Preparation of hollow spherical magnetite nanoparticles

We have developed and tested procedures for the synthesis of hollow spherical magnetite nanoparticles and analyzed the general mechanisms of their formation in relation to their structure and morphology. The phase composition, elemental composition, and morphology of the synthesized particles have been examined by X-ray diffraction, Auger electron spectroscopy, scanning electron microscopy, and atomic force microscopy, and their magnetic properties have been studied by an induction method using a vibrating sample magnetometer. The results demonstrate that the proposed procedures enable the preparation of hollow porous spherical magnetite particles 40 nm to 100 μm in diameter, with a wall thickness ≃d/10 and a narrow size distribution.     

Solvothermal synthesis and magnetic properties of magnetite nanoplatelets

Nanostructured magnetite plates were synthesized by a simple solvothermal route where ethylenediamine was used as the solvent and reducing agent. The morphology and structure of the as-prepared platelets were characterized using X-ray diffraction, infrared spectroscopy and transmission electron microscopy. The results showed that the products are magnetite crystals with plate like morphology whose thickness is estimated to be 20 nm. Magnetic measurements at 300 K gave the saturation magnetization and the coercive field of nanostructured magnetite 87.4 emu/g and 178 Oe, respectively, which are higher than those of cubic nanoparticles, due to the higher shape anisotropy of magnetite nanoplatelets.     

Extracellular synthesis of magnetite and metal-substituted magnetite nanoparticles

We have developed a novel microbial process that exploits the ability of Fe(III)-reducing microorganisms to produce copious amounts of extracellular magentites and metal-substituted magnetite nanoparticles. The Fe(III)-reducing bacteria (Theroanaerobacter ethanolicus and Shewanella sp.) have the ability to reduce Fe(III) and various metals in aqueous media and form various sized magnetite and metal-substituted magnetite nano-crystals. The Fe(III)-reducing bacteria formed metalsubstituted magnetites using iron oxide plus metals (e.g., Co, Cr, Mn, Ni) under conditions of relatively low temperature (<70 degrees C), ambient pressure, and pH values near neutral to slightly basic (pH = 6.5 to 9). Precise biological control over activation and regulation of the biosolid-state processes can produce magnetite particles of well-defined size (typically tens of nanometers) and crystallographic morphology, containing selected dopant metals into the magnetite (Fe(3-y)XyO4) structure (where X = Co, Cr, Mn, Ni). Magnetite yields of up to 20 g/L per day have been observed in 20-L vessels. Water-based ferrofluids were formed with the nanometer sized, magnetite, and metal-substituted biomagnetite particles.     

溶剂热法制备Fe_3O_4/氧化石墨烯复合材料及其性能研究

以氧化石墨和二茂铁为原料,采用溶剂热法原位一步合成了Fe3O4/还原氧化石墨烯(Fe3O4/RGO)复合物,通过X射线衍射(XRD)、傅里叶变换红外光谱(FT-IR)、扫描电镜(SEM)、透射电镜(TEM)、振动样品磁强计(VSM)、循环伏安测试等手段对复合材料的形貌、结构、磁性能和电化学性能进行了表征。结果表明,该方法具有简单、可控的优点,通过调变前驱物中氧化石墨和二茂铁的比例,可以控制复合物中Fe3O4纳米粒子的负载量。所制备Fe3O4/RGO复合材料由平均粒径约20nm的Fe3O4纳米颗粒高度分散在还原氧化石墨烯片层上组成,具有较好的超顺磁性,电化学稳定性和良好的倍率性能。     

Low temperature synthesis of magnetite and maghemite nanoparticles

We report on the synthesis of iron oxide nanoparticles below 100 degrees C by a simple chemical protocol. The uniqueness of the method lies in the use of Ferrous ammonium sulphate (in conjugation with FeCl3) which helps maintain the stability of Fe2+ state in the reaction sequence thereby controlling the phase formation. Hexamine was added as the stabilizer. The nanoparticles synthesized at three different temperatures viz, 5 degrees, 27 degrees, and 95 degrees C are characterized by several techniques. Generally, when a mixture of Fe3+ and Fe2+ is added to sodium hydroxide, alpha-Fe2O3 (the anti-ferromagnetic phase) is formed after the dehydration process of the hydroxide. In our case however, the phases formed at all the three temperatures were found to be ferro (ferri) magnetic, implying modification of the formation chemistry due to the specifics of our method. The nanoparticles synthesized at the lowest temperature exhibit magnetite phase, while increase in growth temperature to 95 degrees C leads to the maghemite phase.     

