Thermal plasma synthesis of superparamagnetic iron oxide nanoparticles

Superparamagnetic iron oxide nanoparticles were synthesized by injecting ferrocene vapor and oxygen into an argon/helium DC thermal plasma. Size distributions of particles in the reactor exhaust were measured online using an aerosol extraction probe interfaced to a scanning mobility particle sizer, and particles were collected on transmission electron microscopy (TEM) grids and glass fiber filters for off-line characterization. The morphology, chemical and phase composition of the nanoparticles were characterized using TEM and X-ray diffraction, and the magnetic properties of the particles were analyzed with a vibrating sample magnetometer and a magnetic property measurement system. Aerosol at the reactor exhaust consisted of both single nanocrystals and small agglomerates, with a modal mobility diameter of 8-9 nm. Powder synthesized with optimum oxygen flow rate consisted primarily of magnetite (Fe 3O 4), and had a room-temperature saturation magnetization of 40.15 emu/g, with a coercivity and remanence of 26 Oe and 1.5 emu/g, respectively. © Springer Science+Business Media, LLC 2011.

Effect of size, composition, and morphology on magnetic performance: First-order reversal curves evaluation of iron oxide nanoparticles

© 2014 AIP Publishing LLC. Superparamagnetic nanoparticles are employed in a broad range of applications that demand detailed magnetic characterization for superior performance, e.g., in drug delivery or cancer treatment. Magnetic hysteresis measurements provide information on saturation magnetization and coercive force for bulk material but can be equivocal for particles having a broad size distribution. Here, first-order reversal curves (FORCs) are used to evaluate the effective magnetic particle size and interaction between equally sized magnetic iron oxide (Fe2O3) nanoparticles with three different morphologies: (i) pure Fe2O3, (ii) Janus-like, and (iii) core/shell Fe2O3/SiO2synthesized using flame technology. By characterizing the distribution in coercive force and interaction field from the FORC diagrams, we find that the presence of SiO2in the core/shell structures significantly reduces the average coercive force in comparison to the Janus-like Fe2O3/SiO2and pure Fe2O3particles. This is attributed to the reduction in the dipolar interaction between particles, which in turn reduces the effective magnetic particle size. Hence, FORC analysis allows for a finer distinction between equally sized Fe2O3particles with similar magnetic hysteresis curves that can significantly influence the final nanoparticle performance.

The phase of iron catalyst nanoparticles during carbon nanotube growth

We study the Fe-catalyzed chemical vapor deposition of carbon nanotubes by complementary in situ grazing-incidence X-ray diffraction, in situ X-ray reflectivity, and environmental transmission electron microscopy. We find that typical oxide supported Fe catalyst films form widely varying mixtures of bcc and fcc phased Fe nanoparticles upon reduction, which we ascribe to variations in minor commonly present carbon contamination levels. Depending on the as-formed phase composition, different growth modes occur upon hydrocarbon exposure: For γ-rich Fe nanoparticle distributions, metallic Fe is the active catalyst phase, implying that carbide formation is not a prerequisite for nanotube growth. For α-rich catalyst mixtures, Fe3C formation more readily occurs and constitutes part of the nanotube growth process. We propose that this behavior can be rationalized in terms of kinetically accessible pathways, which we discuss in the context of the bulk iron-carbon phase diagram with the inclusion of phase equilibrium lines for metastable Fe3C. Our results indicate that kinetic effects dominate the complex catalyst phase evolution during realistic CNT growth recipes. © 2012 American Chemical Society.

The production of separate streams of pure hydrogen and carbon dioxide from coal via an iron-oxide redox cycle

A chemical looping process using the redox reactions of iron oxide has been used to produce separate streams of pure H2 and CO2 from a solid fuel. An iron oxide carrier prepared using a mechanical mixing technique and comprised of 100wt.% Fe2O3 was used. It was demonstrated that hydrogen can be produced from three representative coals - a Russian bituminous, a German lignite and a UK sub-bituminous coal. Depending on the fuel, pure H2 with [CO] ≲50vol.ppm can be obtained from the proposed process. The cyclic stability of the iron oxide carrier was not adversely affected by contaminants found in syngas which are gaseous above 273K. Stable quantities of H2 were produced over five cycles for all three coals investigated. Independent of the fuel, SO2 was not formed during the oxidation with steam, i.e. the produced H2 was not contaminated with SO2. Since oxidation with air removes contaminants and generates useful heat and pure N2 for purging, it should be included in the operating cycle. Overall, it was demonstrated that the proposed process may be an attractive approach to upgrade crude syngas produced by the gasification of low-rank coals to pure H2, representing a substantial increase in calorific value, whilst simultaneous capturing CO2, a greenhouse gas. © 2010 Elsevier B.V.

Hermetically-coated superparamagnetic Fe2O3 particles with SiO2 nanofilms

Magnetic nanoparticles are frequently coated with SiO2to improve their functionality and bio-compatibility in a range of biomedical and polymer nanocomposile applications. In this paper, a scalable flame aerosol technology is used to produce highly dispersible, superparamagnetic iron oxide nanoparticles hermetically coaled with silica to retain full magnetization performance. Iron oxide particles were produced by flame spray pyrolysis (FSP) of iron acelylacetonale in xylene/acetonitrile solutions, and the resulting aerosol was in situ coaled with SiO2 by oxidation of swirling hexamethlydisiloxane vapor. The process allows independent control of the core Fe2O3, particle properties and the thickness of their silica coaling film. This ensures that the non-magnetic SiO2 layer can be closely controlled and minimized. The optimal SiO2 content for complete (hermetic) encapsulation of the magnetic core particles was determined by isopropanol chemisorption. The magnetization of Fe2O3 coated with about 2 nm thin SiO2 layers was nearly identical lo that of uncoated, pure Fe2O3 nanoparlicles.

