Instytut Podstawowych Problemów Techniki

Streszczenie:

The synthesis of magnetically-active nickel-yttrium oxide (Ni-Y2O3) nanocomposite particles is described in this work. The investigated material is produced with a modified ultrasound spray pyrolysis (USP) device which differs from a common USP setup in terms of use of three independently heating zones. They provide a direct feed of H2 to the second reaction zone and allow controlling the formation of the nanocomposite particles and facilitating their post-reaction stabilization with polyvinylpyrrolidone (PVP). According to the morphological and structural studies, the Ni-Y2O3 material takes a form of nanoparticles whose sizes are not homogeneously distributed as well as shapes are not smooth due to the successful formation of composite material with two interpenetrating phases. Moreover, the organic layer is detected on the surface of the nanoparticles which confirms the presence of PVP stabilizer. The magnetic investigations confirm that the Ni-Y2O3 nanocomposite reveals a spin glass-like behavior in which a collective freezing of magnetic moments might occur due to the interparticle interactions between Ni nanocrystallites presented in the sample.

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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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In order to use the infrared (IR) radiation shielding materials, they should take a form of thin film coatings deposited on glass/polymer substrates or be used as fillers of glass/polymer. The first approach usually suffers from several
technological problems. Therefore, the second strategy gains more and more attention. Taking into account this trend, this work presents the usage of iron nanoparticles (Fe NPs) embedded into the poly(vinylidene fluoride-co-hexafluoropropylene) (PVDF-HFP) films as the shielding material in near-infrared (NIR) and mid-infrared (MIR) region. The performed
investigations show that the transmittance of copolymer films decreases with
increasing content of the Fe NPs inside them. It is found that the average fade of IR transmittance for 1, 2.5, 5, 10, and 50 mg of Fe NPs is about 13%, 24%, 31%, 77%, and 98%, respectively. Moreover, it is observed that the PVDF-HFP films filled in the Fe NPs almost does not reflect the NIR and MIR radiation. Hence, the IR shielding properties of the PVDF-HFP films can be effectively tuned by the addition of proper amount of the Fe NPs. This, in turn, shows that the PVDF-HFP films filled in the Fe NPs constitute a great option for IR antireflective and shielding applications.

Słowa kluczowe:

antireflective materials, copolymer films, infrared radiation shielding materials, iron nanoparticles, nanofillers

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This work presents a growth of Fe3O4 nanoparticle films on silicon substrate. The iron oxide is deposited applying a pulsed laser deposition technique. The process is performed in open air in the absence and presence of external magnetic field. In fact, the morphologies of the obtained Fe3O4–Si samples are similar. The Fe3O4 nanoparticles are spherical with average diameters of 30 nm and are densely agglomerated on the Si substrate. The Fe3O4–Si material prepared in the absence of magnetic field has revealed more intense signals during X-ray diffraction and Raman measurements. The magnetic investigations indicate that the Fe3O4 nanoparticles are significantly coupled with the Si substrate and do not exhibit superparamagnetic behavior. Moreover, the Verwey transition is 98 K for both investigated Fe3O4–Si samples.

Słowa kluczowe:

Fe3O4 nanoparticles,magnetic materials,pulsed laser deposition

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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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This work presents the evolution of morphological, structural and magnetic properties of amorphous Fe-Ni wire-like nanochains caused by thermal oxidation. The initial Fe1−xNix samples (x = 0.75; 0.50; 0.25) were prepared through the magnetic-field-induced synthesis, and then they were heated in dry air at 400 °C and 500 °C. These treatments led to two competing simultaneous processes occurring in the investigated samples, i.e., (i) a conversion of amorphous material into crystalline material, and (ii) their oxidation. Both of them strictly affected the morphological and structural properties of the Fe-Ni nanochains which, in turn, were associated with the amount of iron in material. It was found that the Fe0.75Ni0.25 and Fe0.50Ni0.50 nanochains were covered during thermal treatment by the nanoparticle oxides. This coverage did not constitute a good barrier against oxidation, and these samples became more oxidized than the Fe0.25Ni0.75 sample which was covered by oxide nanosheets and contained additional Ni3B phase. The specific morphological evolutions of the Fe-Ni nanochains also influenced their saturation magnetizations, whereas their coercivities did not vary significantly. The obtained results constitute an important source of information for future application of the thermally treated Fe-Ni nanochains which could be applied in the energy storage devices or catalysis.

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Thermal treatment is a post-synthesis treatment that aims to improve the crystallinity and interrelated physical properties of as-prepared materials. This process may also cause some unwanted changes in materials like their oxidation or contamination. In this work, we present the post-synthesis annealing treatments of the amorphous Fe1−xCox (x = 0.25; 0.50; 0.75) Wire-like nanochains performed at 400 °C in two different atmospheres, i.e., a mixture of 80% nitrogen and 20% hydrogen and argon. These processes caused significantly different changes of structural and magnetic properties of the initially-formed Fe-Co nanostructures. All of them crystallized and their cores were composed of body-centered cubic Fe-Co phase, whereas their oxide shells comprised of a mixture of CoFe2O4 and Fe3O4 phases. However, the annealing carried out in hydrogen-containing atmosphere caused a decomposition of the initial oxide shell layer, whereas a similar process in argon led to its slight thickening. Moreover, it was found that the cores of thermally-treated Fe0.25Co0.75 nanochains contained the hexagonal closest packed (hcp) Co phase and were covered by the nanosheet-like shell layer in the case of annealing performed in argon. Considering the evolution of magnetic properties induced by structural changes, it was observed that the coercivities of annealed Fe-Co nanochains increased in comparison with their non-annealed counterparts. The saturation magnetization (MS) of the Fe0.25Co0.75 nanomaterial annealed in both atmospheres was higher than that for the non-annealed sample. In turn, the MS of the Fe0.75Co0.25 and Fe0.50Co0.50 nanochains annealed in argon were lower than those recorded for non-annealed samples due to their partial oxidation during thermal processing.