Synthesis of hollow spheres with mesoporous silica nanoparticles shell

Hollow spheres with mesoporous silica nanoparticles shell were synthesized with the use of cetyltrimethylammonium bromide (CTAB) and polystyrene (PS) hollow spheres as dual templates. The key to this study is that the uneven surface of the template provides nucleation sites for mesoporous nanoparticles, resulting in the formation of hollow spheres with mesoporous silica nanoparticles shell. The final products with hierarchical mesopores can be obtained through a simple one-step approach.     

溶剂热法合成粒径可控的Fe3O4磁性介孔/空心球

采用简便的溶剂热法合成粒径可控的Fe3O4磁性介孔/空心球(mesoporous/hollow spheres of magne-tite,MHSM),粒径从80 nm至400 nm可调.通过调节反应时间、NH4HCO3与NH4Ac的摩尔比来控制MHSM的形貌、粒径以及介孔-空心的程度.采用XRD、SEM、TEM、VSM多种表征手段对MHSM进行了表征,结果表明NH4HCO3和NH4Ac的摩尔比对MHSM结构的形成、形貌、粒径起关键性的作用;NH4+的浓度对MHSM的粒径和磁性有决定性的影响;保持NH4HCO3和NH4Ac的摩尔比不变,延长反应时间对MHSM的结构与空腔生长有一定的影响.     

葡聚糖包被磁性纳米材料的合成及其特异性细胞毒性

利用二甘醇作溶剂和还原剂水解还原三氯化铁,合成水溶性的葡聚糖包被磁性纳米材料(MNPs),选择大鼠的肝脏细胞BRL3A、肾脏细胞NRK、星型角质细胞和外周血单个核细胞(PBMC),运用流式细胞仪(FCM)检测细胞凋亡和苏木素伊红(HE)染色细胞形态学观察进行细胞毒性研究.结果发现,MNPs共培养浓度达到64μg/ml时,PBMC出现明显凋亡(p＜0.01),而其它几种细胞在MNPs共培养浓度达到128μg/ml时,仍未出现明显凋亡(p＞0.05).电镜观察发现BRL3A、NRK和星型角质细胞均出现内吞该纳米颗粒,而未观察到PBMC的吞噬现象.结果提示,葡聚糖包被的MNPs的细胞毒性具有细胞特异性,实质性脏器细胞毒性较小,可能与其存在内吞MNPs能力有关,提示葡聚糖包被的MNPs可以运用于机体实质脏器核磁造影剂和药物载体.     

Solvothermal synthesis and characterization of functionalized graphene sheets (FGSs)/magnetite hybrids

Novel functionalized graphene sheets (FGSs)/Fe₃O₄ hybrids were synthesized through a facile one-step solvothermal method using FeCl₃ as iron source, ethylene glycol as the reducing agent and graphene nanosheets as templates. The morphology, composition and phase structure of as-prepared hybrid materials were characterized by scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS), X-ray diffraction (XRD), and transmission electron microscopy (TEM). These results showed that denseness, size and crystallinity of magnetite can be altered by controlling the reaction parameters. Magnetization measurement indicated that both coercivity and saturation magnetization increased linearly with increasing magnetite concentration in hybrid materials. The measured relative complex permittivity indicated that a high resistivity existed in the FGSs/Fe₃O₄ inorganic hybrids. The magnetic loss was caused mainly by ferromagnetic natural resonance, which is in agreement with the Kittel equation. The novel inorganic hybrid materials are believed to have potential applications in the microwave absorbing performances.     

