Synthesis and characterization of Fe3O4 magnetic nanoparticles and their heating effects under radiofrequency capacitive field

Fe₃O₄ magnetic nanoparticles with diameters varying from 10 to 426 nm were synthesized and characterized. Heating effects of Fe₃O₄ magnetic nanoparticles under radiofrequency capacitive field (RCF) with frequency of 27.12 MHz and power of 60–150 W were investigated. When the power of RCF is lower than 90 W, temperatures of Fe₃O₄ magnetic nanoparticles (75–150 mg/mL) can be raised and maximal temperatures are all lower than 50 °C. When the power of RCF is 90–150 W, temperatures of Fe₃O₄ magnetic nanoparticles can be quickly raised and are all obviously higher than those of normal saline and distilled water under the same conditions. Temperature of Fe₃O₄ magnetic nanoparticles can even reach 70.2 °C under 150 W RCF. Heating effects of Fe₃O₄ magnetic nanoparticles are related to RCF power, particle size and particle concentration.     

Modification of Fe<Subscript>3</Subscript>O<Subscript>4</Subscript> 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.     

Self-cleaning glass coated with Fe^3＋ -TiO2 thin film

The self-cleaning glass coated with Fe^3 -TiO2 photocatalytic thin film was prepared by sol-gel process from the system Ti(OC4H9),-NH(C2H4OH)2-C2H5OH-H2O containing FeCl3. The microstructure and properties of the film were studied using differential thermal analysis-thermogravimetry(DTA-TG), X-ray diffration (XRD) and scanning electron microscope(SEM). The transmittance of the self-cleaning glass was measured by using UV-Vis spectrometer. The effects of content of Fe^3 and the thickness of Fe^3 -TiO2 thin film on the photocatalytic ac-tivity were examined. The results show that the photocatalytic thin films are mainly composed of Fe3O4 and TiO2 particles within 10-100 nm. The appropriate amount of Fe^3 is effective for improving the photocatalytic activities of TiO2. The best photocatalytic activity is obtained when the molar ratio of Fe^3 to TiO2 is 0. 005 and the glass is coated with 9 layers.     

Surface organic modification of Fe<Subscript>3</Subscript>O<Subscript>4</Subscript> 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.     

Synthesis and characterization of biomimetic Fe<Subscript>3</Subscript>O<Subscript>4</Subscript>/coke magnetic nanoparticles composite material

A composite material (Fe₃O₄/Coke) using coke supported Fe₃O₄ magnetic nanoparticles was successfully prepared via an in-situ chemical oxidation 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 °C and the best ratio of Coke/Fe₃O₄ 0.6, was evaluated to be 0.027 min^–1, the removal rate of COD_Cr 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 environmental catalyst with high catalytic activity, showing a good chemical stability and reusability.     

Preparation of LiFePO4 for lithium ion battery using Fe2P2O7 as precursor

In order to obtain a new precursor for LiFePO4, Fe2P2O7 with high purity was prepared through solid phase reaction at 650 ℃ using starting materials of FeC2O4 and NH4H2PO4 in an argon atmosphere. Using the as-prepared Fe2P2O7, Li2CO3 and glucose as raw materials, pure LiFePO4 and LiFePO4/C composite materials were respectively synthesized by solid state reaction at 700 ℃ in an argon atmosphere. X-ray diffractometry and scanning electron microscopy（SEM） were employed to characterize the as-prepared Fe2P2O7, LiFePO4 and LiFePO4/C. The as-prepared Fe2P2O7 crystallizes in the Cl space group and belongs to β-Fe2P2O7 for crystal phase. The particle size distribution of Fe2P2O7 observed by SEM is 0.4-3.0 μm. During the Li^＋ ion chemical intercalation, radical P2O7^4- is disrupted into two PO4^3- ions in the presence of O^2-, thus providing a feasible technique to dispose this poor dissolvable pyrophosphate. LiFePO4/C composite exhibits initial charge and discharge capacities of 154 and 132 mA·h/g, respectively.     

