Formation, characterization and magnetic properties of carbon-encapsulated iron carbide nanoparticles

Fe₃C nanoparticles encapsulated in carbon shell with a size range of 20–50 nm were obtained in large scale by reacting anhydrous FeCl₃, hexamethylenetetramine and metal Na in an autoclave at 650 °C. Magnetization measurements show that the as-obtained materials display superparamagnetic properties at room temperature. A possible formation mechanism of the core–shell nano-structures was discussed.     

Preparation and magnetic behavior of carbon-encapsulated iron nanoparticles by detonation method

Carbon-encapsulated iron (Fe@C) nanoparticles with core/shell structure have been successfully synthesized by detonation method, using a homemade composite explosive precursor. The detonation reaction was ignited by a non-electric detonator in nitrogen gas in an explosion vessel. The as-prepared detonation products were characterized by X-ray Diffraction, Transmission electron Microscopy, Raman spectroscopy and X-ray fluorescence. The magnetic behavior of the Fe@C materials was measured by vibrating sample magnetometer. The results showed that the detonation products were made up of the body centered cubic iron core and the graphitic carbon shell, of which the core diameter was in the range of 15–50 nm. Raman spectroscopy indicated that both graphitic and amorphous carbon occured in the outside shell structures. The hysteresis loops showed the as-made Fe@C nanoparticles were of superparamagnetic at 300 K temperature. A detonation reaction mechanism was proposed to explain the growth process of Fe@C nanoparticles based on these results.     

Nickel-cobalt nanoparticles supported on single-walled carbon nanotubes and their catalytic hydrogenation activity

Single-walled carbon nanotubes were synthesized from graphite using the arc discharge technique. A nickel/yttrium/graphite mixture was used as the catalyst. After purification by sonication in a Triton X-100 solution, nickel-cobalt metal nanoparticles were deposited on the surface of the single-walled carbon nanotubes. The resulting material and/or the nanotubes themselves were characterized by physisorption, Raman spectroscopy, high-resolution transition electron microscopy and X-ray diffraction. Raman spectroscopy indicates that the nanotubes, prepared by the arc discharge technique, are semi-conducting with a diameter centering at 1.4 nm. The average nickel-cobalt particle size is estimated to be in the region of 8 nm. The catalytic activity of the material was examined for the hydrogenation of unsaturated fatty acid methyl esters obtained from avocado oil. The carbon nanotube supported nickel-cobalt particles effectively hydrogenate polyunsaturated methyl linoleate to monounsaturated methyl oleate. In contrast to a conventional nickel on kieselghur catalyst, further hydrogenation of methyl oleate to undesired methyl stearate was not observed.     

Preparation of iron oxide nanoparticles by microwave synthesis and their characterization

In this study production of fine particle Fe2O3 via microwave processing of Fe(NO3)3.nH2O followed by low temperature annealing was reported. XRD was used to characterize the structural properties of nanoparticles. Approximate particle sizes were between 3-13 nm according to Scherrer's equation. Single point BET measurement results also show that samples have large surface area and they are nanometer sized particles. TEM study was conducted to examine the structure of the nanoparticles. TEM figure is in good agreement with the results obtained from Scherrer's equation using XRD spectra. In order to characterize the magnetic properties of the nanoparticles VSM (Vibrating Sample Magnetometer) was used. From these results it can be concluded that the sample containing only maghemite phase exhibits superparamagnetic behaviour, on the other hand sample containing both hematite and maghemite phases shows paramagnetic behaviour above 300 K, superparamagnetic behavior at lower temperatures.     

Continuous synthesis of controlled size carbon-encapsulated iron nanoparticles

Carbon-encapsulated iron nanoparticles were continuously and selectively synthesised in a thermal plasma jet from ethanol (carbon source) and Fe powders with different grain sizes. The grain size of the Fe powder influenced the size distribution of the as-produced carbon encapsulates. The products obtained from large Fe particles (50-78 μm) were comprised of small encapsulates with diameters between 5 and 10 nm. Larger carbon encapsulates with a broad diameter distribution (10-100 nm) were synthesised from the finest Fe particles (18 μm). It was also found that Fe particle size was the most crucial parameter for determining the encapsulation yield. The encapsulation yield was also influenced by the carbon to iron ratio and the thermal conductivity of the plasma gas.     

