Preparation of cobalt ferrite nanoparticles by using spent Li-ion batteries

Cobalt ferrite nanoparticles are a soft magnetic material have been extensively used in many electronic and magnetic applications. In this study, Co_0.8Fe_2.2O₄ nanoparticles with particle size of about 23.5 nm were directly synthesized by sol–gel auto-combustion and calcination methods using spent Li-ion batteries as raw materials. The overall process involves four steps: formation of homogeneous sols; formation of dried gels; combustion of the dried gels; and calcination of the dried gels after combustion at 1173 K for 2 h. The DTA–TG and IR were used to study the auto-combustion and thermal decomposition of the precursor, the morphology and structure of cobalt ferrite nanoparticles were characterized by XRD and TEM techniques. Moreover, the precise metal ion stoichiometry of cobalt ferrite nanoparticles was analyzed by ICP. The results revealed that the auto-combustion process was considered as a heat-induced exothermic oxidation–reduction reaction between nitrate ions and carboxyl group. The XRD patterns of calcination the dried gels after combustion confirmed the single phase spinel structure for the synthesized materials. The crystallite size was calculated from the most intense peak (3 1 1) using the Scherrer equation. The TEM photograph also shown that cobalt ferrite nanoparticles were well-dispersed and with little aggregation.     

柠檬酸在磁性纳米粒子上的吸附及性能表征

采用柠檬酸对Fe3O4磁性纳米粒子进行表面改性,制备了高稳定性的水基磁流体.利用衰减全反射红外光谱(ATR-FTIR)、热重分析(TG)、透射电镜(TEM)、X射线衍射(XRD)和振动样品磁强计(VSM)对改性前后的磁性粒子进行了表征.结果表明,柠檬酸在Fe3O4表面的吸附是氢键、静电力和共价键共同作用的结果,pH为4.8时化学吸附达到最大,符合Langmuir等温吸附,建立了等温吸附方程,饱和吸附量为100mg/g.     

钴铁氧体纳米粒子制备及其镧掺杂的磁性能研究

为了制备性能良好的钴铁氧体及改善其磁性能,通过改进的溶胶凝胶自蔓延燃烧法成功地制备了钴铁氧体(CoFe2O4)及掺镧(La)钴铁氧体纳米粒子.采用X射线衍射(XRD),透射电镜(TEM)、能谱分析(EDS)、振动样品磁场计(VSM)对所得粒子进行了结构、形貌、成分及磁性能表征.测试结果表明,利用改进的溶胶凝胶法制得钴铁氧体粒度均匀,且成相温度较低,500℃煅烧1h时平均粒径12nm左右;通过掺杂稀土镧元素对所得铁氧体的相结构有较强的影响,所得掺镧钴铁氧体与目标产物一致;所得钴铁氧体具有较高的矫顽力(737.33Oe),并且通过稀土元素镧的掺杂提高了钴铁氧体的矫顽力.     

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。     

Synthesis and characterization of nickel ferrite magnetic nanoparticles

Nickel ferrite (NiFe₂O₄) nanoparticles are prepared by a polyvinyl alcohol (PVA) assisted sol-gel auto-combustion method. The structure, composition, morphology and magnetic properties of the gel precursor are characterized by powder XRD, FT-IR, TGA, HR-SEM, TEM, HR-TEM and VSM. XRD confirms the formation of single-phase nickel ferrite with space group of Fd3m and inverse spinel structure. The vibration properties of nanoparticles are analysed by FT-IR spectrum. The thermal decomposition of the gel precursors is investigated by TGA. HR-SEM and TEM images show that the particles have spherical shape with particle size in the range of ∼30 nm and consistent with XRD result. The magnetic properties of these nanoparticles are studied for confirming the ferromagnetic behaviour at room temperature.     