Electrodeposition of Ni-Co-Fe2O3 composite coatings

Ni-Co-Fe₂O₃ composite coatings were electrodeposited using cetyltrimethylammonium bromide (CTAB)-modified Watt’s nickel bath with Fe₂O₃ particles dispersed in it. The effects of the plating parameters on the chemical composition, structural and morphological characteristics of the electrodeposited Ni-Co-Fe₂O₃ composite coatings were investigated by energy dispersive X-ray (EDS) spectroscopy, X-ray diffractometry (XRD) and scanning electron microscopy (SEM). The results reveal that Fe₂O₃ particles can be codeposited in the Ni-Co matrix. The codeposition of Fe₂O₃ particles with Ni-Co is favoured at high Fe₂O₃ particle concentration and medium stirring, and the deposition of Co is favoured at high concentration of CTAB. Moreover, the study of the textural perfection of the deposits reveals that the presence of particles leads to the worsening of the quality of the observed 〈220〉 preferred orientation. Composites with high concentration of embedded particles exhibit a preferred crystal orientation of 〈111〉. The more the embedded Fe₂O₃ particles in the metallic matrix, the smaller the sizes of the crystallite for the composite deposits.     

一种基于 MXene 的Fe2O3/Nb2O5/Nb4C3Tx 高灵敏丙酮传感器

MXene 具有较大比表面积和优异的导电性, 当与金属氧化物半导体结合时可以抑制片层团聚, 还可以大大提高载流子转移速率, 提高气敏性能。通过简单的水热和煅烧两步法成功合成了Fe₂O₃/Nb₂O₅/Nb₄C₃T_x 三元复合材料。通过表征, Fe₂O₃ 微米球分布在 MXene 纳米片层之间。气敏测试结果表明, 与原始Fe₂O₃相 比, Fe₂O₃/Nb₂O₅/Nb₄C₃T_x 传感器对丙酮的响应能力有明显的提高。传感器灵敏度高, 选择性较好, 对环境中 浓度为 5 ×10^?6 的丙酮响应高 (R_a /R_g = 7.81, 30% RH), 响应和恢复速度快, 具有出色的重复性和长期稳定性。Fe₂O₃/Nb₂O₅/Nb₄C₃T_x 传感器具有良好的气敏性能, 主要因为三元复合材料提供了较大比表面积和丰富的氧空位, 增强了活性位点, 使得气体易于在传感器表面扩散, 为开发丙酮敏感复合材料提供了参考。     

Fe<Subscript>3</Subscript>O<Subscript>4</Subscript>@PAM@NTA-Ni<Superscript>2+</Superscript> Magnetic Composite Nanoparticles for Highly Specific Separation of His-tagged Proteins

A facile approach has been developed to synthesize Fe₃O₄@PAM (polyacrylamide) nanoparticles (NPs) with carboxyl groups on the surfaces by copolymerization with acrylamide and acrylic acid in Fe₃O₄ NPs aqueous suspension. Nitrilotriacetic acid (NTA) was conjugated to the magnetic NPs via well-known carboniimide chemistry using EDC and NHS. The Ni²⁺ ions loaded on the surface of NPs provide abundant docking sites for immobilization of His-tagged green fluorescent proteins (His-tagged GFP). The high magnetic property of Fe₃O₄@PAM@NTA-Ni²⁺ allows an easy separation of the NPs from solution under an external magnetic field, with high His-tagged protein binding capacity (42 μg protein/mg of NPs). The NPs can be recycled for at least four times without significant loss of binding capacity to proteins. These materials show great potential to separate His-tagged protein with low-cost purification at industrial scale.     

Modification of LiCo1/3Ni1/3Mn1/3O2 cathode material by CeO2-coating

LiCo_1/3Ni_1/3Mn_1/3O₂ was coated by a layer of 1.0 wt% CeO₂ via sol-gel method. The bared and coated LiMn_1/3Co_1/3Ni_1/3O₂ was characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), cyclic voltammogram (CV) and galvanotactic charge-discharge test. The results show that the coating layer has no effect on the crystal structure, only coating on the surface; the 1.0 wt% CeO₂-coated LiCo_1/3Ni_1/3Mn_1/3O₂ exhibits better discharge capacity and cycling performance than the bared LiCo_1/3Ni_1/3Mn_1/3O₂. The discharge capacity of 1.0 wt% CeO₂-coated cathode is 182.5 mAh·g⁻¹ at a current density of 20 mA·g⁻¹, in contrast to 165.8 mAh·g⁻¹of the bared sample. The discharge capacity retention of 1.0 wt% CeO₂-coated sample after 12 cycles reaches 93.2%, in comparison with 86.6% of the bared sample. CV results show that the CeO₂ coating could suppress phase transitions and prevent the surface of cathode material from direct contact with the electrolyte, thus enhance the electrochemical performance of the coated material.     

