KH570 was adsorbed on surface and formed chemistry bond to be steric hindrance repulsion which prevented nanoparticles from reuniting. Then glycol-based Fe3O4 magnetic liquids dispersed stably was gained.

Fe3O4 nanoparticles impregnated eggshell as a novel catalyst for enhanced biodiesel production

Biodiesel is a green fuel which can replace diesel while addressing various issues such as scarcity of hydrocarbon fuels and environmental pollution to an extent. The high production cost of biodiesel and the recovery of the catalyst after the transesterification process are the major challenges to be addressed in biodiesel production. In the present work, a cheap and promising solid base oxide catalyst was synthesized from chicken eggshell by calcination at 900 ℃ forming catalyst eggshells(CES) and was impregnated with the nanomagnetic material(Fe3O4) to obtain Fe3O4 loaded catalytic eggshell(CES–Fe3O4). Fe3O4 nanomaterials were synthesized by co-precipitation method and were loaded in catalytic eggshell by sonication, for better recovery of the catalyst after transesterification process. CES–Fe3O4 material was characterized by Thermogravimetric analysis, X-ray diffraction, Fourier transform infrared spectroscopy, a vibrating-sample magnetometer, Brunauer-Emmett-Teller, Dynamic light scattering, and Scanning electron microscopy. Biodiesel was synthesized by transesterification of Pongamia pinnata raw oil with 1:12 oil to methanol molar ratio and 2 wt% catalyst loading for 2 h at a temperature of 65 ℃ and yields were compared. The reusability of the catalyst was studied by the transesterification of the raw oil and its catalytic activity was found to be retained up to 7 cycles with a yield of 98%.

Intensification of levofloxacin sono-degradation in a US/H_2O_2 system with Fe_3O_4 magnetic nanoparticles

Fe3O4 magnetic nanoparticles(MNPs) were synthesised, characterised, and used as a peroxidase mimetic to accelerate levofloxacin sono-degradation in an ultrasound(US)/H2O2 system. The Fe3O4 MNPs were in nanometre scale with an average diameter of approximately 12 to 18 nm. The introduction of Fe3O4 MNPs increased levofloxacin sono-degradation in the US/H2O2 system. Experimental parameters, such as Fe3O4 MNP dose, initial solution p H, and H2O2 concentration, were investigated by a one-factor-at-a-time approach. The results showed that Fe3O4 MNPs enhanced levofloxacin removal in the p H range from 4.0 to 9.0. Levofloxacin removal ratio increased with Fe3O4 MNP dose up to 1.0 g·L-1and with H2O2 concentration until reaching the maximum. Moreover, three main intermediate compounds were identified by HPLC with electrospray ionisation tandem mass spectrometry, and a possible degradation pathway was proposed. This study suggests that combination of H2O2, Fe3O4 MNPs and US is a good way to improve the degradation efficiency of antibiotics.

Loading Fe3O4 nanoparticles on paper-derived carbon scaffold toward advanced lithium-sulfur batteries

Lithium-sulfur batteries(LSBs) are regarded as a competitive next-generation energy storage device.However, their practical performance is seriously restricted due to the undesired polysulfides shuttling.Herein, a multifunctional interlayer composed of paper-derived carbon(PC) scaffold, Fe3O4 nanoparticles,graphene, and graphite sheets is designed for applications in LSBs. The porous PC skeleton formed by the interweaving long-fibers not only facilitates fast transfer of Li ions and electrons but also provides a physical barrier for the polysulfide shuttling. The secondary Fe3O4@graphene component can reduce the polarization, boost the attachment of polysulfides, and promote the charging-discharging kinetics. The outer graphitic sheets layers benefit the interfacial electrochemistry and the utilization of S-containing species.The efficient obstruction of polysulfides diffusion is further witnessed via in situ ultraviolet-visible characterization and first-principles simulations. When 73% sulfur/commercial acetylene black is used as the cathode, the cell exhibits excellent capacity retention with high capacities at 0.5 C for 1000 cycles and even up to 10 C for 500 cycles, an ultrahigh rate capability up to 10 C(478 m Ah g-1), and a high arealsulfur loading of 8.05 mg cm-2. The strategy paves the way for developing multifunctional composites for LSBs with superior performance.