磁流体浸没物磁场力分析及磁浮特性

物体浸没于磁流体中表现出磁浮特性，对其受力状态分析是准确描述其悬浮状态的前提和基础。基于非线性磁流体应力张量模型和稳态Bernoulli方程，建立磁流体中浸没物受力模型。借助非磁性体受力模型的简化计算方法以及磁性体与磁流体之间的多场效应关系，分别对非磁性体、磁性体两类浸没物在磁流体中所受磁浮力进行分析，结果表明非磁性浸没物在磁流体中仅受到外加磁场贡献的一次磁浮力，而磁性浸没物除受到一次磁浮力外，还受到其自身激发磁场贡献的二次磁浮力．永磁体在磁流体中位置决定的磁浮力满足一定条件时，永磁体能够自悬浮于磁流体中。     

Magnetisation behaviour of mixtures of ferrofluids and paramagnetic fluids with same particle volume fractions

In this study, γ-Fe₂O₃ ferrimagnetic nanoparticles and paramagnetic nanoparticles of p-MgFe₂O₄ (a hydroxide precursor for the preparation of magnesium ferrite materials) are produced by chemical precipitation technology. The γ-Fe₂O₃ ferrofluids and p-MgFe₂O₄ paramagnetic fluids are synthesised by Massart's method. The binary ferrofluids are obtained by mixing the ferrofluids and the paramagnetic fluids. There is insufficient magnetic interaction to aggregate the γ-Fe₂O₃ ferrimagnetic system and the p-MgFe₂O₄ paramagnetic system, so the magnetisation behaviour of the binary ferrofluids can be explored with reference to those of the single fluids. The magnetisation behaviour of single γ-Fe₂O₃ ferrofluids may be described by a model of gas-like compression. In the absence of a magnetic field, some particles can self-assemble into aggregates with a closed ring-like structure which make no contribution to the magnetisation of the γ-Fe₂O₃ ferrofluids. These ring-like aggregates result in the measured saturation magnetisation of the γ-Fe₂O₃ ferrofluids being smaller than the theoretical value calculated from the particles. During the magnetisation process, the polarised p-MgFe₂O₄ particles gas can orient the rings towards the direction of the field, so that the rings may fragment. Therefore, the measured saturation magnetisation of the γ-Fe₂O₃ ferrofluid component of the binary ferrofluids strengthens and the magnetisation process becomes easier than for pure γ-Fe₂O₃ ferrofluids.     

基于中空钴微米颗粒的磁流变液性能研究

采用水热法制备钴微米颗粒,通过X射线衍射仪、扫描电镜和振动样品磁强计对颗粒的相结构、形貌及磁性能进行表征。结果表明,颗粒为密排六方结构的单质钴,粒径3~5μm,内部呈中空结构,饱和磁化强度为161A·m2/kg。以中空钴微米颗粒为悬浮相,以硅油为基液,制备颗粒体积分数为12%的磁流变液。测试结果表明,基于中空钴微米颗粒的磁流变液的磁致剪切屈服强度在250kA/m磁场下达到37kPa,剪切应力的时间稳定性、长期静置的沉降稳定性等均优于同体积浓度的羰基铁粉磁流变液。     

Synthesis and characterization of biocompatible hydroxyapatite coated ferrite

Ferrite particles coated with biocompatible phases can be used for hyperthermia treatment of cancer. We have synthesized substituted calcium hexaferrite, which is not stable on its own but is stabilized with small substitution of La. Hexaferrite of chemical composition (CaO)_0.75(La₂0₃)_0.20(Fe₂O₃)₆ was prepared using citrate gel method. Hydroxyapatite was prepared by precipitating it from aqueous solution of Ca(NO₃)₂ and (NH₄)₂HPO₄ maintaining pH above 11. Four different methods were used for coating of hydroxyapatite on ferrite particles. SEM with EDX and X-ray diffraction analysis shows clear evidence of coating of hydroxyapatite on ferrite particles. These coated ferrite particles exhibited coercive field up to 2 kOe, which could be made useful for hysteresis heating in hyperthermia. Studies by culturing BHK-21 cells and WBC over the samples show evidence of biocompatibility. SEM micrographs and cell counts give clear indication of cell growth on the surface of the sample. Finally coated ferrite particle was implanted in Kasaulli mouse to test its biocompatibility. The magnetic properties and biocompatibility studies show that these hydroxyapatite coated ferrites could be useful for hyperthermia.     