Luminescent properties of BaO-La2O3-B2O3 glasses with dopant

The luminescent properties of glasses synthesized in air atmosphere by conventional high temperature process were stud{ed. The emissions spectra of Eu^2 and Eu^3 were observed in BaO-La2O3-B2O3-Eu2O3 glasses.The results show that the broad emission peaks at 430 nm correspond to 5d→4f emission transition of Eu^2 , the sharp emission peaks at 592, 616, 650 and 250 nm correspond to 5^D0→1Fj(j=1--4) emission transition of Eu^3 ,respectively, which indicates that the BaO-La2O3a-B2O3-Eu2O3 glass can convert ultraviolet and green omponents of sunlight into blue and red light so as to increase the intensity of blue and red light, respectively. The luminescent in--tensity of Eu^2 increases with increasing the molar ratio of Tb^3 in BaO-La2O3-B2O3-Eu2O3a-Tb4O3 glasses, whereas the luminescent intensity of Eua^3 decreases. So the luminescent intensity of Eu(Ⅲ,Ⅱ) is influenced by Tb^3 .These phenomena can be explained by electron transfer mechanism; Eu^3 (4f6) Tb^3 (4f^8)→Eu^2 (4f′) Tb^4 (4f′). Taking advantage of the luminescent properties of BaO-La2O3-B2O3-Eu2O3 glasses, light-conversion glass for agriculture can be produced.     

Synthesis of γ-Al2O3 nanoparticles by chemical precipitation method

Highly pure active γ-Al₂O₃ nanoparticles were synthesized from aluminum nitrate and ammonium carbonate with a little surfactant by chemical precipitation method. The factors affecting the synthesis process were studied. The properties of γ-Al₂O₃ nanoparticles were characterized by DTA, XRD, BET, TEM, laser granularity analysis and impurity content analysis. The results show that the amorphous precursor Al(OH)₃ sols are produced by using 0.1 mol/L Al(NO₃)₃ · 9H₂O and 0.16 mol/L (NH₄)₂CO₃ · H₂O reaction solutions, according to the volume ratio 1.33, adding 0.024% (volume fraction) surfactant PEG600, and reacting at 40 °C, 1 000 r/min stirring rate for 15 min. Then, after stabilizing for 24 h, the precursors were extracted and filtrated by vacuum, washed thoroughly with deionized water and dehydrated ethanol, dried in vacuum at 80°C for 8 h, final calcined at 800 °C for 1 h in the air, and high purity active γ-Al₂O₃ nanoparticles can be prepared with cubic in crystal system, O _H ⁷ -FD3M in space group, about 9 nm in crystal grain size, about 20 nm in particle size and uniform size distribution, 131. 35 m²/g in BET specific surface area, 7 – 11 nm in pore diameter, and not lower than 99.93% in purity. Foundation item: Project(03JJY3015) supported by the Natural Science Foundation of Hunan Province     

Gap-plasmon of Fe<Subscript>3</Subscript>O<Subscript>4</Subscript>@Ag core-shell nanostructures for highly enhanced fluorescence detection of Rhodamine B