Characteristics of magnetic Fe_3O_4 nanoparticles encapsulated with human serum albumin

Magnetic nanoparticles （Fe304） were prepared by chemical precipitation method using Fe^2＋ and Fe^3＋ salts with sodium hydroxide in the nitrogen atmosphere. Fe3O4 nanoparticles were coated with human serum albumin（HSA） for magnetic resonance imaging as contrast agent. Characteristics of magnetic particles coated or uncoated were carried out using scanning electron microscopy and X-ray diffraction. Zeta potentials, package effects and distributions of colloid particles were measured to confirm the attachment of HSA on magnetic particles. Effects of Fe3O4 nanoparticles coated with HSA on magnetic resonance imaging were investigated with rats. The experimental results show that the adsorption of HSA on magnetic particles is very favorable to dispersing of magnetic Fe3O4 particles, while the sizes of Fe3O4 particles coated are related to the molar ratio of Fe3O4 to HSA. The diameters of the majority of particles coated are less than 100 nm. Fe3O4 nanoparticle coated with HSA has a good biocompatibility and low toxicity. This new contrast agent has some effects on the nuclear magnetic resonance imaging of liver and the lowest dosage is 20μmol/kg for the demands of diagnosis.

Modification of Fe_3O_4 Magnetic Nanoparticles by L-dopa or Dopamine as an Enzyme Support

Fe3O4 magnetic nanoparticles were prepared by co-precipitation of Fe^2＋ and Fe^3＋ in an ammonia solution, and its size was about 36 nm measured by an atomic force microscope. Fe3O4 magnetic nanoparticles were modified by L-dopa or dopamine using sonication method. The analysis of FTIR clearly indicated the formation of Fe-O-C bond. Direct immobilization of trypsin （EC： 3.4.21.4） on Fe3O4 magnetic nanoparticles with L-dopa and dopamine spacer was investigated using glutaraldehyde as a coupling agent. No significant changes in the size and magnetic property of the three kinds of magnetic nanoparticles linked with or without trypsin were observed. The existence of the spacer molecule on magnetic nanoparticles could greatly improve the activity and the storage stability of bound trypsin through increasing the flexibility of enzyme and changing the microenvironment on nanoparticles surface compared to the naked magnetic nanoparticles.

Fe_3O_4 Magnetic Nanoparticles Modified Electrode as a Sensor for Determination of Nimesulide

A novel type of Fe3O4 nanoparticles modified glass carbon electrode（Fe3O4/GCE） was constructed and the electrochemical properties of N-（4-nitro-2-phenoxyphenyl）methanesulfonamide（nimesulide） were studied on the Fe3O4/GCE.In 0.4mol/L HAc-NaAc buffer solution（pH=5.0）,the electrode process of nimesulide was irreversible at bare GCE and Fe3O4/GCE.The Fe3O4/GCE exhibited a remarkable catalytic and enhancement effect on the reduction of nimesulide.The reduction peak potential of nimesulide shifted positively from-0.683 V at bare GCE to-0.625 V at Fe3O4/GCE,and the sensitivity was increased by ca.3 times.Some experimental conditions were optimized.The linear range between the peak current and the concentration of nimesulide was 2.6×10-6 ＂1.0×10-4mol/L（R=0.993） with a detection limit of 1.3×10-7mol/L.This method has been used to determine the content of nimesulide in medical tablets.The recovery was determined to be 96.9% ＂101.9% by means of standard addition method.The method is comparable to UV-Vis spectrometry.