Electrochemical characterization of core-shell carbon-encapsulated magnetic nanoparticles

In this paper we studied the electrochemical behaviour of core-shell carbon-encapsulated magnetic nanoparticles (CEMNPs). CEMNPs have core diameters between 15 and 35 nm and are comprised of Fe, Fe₃C and NdC₂ nanoparticles encapsulated in crystalline carbon cages. Direct current cyclic voltammetry (CV) studies showed that carbon-encapsulated magnetic nanoparticles are stable in electrolyte environments. The graphitic coating perfectly isolates the encapsulated particles from the electrolyte in a wide range of potentials. CEMNP-based electrodes have low resistance (0.43-1.44 Ω cm²) and posses a specific capacity of 10-40 F g^− 1, which depends on the surface area and the crystallinity. It was shown, that CEMNPs are interesting multi-functional materials with a high potential to be used in various electrochemical devices.     

碳包覆NiO纳米颗粒的制备与性能

采用直流电弧放电等离子体技术成功制备了碳包覆NiO(NiO@C)纳米颗粒,并对样品的形貌、晶体结构、粒度、比表面积和孔结构采用高分辨透射电子显微镜、X射线衍射、X射线能量色散分析谱仪、拉曼散射光谱和N_2吸-脱附等测试手段进行了分析。实验结果表明:直流电弧等离子体技术制备的NiO@C纳米颗粒具有典型的核壳结构,内核为面心立方结构的NiO纳米颗粒,外壳为碳层。颗粒形貌主要为立方体结构,粒度均匀,分散性良好,粒径分布在30~70nm范围,平均粒径为50nm,外壳碳层的厚度为5nm。NiO@C纳米颗粒BET比表面积为28m~2/g,等效直径为46nm,与TEM和XRD测得的结果基本一致。Raman光谱说明样品中碳包覆层的石墨化程度较低,发生了红移现象。     

Preparation and characterization of thermosensitive PNIPAA-coated iron oxide nanoparticles

A new and facile approach was established to fabricate thermoresponsive poly(N-isopropylacrylamide) (PNIPAA) coated iron oxide nanoparticles in a non-aqueous medium. The morphology and structure of the nanoparticle-doped composite were analyzed by?means of transmission electron microscopy (TEM), x-ray powder diffraction (XRD), and Fourier transformation infrared spectrometry (FTIR). The thermosensitivity of the composite was also investigated. Results indicated that the oil-soluble iron oxide nanoparticles encapsulated with PNIPAA, composed of an inorganic iron oxide core and biocompatible PNIPAA shell, were dispersed well in water and had a sphere-like shape. The PNIPAA-coated iron oxide nanoparticles with such a kind of core-shell structure showed excellent thermosensitivity. Namely, the aqueous suspension of PNIPAA-coated iron oxide nanoparticles dramatically changed from transparent to opaque as the temperature increased from room temperature to 38?°C, showing potential as optical transmittance switch materials and their significance in the fields of protein adsorption and purification controlled release, and drug?delivery.     

Facile synthesis of magnetic iron oxide nanoparticles and their characterization

Magnetic iron oxide nanoparticles are synthesized by suitable modification of the standard synthetic procedure without use of inert atmosphere and at room temperature. The facile synthesis procedure can be easily scaled up and is of important from industrial point of view for the commercial large scale production of magnetic iron oxide nanoparticles. The synthesized nanoparticles were characterized by thermal, dynamic light scattering, scanning electron microscopy and transmission electron microscopy analyses.     