A novel gap-plasmon of Fe₃O₄@Ag core-shell nanoparticles for surface enhanced fluorescence detection of Rhodamine B (RB) was developed. Fe₃O₄@Ag core-shell nanostructures with Ag shell and Fe₃O₄ core were synthetized by self-assembled method with the assistance of 3-mercaptopropyl trimethoxy silane (MPTS). To study the RB fluorescence enhanced by gap-plasmon, the fluorescence properties of RB on the substrates with different nanogap densities were systematically investigated, and the results showed that the fluorescence intensity of RB on Fe₃O₄@Ag core-shell NPs substrate was much stronger than that on bare glass substrate, and the fluorescence intensity was further improved by using multilayer Fe₃O₄@Ag core-shell NPs substrate which had higher nanogap density. Different from the mechanism that is based on the maximum overlap of the surface plasmon resonance (SPR) band and emission band, the mechanism of the fluorescence enhancement in our work is based on the localized surface plasmon (LSP) and the gap plasmon near-field coupling with the Fe₃O₄@Ag core-shell NPs. Besides, the detection limit obtained was as low as 1×10^-7 mol/L, and the Fe₃O₄@Ag core-shell NPs substrate had high selectivity for RB fluorophores. It was demonstrated that the Fe₃O₄@Ag core-shell NPs substrate had activity, good stability, and selectivity for fluorescence detection of RB. And the detection of RB by the surface plasmon enhanced fluorescence was more convenient and rapid than the traditional detection methods in previous works.     

Preparation, characterization and photocatalytic behavior of WO3-TiO2/Nb2O5 catalysts

TiO2/Nb2O5 photocatalyst loaded with WO3 (WO3-TiO2/Nb2O5) was prepared by a modified hydrolysis process, and characterized by X-ray diffractometry, transmission electron microscopy, Raman spectra and UV-Vis diffuse refraction spectroscopy. The photocatalytic activity of WO3-TiO2/Nb2O5 was investigated by employing splitting of water for O2 evolution. The results indicate that WO3 loading can pronouncedly improve the photocatalytic activity of TiO2/Nb2O5 by using Fe3 as an electron acceptor under UV irradiation. The optimum molar fraction of the loaded WO3 is 2%, and the largest speed of O2 evolution for 2% WO3-TiO2/Nb2O5 catalyst is 151.8 μmol/(L·h).     

Kinetics of Fe3O4 formation by air oxidation

The kinetics of Fe₃O₄ formation by air oxidation of slightly acidic suspension of Fe(OH)₂ was studied. The effects of initial concentration of Fe(II), temperature, partial pressure of oxygen, air flow rate and stirring rate on the oxidation rate were investigated. The results show that Fe₃O₄ formation is composed of two-step reaction, the first step is the formation of Fe(OH) ₂ ⁺ by oxidation of Fe(OH)⁺ complex ions, the second step is the formation of magnetite by dehydration and deprotonation of Fe(OH)⁺ and Fe(OH) ₂ ⁺ . The oxidation reaction is zero-order with respect to the concentration of Fe(II) and around 0.5-order with respect to partial pressure of oxygen, and oxygen transfer process is rate-limiting step of oxidation reaction with apparent activation energy of 2.74 kJ · mol⁻¹.     

Magnetically Recoverable PEI/Titanate@Fe<Subscript>3</Subscript>O<Subscript>4</Subscript> Photocatalysts: Fabrication and Photocatalytic Properties

The magnetically separable ternary polyetherimide/titanate@Fe₃O₄ (PTF) photocatalysts of special heterostructure between magnetite (Fe₃O₄) microspheres and titanates nanosheets modified by polyetherimide (PEI) were successfully fabricated via a simple facile hydrothermal deposition method. The as-prepared photocatalysts were characterized by Fourier transform infrared spectroscopy, X-ray diffraction, Transmission electron microscopy and UV-vis diffuse reflectance spectroscopy etc. The results showed that the as-fabricated material had a structure of Fe₃O₄ microspheres coated with titanates nanosheets modified by PEI. The special interfacial contact between 3D microsphere and 2D nanosheets in the nanoarchitectures was formed via electrostatic attraction. Furthermore, the resulted photocatalysts were tested by degradation reaction of methylene blue under visible light irradiation and demonstrated an enhanced performance than the pure Fe₃O₄ microspheres, and the photocatalytic activity enhanced with the molar ratio of Fe₃O₄ microspheres and modified titanate gradually, which was attributed to the expansion of the surface area and the different electrostatic contact between the Fe₃O₄ microspheres and titanate nanosheets. Moreover, the obtained results revealed the high yield magnetic separation and efficient reusability of PTF-5 (96.7%) over 3 times reuse.     