Synthesis and Characterization of Superparamagnetic Fe₃O₄@SiO₂Core-Shell Composite Nanoparticles

The Fe3O4@SiO2 composite nanoparticles were obtained from as-synthesized magnetite (Fe3O4) nanoparticles through the modified St?ber method. Then, the Fe3O4 nanoparticles and Fe3O4@SiO2 composite nanoparticles were characterized by means of X-ray diffraction (XRD), Raman spectra, scanning electron microscope (SEM) and vibrating sample magnetometer (VSM). Recently, the studies focus on how to improve the dispersion of composite particle and achieve good magnetic performance. Hence effects of the volume ratio of tetraethyl orthosilicate (TEOS) and magnetite colloid on the structural, morphological and magnetic properties of the composite nanoparticles were systematically investi-gated. The results revealed that the Fe3O4@SiO2 had better thermal stability and dispersion than the magnetite nanoparticles. Furthermore, the particle size and magnetic property of the Fe3O4@SiO2 composite nanoparticles can be adjusted by changing the volume ratio of TEOS and magnetite colloid.

PREPARATION AND MAGNETORHEOLOGICAL PROPERTIES OF AQUEOUS SUSPENSION BASED ON EMULSION DROPLETS CONTAINING Fe_3O_4 NANOPARTICLES

The Fe3O4 nanoparticles with mean size of 10 nm were prepared by chemical common precipitation . The factors influencing the size and shape of Fe3O4 nanoparticles such as the adding rate of NaOII to the mixed solution and the final pH of the solution were studied . The Fe3O4 based magnetorheological(MR) fluid was formed by adding surfactant . The rheological properties of this MR fluid were studied when the magnetic fields with different direction are applied. It has been found that the MR fluid has the magnetic anisotropy.

Static magnetic field-assisted synthesis of Fe3O4 nanoparticles and their adsorption of Mn(Ⅱ) in aqueous solution

A facile method for synthesis of the magnetic Fe_3O_4 nanoparticles was introduced.Magnetic nanoparticles were prepared via co-precipitation method with(PMF) and without(AMF) 0.15 T static magnetic field.The effects of magnetic field on the properties of magnetic nanoparticles were studied by XRD,TEM,SEM,VSM and BET.The results showed that the magnetic field in the co-precipitation reaction process did not result in the phase change of the Fe_3O_4 nanoparticles but improved the crystallinity.The morphology of Fe_3O_4 nanoparticles was varied from random spherical particles to rod-like cluster structure.The VSM results indicated that the saturation magnetization value of the Fe_3O_4 nanoparticles was significantly improved by the magnetic field.The BET of Fe_3O_4nanoparticles prepared with the magnetic field was larger than the control by 23.5%.The batch adsorption experiments of Mn(Ⅱ) on the PMF and AMF Fe_3O_4 nanoparticles showed that the Mn(II) equilibrium capacity was increased with the pH value increased.At pH 8,the Mn(Ⅱ) adsorption capacity for the PMF and AMF Fe_3O_4 was reached at 36.81 and 28.36 mg·g^(-1),respectively.The pseudo-second-order model fitted better the kinetic models and the Freundlich model fitted isotherm model well for both PMF and AMF Fe_3O_4.The results suggested that magnetic nanoparticles prepared by the magnetic field presented a fairly good potential as an adsorbent for an efficient removal of Mn(Ⅱ) from aqueous solution.

Synthesis and Characterization of Biomimetic Fe3O4/Coke Magnetic Nanoparticles Composite Material

A composite material（Fe3O4/Coke）using coke supported Fe3O4 magnetic nanoparticles was successfully prepared via an in-situ chemicaloxidation precipitation method and characterized by SEM,XRD,Raman,and FTIR.The results showed that the Fe3O4 nanoparticles existed steadily on the surface of coke,with better dispersing and smaller particle size.The catalytic ability of Fe3O4/Coke were investigatied by degrading p-nitrophenol（P-NP）.The results showed that the apparent rate constant for the P-NP at 1.0 g·L^-1 catalyst,30 mmol·L^-1 H2O2,pH=3.0,30 ℃ and the best ratio of Coke/Fe3O4 0.6,was evaluated to be 0.027 min^-1,the removalrate of CODCr was 75.47%,and the dissolubility of Fe was 2.42 mg·L^-1.Compared with pure Fe3O4,the catalytic ability of Fe3O4/Coke in the presence of H2O2 was greatly enhanced.And Fe3O4/Coke was a green and environmentalcatalyst with high catalytic activity,showing a good chemicalstability and reusability.