快速热解法制备炭包覆纳米金属磁性颗粒(英文)

以简单金属前躯体为原料通过快速热解法制备炭包覆纳米金属磁性颗粒,通过透射电镜、X-射线衍射、热重-示差扫描同步热分析及振动样品磁强计等对产物形貌、结构、成分与磁性能进行表征。结果表明:采用该方法制备的炭包覆纳米金属磁性颗粒形状为近球形颗粒,粒径均一,其中炭包覆镍纳米磁性颗粒的粒径集中在10nm～30nm范围,炭包覆铁纳米磁性颗粒粒径则在50nm～60nm范围;所制炭包覆纳米金属磁性颗粒在室温下具有顺磁性,其磁性能随金属颗粒含量的变化而改变。该方法有望发展成一种工艺简单,可进行连续工业化生产炭包覆纳米金属磁性颗粒的方法。     

Preparation and characterization of iron nanoparticles protected by an oxide film

Iron nanopowders ranging in particle size from 20 to 100 nm have been synthesized by reducing a 1-mm-thick iron(III) hydroxide layer in flowing hydrogen at 400°C and then passivated for 6–60 min in flowing argon containing 3% air. Our results demonstrate that the passivated iron nanopowders do not oxidize in air for six months. The iron nanoparticles have been characterized by X-ray diffraction (crystallite size evaluation), Auger electron spectroscopy, and polymolecular adsorption. The passivated iron nanoparticles have been shown to consist of a metallic core and oxide shell 2–4 nm in thickness.     

Preparation and characterization of bio-functionalized iron oxide nanoparticles for biomedical application

Amine modified iron oxide (Fe₃O₄) nanoparticles were synthesized by thermal decomposition method and were further used to bio-functionalize by grafting of N-hydroxysuccinimide (NHS) ester of folate and ethylenediaminetetraacetate (EDTA). Fe₃O₄ nanoparticles of ~ 22 nm were confirmed from X-ray diffraction (XRD) and transmission electron microscopy (TEM) studies. FT-IR studies indicated two bands at 1515 cm^− 1and 1646 cm^− 1, which can be attributed to carboxylic group and the amide linkage respectively, revealing the conjugation of folate with Fe₃O₄. The conjugation of the chelating agent showed strong C=O stretch and Fe-O vibrations at 1647 and 588 cm^− 1 respectively. The value of saturation magnetization for Fe₃O₄ nanoparticles was found to be 88 emu/g, which further reduced to 18 and 32% upon functionalization with EDTA and NHS ester folate, respectively. These amine modified Fe₃O₄ nanoparticles can also be functionalized with other bifunctional chelators, such as amino acids based diethylene triamine pentaacetic acid (DTPA), and thus find potential applications in radio-labeling, biosensors and cancer detection, etc.     

Hierarchically nanoporous ceria nanoparticles with a high-surface area: synthesis, characterization, and their catalytic activity

A redox route based on ethylene glycol mediated process was developed to synthesize hierarchically nanoporpous ceria nanoparticles (ceria HNPNPs). The synthesized ceria HNPNPs are composed of building blocks fabricated with cubic ceria nanocrystals of several nanometers in diameter. Scanning electron microscopy was performed to investigate the evolution process of ceria precursor, and a two-step growth process was suggested for the morphology evolution. The synthesized ceria HNPNPs exhibit high surface area, which lead to high catalytic activity for CO oxidation.     

Effect of oxidation and heat treatment on the morphology and electronic structure of carbon-encapsulated iron carbide nanoparticles

Carbon-encapsulated iron carbide nanoparticles have been produced by co-carbonization of a mixture of an aromatic heavy oil and ferrocene at 450 °C under autogenous pressure. Transformations of the morphology and electronic structure of nanoparticles induced by air oxidation and subsequent heat treatment in a nitrogen atmosphere were examined using transmission electron microscopy, X-ray diffraction, near edge X-ray absorption fine structure spectroscopy, and X-ray emission spectroscopy. It was found that hollow nanoparticles, composed of iron oxides and oxidized carbon, were developed with thermal air oxidation of the initial product at 280 °C for 5 h. The mild oxidation of the product (250 °C for 3 h) followed by the carbonization at 500–550 °C yielded the hollow nanoparticles containing iron carbide/oxides and defective graphite-like carbon. The further annealing of nanoparticles at 1000 °C produced carbon nanocapsules with highly graphitized carbon walls and partially filled by spherical iron carbide nanoparticles.     

