Instytut Podstawowych Problemów Techniki

Streszczenie:

This work presents a synthesis of iron nanochains through magnetic-field-induced reduction reaction performed with sodium borohydride in water, ethanol and isopropanol. After their preparation, the nanomaterials obtained in three different processes are washed several times in ethanol and acetone to remove side-products. The performed cleaning step is very sufficient for water-based synthesis of iron nanochains. In contrary, the nanostructures obtained in ethanol and isopropanol contain a significant amount of sodium chlorides which is hard to dispose. Moreover, the use of ethanol and isopropanol solvents causes the reduction of nanochains’ diameters. Both the presence of sodium chlorides and the reduction of diameter size result in the decrease of saturation magnetization of iron nanochains and the increase of their coercivities.

Słowa kluczowe:

One-dimensional nanostructures, Iron nanochains, Magnetic materials, Magnetic-field-induced synthesis

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Streszczenie:

The main aim of this work was to use the iron–iron oxide nanochains (Fe NCs) as adsorbents of the carcinogenic cationic crystal violet (CV) and anionic Congo red (CR) dyes from water. The investigated adsorbent was prepared by a magnetic-field-induced reduction reaction, and it revealed a typical core–shell structure. It was composed of an iron core covered by a thin Fe3O4 shell (<4 nm). The adsorption measurements conducted with UV–vis spectroscopy revealed that 15 mg of Fe NCs constituted an efficient dose to be used in the CV and CR treatment. The highest effectiveness of CV and CR removal was found for a contact time of 90 min at pH 7 and 150 min at pH 8, respectively. Kinetic studies indicated that the adsorption followed the pseudo-first-order kinetic model. The adsorption process followed the Temkin model for both dyes taking into account the highest value of the R2 coefficient, whereas in the case of CR, the Redlich–Peterson model could be also considered. The maximal adsorption capacity estimated from the Langmuir isotherms for the CV and CR was 778.47 and 348.46 mg g–1, respectively. Based on the Freundlich model, both dyes adsorbed on the Fe NCs through chemisorption, but Coulombic interactions between the dye and adsorbent cannot be excluded in the case of the CV dye. The obtained results proved that the investigated Fe NCs had an excellent adsorption ability for both dye molecules within five cycles of adsorption/desorption, and therefore, they can be considered as a promising material for water purification and environmental applications.

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Streszczenie:

The zerovalent iron (Fe0) nanomaterials tend to be spontaneously oxidized in the presence of oxygen. This leads to the formation of interface composed of iron core and thin iron oxide shell. These structures are frequently observed with transmission electron microscope but, at the same time, it is hard to determine the precise structural and chemical composition of oxide shell. This feature is very important for possible applications of Fe0 nanostructures. Hence, the present work aims to deliver more detailed insights in this topic. The investigations are performed for the iron nanochains prepared in the magnetic-field-induce reduction of FeCl3 by NaBH4. The high-resolution transmission electron microscopy, electron energy loss spectroscopy, and x-ray photoemission spectroscopy confirm that the iron nanochains are covered by very thin oxide layer not exceeding over 3 nm. Moreover, the detailed XPS analyses of O 1s and Fe 2p lines indicate that the iron oxide shell reveals Fe3O4 nature. Moreover, this work demonstrated that some by-products of the reaction containing boron are presented in the sample even after a removal of the thin iron oxide shell by Ar+ treatment.

Słowa kluczowe:

iron nanochains, magnetic-field-induced synthesis, surface oxidation, x-ray photoemission spectroscopy

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Streszczenie:

A coupled process of ultrasonic spray pyrolysis and lyophilisation was used for the synthesis of dried gold nanoparticles. Two methods were applied for determining their melting temperature: uniaxial microcompression and differential scanning calorimetry (DSC) analysis. Uniaxial microcompression resulted in sintering of the dried gold nanoparticles at room temperature with an activation energy of 26–32.5 J/g, which made it impossible to evaluate their melting point. Using DSC, the melting point of the dried gold nanoparticles was measured to be around 1064.3°C, which is close to pure gold. The reason for the absence of a melting point depression in dried gold nanoparticles was their exothermic sintering between 712 and 908.1°C.

Słowa kluczowe:

gold nanoparticles, melting point, ultrasonic spray pyrolysis, characterisation

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Streszczenie:

Preparation and detailed structural characterization of iron-nickel wire-like nanochains with Fe0.75Ni0.25, Fe0.50Ni0.50, and Fe0.25Ni0.75 compositions are reported. The investigated nanomaterials were produced in the novel template-free magnetic-field-induced reduction reaction with NaBH4 as a reducing agent. It is demonstrated that this method leads to the formation of Fe-Ni nanochains composed of spherical nanoparticles with an average diameter of 50-70 nm and with a very high degree of atomic disorder manifested as the lack of clearly developed bcc and fcc phases, which are usually observed for nano- and polycrystalline Fe-Ni species. The recorded wide-angle X-ray scattering data for the obtained Fe-Ni nanochains exhibit a strong resemblance to those obtained for bulk metallic glasses. The atomic scale structure of the investigated nanochains has been studied using pair distribution function analysis of the recorded total scattering data. The best fits to the experimental pair distribution functions have been achieved assuming two-phase models of hcp and bcc networks with the size of coherently scattering regions of about 2.5 nm in diameter, for each Fe-Ni composition. Transmission electron microscopy images indicate that the glass-like bimetallic alloy cores are covered by amorphous oxide/hydroxide shells with thickness ranging from 2 to 5 nm. Moreover, electron energy loss spectroscopy, X-ray photoelectron spectroscopy, and Mössbauer spectroscopy results confirm the core-shell structure of the Fe-Ni nanochains and a complex character of shell layer which consists of several iron- and nickel-containing phases.

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