Abstract:One of the major obstacles in the incorporation of nanomaterials in high technology is the lack of new processes for the bulk production of the materials with compositions tailored to suit the application. Oxides can potentially be reduced to metals, intermetallics or alloys by hydrogen or natural gas. The formation of homogeneous alloys and intermetallics by this method has been confirmed by a number of experimental studies. The kinetics of hydrogen reduction of pure oxides of transition metals as well as com… Show more
“…The reduction in a hydrogen atmosphere to produce high-purity nanoparticles from fine metal oxides is significant. [25][26][27][28][29][30][31] Regarding the application, the synthesis of particles with a definite shape, tailor-made size, and narrow size distribution may be the main goal with a definite composition either as a crystal or amorphous phase.…”
The synthesis of magnetic Ni nanoparticles is being investigated by the reduction of NiO nanoparticles in the presence of hydrogen gas. In this study, nanocrystalline NiO particles have been synthesized by a homogenous carbonate precipitation method employing nickel electrolyte (NiSO 4 ) as the source of nickel and ammonium hydrogen carbonate as the precipitating agent. Nickel electrolyte (NiSO 4 ) was obtained after processing of sea nodules by the roastingammonia leaching-solvent extraction method. The physicochemical characterization of NiO and Ni particles, i.e., bright field image by transmission electron microscope, X-ray diffraction, scanning electron microscope, energy dispersive X-ray analysis, Fourier transform-infrared (FT-IR) study, and magnetic measurements by vibration sample magnetometer (VSM) are studied. The particles are observed to be superparamagnetic.
“…The reduction in a hydrogen atmosphere to produce high-purity nanoparticles from fine metal oxides is significant. [25][26][27][28][29][30][31] Regarding the application, the synthesis of particles with a definite shape, tailor-made size, and narrow size distribution may be the main goal with a definite composition either as a crystal or amorphous phase.…”
The synthesis of magnetic Ni nanoparticles is being investigated by the reduction of NiO nanoparticles in the presence of hydrogen gas. In this study, nanocrystalline NiO particles have been synthesized by a homogenous carbonate precipitation method employing nickel electrolyte (NiSO 4 ) as the source of nickel and ammonium hydrogen carbonate as the precipitating agent. Nickel electrolyte (NiSO 4 ) was obtained after processing of sea nodules by the roastingammonia leaching-solvent extraction method. The physicochemical characterization of NiO and Ni particles, i.e., bright field image by transmission electron microscope, X-ray diffraction, scanning electron microscope, energy dispersive X-ray analysis, Fourier transform-infrared (FT-IR) study, and magnetic measurements by vibration sample magnetometer (VSM) are studied. The particles are observed to be superparamagnetic.
“…In this work, we report on an alternative strategy of using hydrogen reduction of an electron beam‐exposed metal naphthenate resist film to form patterned metal lines of good integrity at the sub‐10 nm size scale. Although the reduction of metal oxides to the base metals (such as Ni, Co, Fe, Cu, Mo, and W) using hydrogen is well known,13–18 there have been no attempts to use this process in the fabrication of metal nanostructures. It has previously been observed, in studies of oxide‐hydrogen reaction kinetics, that nanometer‐scale‐grained pure metal and alloy films can be produced successfully 13.…”
Section: Introductionmentioning
confidence: 99%
“…Although the reduction of metal oxides to the base metals (such as Ni, Co, Fe, Cu, Mo, and W) using hydrogen is well known,13–18 there have been no attempts to use this process in the fabrication of metal nanostructures. It has previously been observed, in studies of oxide‐hydrogen reaction kinetics, that nanometer‐scale‐grained pure metal and alloy films can be produced successfully 13. The reduction of metal oxides to their respective metals by hydrogen is best understood by studying the principles of extractive metallurgy, and in particular, the Ellingham diagram of oxides 19.…”
The fabrication of very narrow metal lines by the lift‐off technique, especially below sub‐10 nm, is challenging due to thinner resist requirements in order to achieve the lithographic resolution. At such small length scales, when the grain size becomes comparable with the line‐width, the built‐in stress in the metal film can cause a break to occur at a grain boundary. Moreover, the line‐width roughness (LWR) from the patterned resist can result in deposited metal lines with a very high LWR, leading to an adverse change in device characteristics. Here a new approach that is not based on the lift‐off technique but rather on low temperature hydrogen reduction of electron‐beam patterned metal naphthenates is demonstrated. This not only enables the fabrication of sub‐10 nm metal lines of good integrity, but also of low LWR, below the limit of 3.2 nm discussed in the International Technology Roadmap for Semiconductors. Using this method, sub‐10 nm nickel wires are obtained by reducing patterned nickel naphthenate lines in a hydrogen‐rich atmosphere at 500 °C for 1 h. The LWR (i.e., 3 σLWR) of these nickel nanolines was found to be 2.9 nm. The technique is general and is likely to be suitable for fabrication of nanostructures of most commonly used metals (and their alloys), such as iron, cobalt, nickel, copper, tungsten, molybdenum, and so on, from their respective metal–organic compounds.
“…The reduction of iron-molybdenum oxides has been previously studied; however, the literature reports varied kinetic results, indicating the importance of analysis methods and experimental conditions [44][45][46][47][48]. Table 3 shows the apparent activation energies (E a ) reported in literature with the corresponding temperature range, experimental conditions, kinetic analysis methods, and proposed reaction mechanisms.…”
The reduction of the molecular iron-molybdenum-nanocluster, [H x , was studied using model free isoconversional methods. The reduction kinetics were evaluated using the nonisothermal thermogravimetric measurements at four different heating rates from 5 to 20°C/min in a 5% hydrogen atmosphere (argon balance). The apparent activation energy dependence on conversion derived from the isoconversional Kissinger-Akahira-Sunose (KAS) and Vyazovkin methods reveals a complex multi-step process with values ranging from 60.8 ± 13.3 to 183 ± 6.3 kJ/mol. The kinetic results were validated by isothermal predictions. The results herein are useful for optimization and development of FeMoC derived Fe-Mo nanoalloy systems.
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