Fabrication of silver-loaded hollow mesoporous aluminosilica nanoparticles and their antibacterial activity

A facile and an effective route for the preparation of silver-loaded hollow mesoporous aluminosilica ([Ag]-HMAS) nanoparticles is reported. In our fabrication process, the solid silica nanoparticles are first converted into high-quality hollow mesoporous aluminosilica particles, and then silver ions are induced into the matrix through an ion-exchange method. By EDX and ICP analysis, it is found that the final [Ag]-HMAS particles have high silver loading (15.8 % by weight), and the release amount of silver ions can be effectively controlled by altering the concentrations of Na⁺ in the solution. The antibacterial properties of the [Ag]-HMAS particles against Escherichia coli (Gram-negative bacteria) and Bacillus subtilis (Gram-positive bacteria) are also investigated, both in liquid systems and on solid agar plates. The results show that the [Ag]-HMAS particles are highly effective against both Gram-negative and Gram-positive bacteria.     

Continuous synthesis of magnetite nanoparticles in supercritical methanol

Magnetite (Fe₃O₄) nanoparticles are synthesized continuously in supercritical methanol (scMeOH) without using reducing agents at 30 MPa, 400 °C and a residence time of 38 s. XRD analysis reveals that particles synthesized in scMeOH retain magnetite crystalline structure while particles synthesized in supercritical water retain hematite (α-Fe₂O₃) crystalline structure. The scMeOH acts both as a reaction medium and a reducing agent. The magnetite nanoparticles are spherical in shape with an average diameter of 21 ± 2 nm, as measured using SEM and TEM. The saturation magnetization of the magnetite nanoparticle is 76.6 emu/g.     

Magnetic properties of magnetite nanoparticles coated with mesoporous silica by sonochemical method

In this paper we present the magnetic properties of mesoporous silica-coated Fe₃O₄ nanoparticles. The coating of magnetite nanoparticles with mesoporous silica shell was performed under ultrasonic irradiation. The obtained mesoporous silica-coated magnetite nanoparticles were characterized by powder X-ray diffraction, focused ion beam-scanning electron microscopy, nitrogen adsorption-desorption isotherms and vibrating sample magnetometer. The hysteretic behavior was studied using first-order reversal curves diagrams. The X-ray diffraction result indicates that the extreme chemical and physical conditions created by acoustic cavitations have an insignificant effect on crystallographic structural characteristic of magnetite nanoparticles. Changes in the coercivity distributions of the magnetite nanoparticles were observed on the first-order reversal curves diagrams for the samples with coated particles compared with the samples containing uncoated particles of magnetite. The coated particles show an increased most probable coercivity of about 20% compared with the uncoated particles which can be associated with an increased anisotropy due to coating even if the interaction field distribution measured on the diagrams are virtually identical for coated/uncoated samples.     

Solvothermal synthesis of ceria nanoparticles with large surface areas

Ceria nanoparticles were obtained by the calcination of precursors synthesised via the solvothermal reaction of cerium acetate. The CeO₂ samples obtained by the thermal decomposition of Ce(C₇H₁₅COO)₃·xH₂O synthesised by solvothermal reaction in 1,4-butanediol in the presence of octanoic acid had an extremely large surface area of 180 m²/g. The Ru catalyst supported on this CeO₂ sample showed a high catalytic activity for benzyl alcohol oxidation.     

Microbial synthesis of magnetite and Mn-substituted magnetite nanoparticles: influence of bacteria and incubation temperature