Fe78Si13B9/铁氧体复合材料磁粉芯制备及其软磁性能

用Mn-Zn铁氧体溶胶对非晶Fe78Si13B9粉体包覆,模压成型制备了复合磁粉芯,并研究了复合材料磁粉芯的软磁性能.实验结果表明,铁氧体粉体在500℃×2h的热处理条件下逐渐生成,并在非晶Fe78Si13B9颗粒表面较好包覆;铁氧体溶胶的加入,大大提高了非晶Fe78Si13B9磁粉芯的品质因数Q值.当铁氧体溶胶量为7%、30℃的测试温度时,Fe78Si13B9/铁氧体复合材料磁粉芯的磁导率在1MHz时达到最大值32,Q值高达23.     

Preparation and characterization of cobalt ferrite by the polymerized complex method

Magnetic nanoparticles of Co-ferrite were prepared by the polymerized complex method. Heating in vacuum of a precursor solution containing citric acid (CA), ethylene glycol (EG) and cobalt and iron salts with a molar ratio of Co/Fe/CA/EG=1/2/9/22.5 at 130 °C produced a brownish transparent polymeric gel, which have been characterized by IR and NMR spectroscopy. The results of both techniques suggest two types of reactions: the formation of metal-CA complexes and successive esterification reactions between CA and EG. The organic fraction was removed by controlled thermal treatments (200–800 °C) whereby the bimetallic oxide was formed. The powders obtained were characterized by X-ray diffraction (XRD), vibrational sample magnetometry (VSM) and transmission electron microscopy (TEM). XRD analysis showed the presence of CoFe₂O₄ at 400 °C. The saturation magnetization values of the samples increased as a function of calcination temperature and reached a maximum of 79.8 emu/g at 800 °C. The TEM images showed spherical nanoparticles with sizes between 20 and 40 nm.     

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。     

Micelle based synthesis of cobalt ferrite nanoparticles and its characterization using Fourier Transform Infrared Transmission Spectrometry and Thermogravimetry

Cobalt ferrite (CoFe₂O₄) nanoparticles of average size 4 nm with narrow size distribution are synthesized by reverse micelle approach. The nanoparticles are characterized using powder X-ray diffraction (XRD), Dynamic Light Scattering (DLS), Theromogravimetric analysis (TGA) and Fourier Transform Infrared Transmission Spectrometry (FTIR). Three successive transformations are observed in the thermogram that correspond to the loss of solvent and surfactant; onset of the amorphous to crystallize conversion; and isochemical transformation, i.e. migration of cations between octahedral and tetrahedral sites in the inverse spinel structure. The isochemical transformation is further confirmed by FTIR. The IR absorption bands observed at 460 and 615 cm⁻¹ in the as-prepared CoFe₂O₄ nanoparticles correspond to the ferrite skeleton of octahedral and tetrahedral sites, respectively. The peak intensity at 615 and 460 cm⁻¹ is shifted to 601 and 440 cm⁻¹, respectively upon annealing at 320 and 400 °C. These results confirm migration of cations from the octahedral to the tetrahedral sites.     

纳米Fe3O4油基磁流体制备及性质研究

用共沉淀法制备磁流体的磁核一纳米Fe3O4，液体石蜡作基液和混合表面活性剂作分散介质而成功地制备出满足制备磁性药物微球需要的油基磁流体。研究了纳米Fe3O4、液体石蜡用量，表面活性剂的种类和组成比以及不同温度对磁流体性质的影响。并用XRD、TEM、旋转粘度计、磁天平等对磁流体的物相、粘度、磁性以及稳定性等进行了表征。     

Preparation,characterization and in vitro anticancer activity of paclitaxel conjugated magnetic nanoparticles

In this study, magnetic nanoparticles (MNPs) coated with L-aspartic acid (F-Asp NPs) were synthesized through a co-precipitation method and conjugated with paclitaxel (PTX) (F-Asp-PTX NPs) by esterification reaction between the carboxylic acid end groups on MNPs surface and the hydroxyl groups of the PTX and studied its cytotoxic effect in vitro. The successful conjugating of PTX onto the nanoparticles (NPs) was confirmed by X-ray diffraction (XRD), thermogravimetric analysis (TGA), differential scanning calorimetry (DSC), fourier transform infrared spectroscopy (FTIR), vibrating sample magnetometer (VSM) and transmission electron microscopy (TEM) techniques. The results showed that the average size was 46.11?±?7.8 (mean?±?SD (n?=?25)) nm. The cytotoxicity of void of PTX and F-Asp-PTX NPs were compared to each other by MTT assay of the treated MCF-7 cell line. The F-Asp-PTX NPs showed pH-dependent drug release behavior. These studies specify that F-Asp-PTX NPs have a very remarkable anticancer effect, for breast cancer cell line.     