Magnetic field aligned orderly arrangement of Fe3O4 nanoparticles in CS/PVA/Fe3O4 membranes

The CS/PVA/Fe_3O_4 nanocomposite membranes with chainlike arrangement of Fe_3O_4 nanoparticles are prepared by a magnetic-field-assisted solution casting method. The aim of this work is to investigate the relationship between the microstructure of the magnetic anisotropic CS/PVA/Fe_3O_4 membrane and the evolved macroscopic physicochemical property. With the same doping content, the relative crystallinity of CS/PVA/Fe_3O_4-M is lower than that of CS/PVA/Fe_3O_4.The Fourier transform infrared spectroscopy（FT-TR） measurements indicate that there is no chemical bonding between polymer molecule and Fe_3O_4 nanoparticle. The Fe_3O_4 nanoparticles in CS/PVA/Fe_3O_4 and CS/PVA/Fe_3O_4-M are wrapped by the chains of CS/PVA, which is also confirmed by scanning electron microscopy（SEM） and x-ray diffraction（XRD）analysis. The saturation magnetization value of CS/PVA/Fe_3O_4-M obviously increases compared with that of non-magnetic aligned membrane, meanwhile the transmittance decreases in the UV-visible region. The o-Ps lifetime distribution provides information about the free-volume nanoholes present in the amorphous region. It is suggested that the microstructure of CS/PVA/Fe_3O_4 membrane can be modified in its curing process under a magnetic field, which could affect the magnetic properties and the transmittance of nanocomposite membrane. In brief, a full understanding of the relationship between the microstructure and the macroscopic property of CS/PVA/Fe_3O_4 nanocomposite plays a vital role in exploring and designing the novel multifunctional materials.

Controllable Synthesis and Magnetic Properties of Monodisperse Fe_3O_4 Nanoparticles

Magnetite （Fe3O4） nanoparticles with different sizes and shapes are synthesized by the thermal decomposition method. Two approaches, non-injection one-pot and hot-injection methods, are designed to investigate the growth mechanism in detail. It is found that the size and shape of nanoparticles are determined by adjusting the precursor concentration and duration time, which can be well explained by the mechanism based on the LaMer model in our synthetic system. The monodisperse Fe3O4 nanoparticles have a mean diameter from 5nm to 16nm, and shape evolution from spherical to triangular and cubic. The magnetic properties are size-dependent, and Fe3O4 nanoparticles in small size about 5 nm exhibit superparamagnetie properties at room temperature and maximum saturation magnetization approaches to 78 emu/g, whereas Fe3O4 nanoparticles develop ferromagnetic properties when the diameter increases to about 16nm.

Field-variable magnetic domain characterization of individual 10 nm Fe3O4 nanoparticles

The local detection of magnetic domains of isolated 10 nm Fe3O4 magnetic nanoparticles(MNPs) has been achieved by field-variable magnetic force microscopy(MFM) with high spatial resolution.The domain configuration of an individual MNP shows a typical dipolar response.The magnetization reversal of MNP domains is governed by a coherent rotation mechanism, which is consistent with the theoretical results given by micromagnetic calculations.Present results suggest that the field-variable MFM has great potential in providing nanoscale magnetic information on magnetic nanostructures,such as nanoparticles, nanodots, skyrmions, and vortices, with high spatial resolution.This is crucial for the development and application of magnetic nanostructures and devices.