Microbial synthesis of magnetite and metal (Co, Cr, Ni)-substituted magnetites has only recently been reported. The objective of this study was to examine the influence of Mn ion on the microbial synthesis of magnetite nanoparticles. The reductive biotransformation of an akaganeite (beta-FeOOH) or a Mn-substituted (2-20 mol%) akaganeite (Fe(1-x)Mn(x)OOH) by Shewanella loiha (PV-4, 25 degrees C) and Thermoanaerobacter ethanolicus (TOR-39, 60 degrees C) was investigated under anaerobic conditions at circumneutral pH (pH = 7-8). Both bacteria formed magnetite nanoparticles using akaganeite as a magnetite precursor. By comparison of iron minerals formed by PV-4 and TOR-39 using Mn-mixed akaganeite as the precursor, it was shown that PV-4 formed siderite (FeCO3), green rust [Fe2+Fe3+(OH)16CO3 x 4H2O], and magnetite at 25 degrees C, whereas TOR-39 formed mainly nm-sized magnetite at 60 degrees C. The presence of Mn in the magnetite formed by TOR-39 was revealed by energy dispersive X-ray analysis (EDX) is indicative of Mn substitution into magnetite crystals. EDX analysis of iron minerals formed by PV-4 showed that Mn was preferentially concentrated in the siderite and green rust. These results demonstrate that coprecipitated/sorbed Mn induced microbial formation of siderite and green rust by PV-4 at 25 degrees C, but the synthesis of Mn-substituted magnetite nanoparticles proceeded by TOR-39 at 60 degrees C. These results indicate that the bacteria have the ability to synthesize magnetite and Mn-substituted magnetite nano-crystals. Microbially facilitated synthesis of magnetite and metal-substituted magnetites at near ambient temperatures may expand the possible use of specialized ferromagnetic nano-particles.     

空心羟基磷灰石亚微球/壳聚糖可注射水凝胶的制备及表征

采用W/O/W复乳法制备空心羟基磷灰石(HAP)亚微球,将空心HAP亚微球均匀分布在壳聚糖/甘油磷酸钠(CS/GP)体系中制备可注射HAP/CS水凝胶(gel 1),同时制备可注射CS水凝胶(gel 2).用X射线衍射仪、场发射透射电镜、红外光谱、扫描电镜对空心HAP亚微球和水凝胶进行了表征,并比较分析了两种溶胶的成胶...     

Simultaneous synthesis of polyaniline nanorods and magnetite nanoparticles via self-assembly method

In this work, polyaniline (PANI) nanorods and magnetite (Fe₃O₄) nanoparticles have been synthesised by using ammonium persulphate as oxidant via in-situ chemical oxidative polymerisation of aniline in presence of excess of organic sulphonic acid. The resulting PANI/Fe₃O₄ nanocomposites materials were characterised using X-ray diffraction, UV-visible spectroscopy, Fourier transform infrared spectroscopy, scanning electron microscopy, transmission electron microscopy, vibrating sampling magnetometer and thermogravimetric analysis. Spectroscopic results indicated the successful formation of PANI/Fe₃O₄ nanocomposites. As obtained, PANI/Fe₃O₄ nanocomposites have Fe₃O₄ particle size in the range of 3.2–7?nm. Morphologies of PANI/Fe₃O₄ nanocomposites were found to be dependent on the molar ratio of aniline to organic acid. Under certain polymerisation conditions, PANI rods like structures were obtained. PANI/Fe₃O₄ nanocomposites have superparamagnetism and higher thermal stability.     

Solvothermal synthesis and characterization of acicular α-Fe2O3 nanoparticles

Nanometer-sized α-Fe₂O₃ particles have been prepared by a simple solvothermal method using ferric acetylacetonate as a precursor. The products were characterized by X-ray diffraction (XRD), energy dispersive X-ray microanalysis (EDAX), X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM), transition electron microscopy (TEM), infrared spectroscopy (IR) and thermal analysis (TG-DTA). XRD indicates that the product is single-phase α-Fe₂O₃ with rhombohedral structure. Bundles of acicular shaped nanoparticles are seen in TEM images with an aspect ratio ～ 12; typically 8–12 nm wide and over 150 nm long. The α-Fe₂O₃ nanoparticles posses a high thermal stability, as observed on thermal analysis traces.     

Solvothermal synthesis of solid and hollow CoO nanospheres and their electrochemical properties in lithium-ion battery

Solid and hollow CoO nanospheres were synthesized by solvothermal method with oleic acid as reactant and SiO₂ as template. Each sample of high-purity CoO was characterized by X-ray diffraction, field-emission scanning electron microscopy, transmission electron microscopy and X-ray photoelectron energy spectroscopy, respectively. Both solid and hollow CoO nanospheres as anode for lithium-ion battery were tested by galvanostatic discharge–charge experiments. The first discharge capacity of 1598 and 1640 mAh g^?1 was obtained at 0.1C for solid and hollow CoO nanospheres, respectively. Hollow CoO nanospheres showed better cycle performance.