Structural,magnetic properties,and induction heating behavior studies of cobalt ferrite nanopowders synthesized using modified co-precipitation method

Nanocrystalline cobalt ferrite CoFe₂O₄ powders have been successfully synthesized via modified co-precipitation at low temperature. Obviously, well crystalline CoFe₂O₄ phase was obtained from the precipitated precursors at pH 10 using 5?M NaOH as a base thermally treated at 80°C for 1?h in aqueous medium in the absence and the presence of 1000?ppm cetyl trimethyl ammonium bromide (CTAB) as well as sodium dodecyl sulfate (SDS) as cationic and anionic surfactants, respectively. Meanwhile, the spinel ferrite was observed with the similar conditions using ethylene glycol as an organic solvent. The microstructures of the formed powders exhibited nanospheres like structure with narrow size distribution from 6 to 10?nm. The magnetic properties of the formed cobalt ferrite powders strongly depend on the synthesis conditions. For instance, the highest saturation magnetization (M_s?=?36.2?emu/g) was achieved in the aqueous medium, whereas the lowest saturation magnetization (M_s?=?16.2?emu/g) was accomplished in the ethylene glycol medium. Indeed, heating properties of the CoFe₂O₄ samples in an alternating magnetic field (AMF) at 160?kHz were estimated. Of note, it is clear that the specific heat rate SAR values were in the range from 104.5 to 302.0?W/g at different synthesis conditions, making co-ferrite appropriate for hyperthermia treatment of cancer.     

化学共沉淀法制备NiCuZn铁氧体微粉及其磁性能

采用预烧氧化法(化学共沉淀法制备的前驱体在高温下预烧)制备了NiCuZn铁氧体微粉。结果表明,预烧氧化法制备的NiCuZn铁氧体微粉平均晶粒尺寸约为44.1nm。随着预烧温度升高,样品D50增大。当预烧温度为850℃时,平均颗粒尺寸为2μm左右,比饱和磁化强度为62A.m2/kg,起始磁导率约为90,损耗也较小,截止频率为59MHz。     

Preparation of cobalt oxide nanoparticles and cobalt powders by solvothermal process and their characterization

Co₃O₄ nanoparticles and cobalt (fcc-Co) powders were successfully synthesized by solvothermal process from a single precursor. The reaction of Co(Ac)₂ with sodium dodecylbenzenesulfonate (SDBS) shows evident-dependent temperature effect. At 180 °C, Co(Ac)₂ reacts with SDBS to produce precursor CoCO₃ plate structures, which are assembled by small nanoparticles. At the temperature of 250 °C, the precursor CoCO₃ can be gradually decomposed to form Co₃O₄ nanoparticles with diameter of ca. 70 nm. While, at 250 °C, the reaction of Co(Ac)₂ with SDBS also produce precursor CoCO₃ nanoparticles/plates, but the CoCO₃ nanoparticles/plates would only decompose to give metal Co. In this process, SDBS acts as not only a surfactant but also a reagent. Magnetic measurements reveal that the as-prepared Co₃O₄ nanoparticles exhibit weak ferromagnetic properties and Co powders show ferromagnetic properties. In addition, a possible formation mechanism was elaborately discussed.     

Preparation of paclitaxel-loaded microspheres with magnetic nanoparticles

The objective of this paper was to prepare paclitaxel-loaded microspheres, a kind of target-orientation anticancer drug. The paclitaxel-loaded microspheres were prepared with magnetic Fe₃O₄ nanoparticles and taxol. The morphology was characterized by scanning electron microscopy (SEM), and the average size and the size distribution were determined by a laser-size distributing instrument. High performance liquid chromatography (HPLC) was used to measure the paxlitaxel content. Experimental results indicated that the effective drug loading and the entrapment ratio of paclitaxel-loaded microspheres were 1.83% and 92.62%, respectively.