Preparation of magnetically separable mesoporous activated carbons from brown coal with Fe_3O_4

Magnetically separable mesoporous activated carbon was prepared from brown coal in the presence of Fe_3O_4 as a bi-functional additive. Magnetic activated carbon(MAC) was characterized by lowtemperature nitrogen adsorption, scanning electron microscopy(SEM), transmission electron microscopy(TEM), X-ray diffraction(XRD), X-ray photoelectron spectroscopy(XPS) and vibrating sample magnetometry(VSM). The evolution behaviors and transition mechanism of Fe_3O_4 during the preparation of MAC were investigated. The results show that prepared MAC with 6 wt% Fe_3O_4 addition having a specific surface area and mesopore ratio of 370 m~2·g~(-1) and 55.7%, which meet the requirements of adsorption application and magnetic recovery. Highly dispersed iron-containing aggregates with the size of 0.1 lm in the MAC were observed. During the preparation of MAC, Fe_3O_4 could enhance the escape of volatiles during the carbonization. Fe_3O_4 could also accelerate burning off the carbon wall during activation, which leads to enlarging micropore size, then resulting in the generation of mesopore and macropore. As a result, a part of Fe_3O_4 converted into FeO, FeOOH, a-Fe, c-Fe, Fe_2 SiO_4 and compound of Aluminum-iron-silicon.The prepared activated carbon, which was magnetized by both of residual Fe_3O_4, reduced a-Fe and cFe, can be easily separated from the original solution by external magnetic field.     

Controlled preparation of monodisperse CoFe<Subscript>2</Subscript>O<Subscript>4</Subscript> nanoparticles by a facile method

CoFe2O4 nanoparticles (NPs) were synthesized by coprecipitation method using FeCl3·6H2O and CoCl2·6H2O as precursors.The synthesized conditions were optimized,such as added means of precipitator,quantity of precipitator,the mol ratio of Fe 3+ to Co2+,reaction temperature and pH value.The synthesized material was characterized by XRD,TEM,FTIR,EDS,Raman and its magnetic properties were studied by VSM.The experimental results confirm that the sample is cubic spinel structure CoFe2O4 with a narrow size distribution and a good dispersion feature.CoFe2O4 NPs with well-controlled shape and size was obtained at 70℃.The magnetic properties indicate superparamagnetic behavior and good saturated magnetization.     

Preparation and structure characteristics of nano-Bi2O3 powders with mixed crystal structure

The nano-Bi2O3 powders were prepared by a chemical precipitation method with Bi(NO3)3, HNO3 and NaOH as reactants. The structural characteristics and morphology of nano-Bi2O3 powders were investigated by X-ray diffraction and transmission electron microscopy, respectively. The results show that under the optimum condition that 300g/L Bi(NO3)3 reacts at 90℃ for 2 h, the Bi203 powders with 60 nm on the average and 99.5% in purity are obtained. The prepared nano-Bi2O3 powders contain a mixed crystal structure of monoclinic and triclinic instead of traditional structure of monoclinic α-Bi2O3. And the mixed crystal structure is stable in air. The reason for the appearance of the mixed crystal structure may be that the ionic radius ratio of Bi^3 to O^2- changes easily during the formation of nano-Bi2O3 particles by a chemical precipitation method.     

Synthesis of polyaniline-Fe<Subscript>3</Subscript>O<Subscript>4</Subscript> nanocomposites and their conductivity and magnetic properties

By using inorganic Fe₃O₄ nanoparticles of different content as nucleation sites, PAn-Fe₃O₄ nanorods were successfully synthesized through a simple, conventional, and inexpensive one-step in-situ polymerization method. The TEM images revealed the size and morphology of the resultant nanocomposite. The EDS pattern confirmed the existence of Fe₃O₄ in the composite. The FT-IR spectral analysis confirmed the formation of PAn encapsulated Fe₃O₄ nanocomposite. With the content of Fe₃O₄ increasing, the conductivity of the nanocomposites gradually decreases, meanwhile, the saturation magnetization increases and reveals a super paramagnetic behavior. With controllable electrical, magnetic, and electromagnetic properties, the well-prepared nanocomposites may have the potential applications in chemical sensors, catalysis, microwave absorbing, and electro-magneto-rheological fluids, etc.