Hermetically coated superparamagnetic Fe2O3 particles with SiO2 nanofilms

Magnetic nanoparticles are frequently coated with SiO2 to improve their functionality and biocom-patibility in a range of biomedical and polymer nanocomposite applications. In this paper, a scalable flame aerosol technology is used to produce highly dispersible, superparamagnetic iron oxide nanoparticles hermetically coated with silica to retain full magnetization performance. Iron oxide particles were produced by flame spray pyrolysis of iron acetylacetonate in xylene/acetonitrile solutions and the resulting aerosol was in situ coated with silicon dioxide by oxidation of swirling hexamethlydisiloxane vapor. The process allows independent control of the core Fe2O3 (maghemite) particle properties and the thickness of their silica coating film. This ensures that the nonmagnetic SiO2 layer can be closely controlled and minimized. The optimal SiO2 content for complete (hermetic) encapsulation of the magnetic core particles was determined by isopropanol chemisorption. The magnetization of Fe 2O3 coated with about 2 nm thin SiO2 layers was nearly identical to that of uncoated, pure Fe2O3 nanoparticles. © 2009 American Chemical Society.

The attrition behaviour of oxygen-carriers under inert and reacting conditions

The attrition of two potential oxygen-carriers for chemical-looping, 100. wt% mechanically-mixed, unsupported iron oxide (400-600 μm diameter) and 25. wt% copper oxide impregnated on alumina (600-900 μm diameter), has been studied. The rates of attrition of batches of these particles whilst they were being fluidised and subjected to successive cycles of reduction and oxidation were determined by measuring the rate of production of fine particles elutriated from the bed, as well as progressive changes in the distribution of particle sizes retained in the bed. The ability of the particles to withstand impacts was also investigated by examining the degree of fragmentation of 1. g of reacted particles of known size on projecting them at a target at various velocities. It was found that the mechanical strength of the iron oxide particles deteriorated significantly after repeated cycles of oxidation and reduction. Thus, the rate of elutriation increased ~35-fold between the 1st and 10th cycle. At an impact velocity of 38. m/s, the amount of fragmentation in the impact test, viz. mass fraction of particles after impact having a size less than that before impact, increased from ~2.3. wt% (fresh particles) to 98. wt% after the 10th cycle. The CuO particles, in comparison, were able to withstand repeated reaction: no signs of increased rates of elutriation or fragmentation were observed over ten cycles. These results highlight the importance of selecting a durable support for oxygen-carriers. © 2011 Elsevier Ltd.

High temperature robust SOI ethanol sensor

In this paper we present a robust SOI-CMOS ethanol sensor based on a tungsten-doped lanthanum iron oxide sensing material. The device shows response to gas, has low power consumption, good uniformity, high temperature stability and can be manufactured at low cost and with integrated circuitry. The platform is a tungsten-based CMOS micro-hotplate that has been shown to be stable for over two thousand hours at a high temperature (600°C) in a form of accelerated life test. The tungsten-doped lanthanum iron oxide was deposited on the micro-hotplate as a slurry with terpineol using a syringe, dried and annealed. Preliminary gas testing was done and the material shows response to ethanol vapour. These results are promising and we believe that this combination of a robust CMOS micro-hotplate and a good sensing material can form the basis for a commercial CMOS gas sensor. © 2011 Published by Elsevier Ltd.

The effect of addition of ZrO2 to Fe2O3 for hydrogen production by chemical looping

In this paper, a synthetic mixture of ZrO2 and Fe 2O3 was prepared by coprecipitation for use in chemical looping and hydrogen production. Cycling experiments in a fluidized bed showed that a material composed of 30 mol % ZrO2 and 70 mol % Fe 2O3 was capable of producing hydrogen with a consistent yield of 90 mol % of the stoichiometric amount over 20 cycles of reduction and oxidation at 1123 K. Here, the iron oxide was subjected to cycles consisting of nearly 100% reduction to Fe followed by reoxidation (with steam or CO 2 and then air) to Fe2O3. There was no contamination by CO of the hydrogen produced, at a lower detection limit of 500 ppm, when the conversion of Fe3O4 to Fe was kept below 90 mol %. A preliminary investigation of the reaction kinetics confirmed that the ZrO2 support does not inhibit rates of reaction compared with those observed with iron oxide alone. © 2012 American Chemical Society.

Electrical/optical dual-function redox potential transistor

We demonstrate a new type of transistors, the electrical/optical "dual-function redox-potential transistors", which is solution processable and environmentally stable. This device consists of vertically staked electrodes that act as gate, emitter and collector. It can perform as a normal transistor, whilst one electrode which is sensitised by dye enables to generate photocurrent when illuminated. Solution processable oxide-nanoparticles were used to form various functional layers, which allow an electrolyte to penetrate through and, consequently, the current between emitter and collector can be controlled by the gate potential modulated distribution of ions. The result here shows that the device performs with high ON-current under low driving voltage (<1â€...V), while the transistor performance can readily be controlled by photo-illumination. Such device with combined optical and electrical functionalities allows single device to perform the tasks that are usually done by a circuit/system with multiple optical and electrical components, and it is promising for various applications.