Preparation of CuO nanopowders and their catalytic activity in photodegradation of Rhodamine-B

CuO nanopowders have been successfully synthesized in two different morphologies from same precursor using a facile gel to crystalline (reflux) and co-precipitation synthesis routes. SEM and TEM observations indicate that the morphology of the products depends on preparation technology, while XRD shows the formation of CuO nanocrystals with monoclinic crystal system in both cases. A comparison of morphological characterization of CuO nanopowders showed flower-like and aggregated nanoparticles in the form of clusters using reflux and co-precipitation techniques, respectively. Photocatalytic activity of the products in the aqueous solution of Rhodamine-B has been investigated under UV-light for a given time using UV–visible spectroscopy and the mineralization of organic substance was measured by total organic carbon (TOC) analysis. It was observed that the photocatalytic activity in the presence of flower-like CuO nanopowders was higher than that of observed with aggregated nanoparticles. Also the mechanisms for the formation of CuO nanopowders and the obtained results of photocatalytic degradation of Rhodamine-B are discussed.     

Highly basic CaO nanoparticles in mesoporous carbon materials and their excellent catalytic activity

Highly basic CaO nanoparticles immobilized mesoporous carbon materials (CaO-CMK-3) with different pore diameters have been successfully prepared by using wet-impregnation method. The prepared materials were subjected to extensive characterization studies using sophisticated techniques such as XRD, nitrogen adsorption, HRSEM-EDX, HRTEM and temperature programmed desorption of CO2 (TPD of CO2). The physico-chemical characterization results revealed that these materials possess highly dispersed CaO nanoparticles, excellent nanopores with well-ordered structure, high specific surface area, large specific pore volume, pore diameter and very high basicity. We have also demonstrated that the basicity of the CaO-CMK-3 samples can be controlled by simply varying the amount of CaO loading and pore diameter of the carbon support. The basic catalytic performance of the samples was investigated in the base-catalyzed transesterification of ethylacetoacetate by aryl, aliphatic and cyclic primary alcohols. CMK-3 catalyst with higher CaO loading and larger pore diameter was found to be highly active with higher conversion within a very short reaction time. The activity of 30% CaO-CMK3-150 catalyst for transesterification of ethylacetoacetate using different alcohols increases in the following order: octanol > butanol > cyclohexanol > benzyl alcohol > furfuryl alcohol.     

Preparation and characterization of magnetic nanofibrous composite membranes with catalytic activity

Magnetic nanofibrous composite membranes were electrospun from the mixtures of poly(acrylonitrile-co-acrylic acid) (PANCAA) and Fe₃O₄ nanoparticles. Field emission scanning electron microscopy (FESEM) and thermal gravimetric analysis (TGA) were used to characterize the composite membranes. TGA results indicate that the addition of Fe₃O₄ nanoparticles catalyzes the carbonization of PANCAA as well as dramatically increases the carbonization temperature. The intrinsic peroxidase-like activity of Fe₃O₄ nanoparticles was measured by the color reaction of phenol/4-amino antipyrine in the presence of H₂O₂. Under optimal conditions, the electrospun composite membranes show high peroxidase-like catalytic activity and reusability. Taking into account of the potentiality for separation, these as-prepared magnetic nanofibrous composite membranes will be applied in phenolic wastewater treatment.     

Preparation of monodispersed cobalt-boron spherical nanoparticles and their behavior during the catalytic decomposition of hydrous hydrazine

Monodispersed cobalt-boron spherical nanoparticles have been prepared through solution plasma processing in the presence of hexadecyltrimethyl ammonium bromide for the first time. The particle size of cobalt-boron can be adjusted by changing either the plasma time or the concentration of hexadecyltrimethyl ammonium bromide. The samples were characterized by X-ray diffraction, X-ray photoelectron spectroscopy, and transmission electron microscopy. During the decomposition of hydrous hydrazine, the obtained monodispersed cobalt-boron spherical nanoparticles exhibit higher catalytic activity and hydrogen selectivity than regular cobalt-boron prepared by direct reduction of Co²⁺ with BH₄⁻. The experimental investigations indicate that hydrous hydrazine along with the monodispersed cobalt-boron spherical nanoparticles may find application in small-scale on-board hydrogen storage and supply.     

铁基纳米粒子的制备及其在生物医学中的应用

综述了铁基纳米粒子以及磁性微球的主要制备原理和方法,并分析了不同方法的优缺点,同时也对磁性微球在医学中的应用作了较为详细的介绍.