Słowa kluczowe:

annealing, amorphous materials, Fe-Co nanochains, magnetic-field-induced synthesis, wire-like nanostructure

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So far, it has been proven that the magnetic-field-induced (MFI) synthesis is a process which mainly leads to the formation of magnetic metallic one-dimensional nanostructures. Taking advantage of this method, the new procedures which allow manufacture of the magnetic bimetallic iron–cobalt wire-like nanochains with Fe0.75 Co0.25, Fe0.50 Co0.50, and Fe0.25 Co0.75 compositions are demonstrated in this work. They were produced through a simple one-step magnetic-field-induced (MFI) chemical co-reduction of three different mixtures containing a proper amount of Fe2+ and Co2+ ions with aqueous sodium borohydride solution as the reducing agent. The synthesis process was carried out at room temperature without the use of templates, surfactants, complexing agents, and organic solvents. The morphological and structural studies indicated that all as-prepared materials were amorphous, and they were composed of nanoparticles aligned in almost straight chains. Moreover, they revealed the core–shell structures with bimetallic alloy cores containing desired iron-to-cobalt ratios and very thin oxide shells. Furthermore, the obtained nanostructures behaved as ferromagnetic materials. Their magnetic properties were correlated with their structural properties and chemical compositions. It was observed that their saturation magnetization decreased significantly with increasing content of cobalt in the chains, whereas the variation of their coercivity was less pronounced.

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Manufacturing process of wire-like binary or ternary metal nanoalloys applying the magnetic-field-induced (MFI) synthesis is still a challenging task. Hence, this work demonstrates for the first time how to produce the iron-nickel wire-like nanostruc-tures with Fe0.75Ni0.25, Fe0.5Ni0.5 and Fe0.25Ni0.75 compositions. In a contrary to the previously reported synthesis of the Fe-Ni wire-like nanomaterials, this process has been carried out at room temperature without employment of templates, surfactants, organic solvents, and other chemical additives. The as-prepared samples exhibit specific structures with the amorphous bimetallic alloy cores covered by thin amorphous oxide shells. Moreover, they are composed of nanoparticles which are aligned in nearly linear chains. The Fe-Ni samples are ferromagnetic materials. Their coercivity values and saturation magnetizations depend on chemical compositions and dimensions of the investigated chains. The highest saturation magnetization and the lowest coercivity is found for the material with the lowest content of nickel and vice versa.

Słowa kluczowe:

amorphous materials, Fe–Ni chains, magnetic-field-induced synthesis, magnetic materials, wire-like nanostructure

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Streszczenie:

The magnetically-assisted growth of the amorphous bimetallic iron–nickel wire-like nanostructures is presented in this work. The applied process is based on a simple reduction reaction of aqueous solutions containing Fe2+ and Ni2+ ions with NaBH4 in the presence of an external magnetic field of about 0.05 T. The morphology, chemical composition, and magnetic properties of as-prepared Fe–Ni nanostructures have been determined by means of scanning electron microscopy, transmission electron microscopy, energy-dispersive X-ray spectroscopy, X-ray diffractometry, and vibrating sample magnetometry. The obtained experimental data indicate that the as-prepared samples exhibit quite complex architectures i.e., they comprise of nanoparticles aligned in almost straight lines. In addition, they reveal the typical core-shell structures where the amorphous bimetallic alloy cores are covered by thin amorphous oxide shells. In turn, the magnetic measurements show that the Fe–Ni wire-like nanostructures behave as typical ferromagnetic nanomaterials and their magnetic parameters like saturation magnetizations and coercivities are strictly dependent on their sizes and chemical compositions.

Słowa kluczowe:

amorphous materials, bimetallic nanostructures, magnetic-field-induced synthesis, magneticmaterials, wire-like nanostructures

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This work describes a use of a composite nanomaterial which consists of multiwall carbon nanotubes covered by iron oxide nanoparticles as a hybrid electrode in aqueous supercapacitor. The investigated nanomaterial was manufactured in a two-step simple chemical synthesis in which the first step was a functionalization of carbon nanotubes whereas the second one was the deposition of iron oxide. According the morphological and structural characterization, the carbon nanotubes with diameters of 10–40 nm were successfully covered by randomly-dispersed magnetite nanoparticles with average diameter of 10 nm. Moreover, the thermogravimetric analysis results indicated that the mass ratio between carbon nanotubes and iron oxide nanoparticles was about 65–35%. The electrochemical performance of studied hybrid electrode was tested in 1M aqueous KCl electrolyte. The highest specific capacitance of 143 F g^‒1 was recorded at a discharge current density of 1 A g^‒1. The investigated nanomaterial also exhibited excellent cycling stability i.e. 81% retention of the initial capacitance after 3000 cycles.

Słowa kluczowe:

hybrid electrode, magnetite, multiwall carbon nanotube, nanocomposite, supercapacitor

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The thermal treatment of chains composed of amorphous Fe 1–x Co x nanoparticles in two different oxygen atmospheres was studied. The nanostructures were manufactured using a magnetic-field-induced coreduction reaction, in which the precursor solutions containing 1:3 and 3:1 proportions of Fe 2+ and Co 2+ ions were reduced with sodium borohydride. The as-prepared nanochains were then heated for 30 min at 400 and 500 °C in dry air or argon containing about 1% oxygen. These processes led to their oxidation, and, as a result, the thermally treated Fe 1–x Co x nanochains were transformed into cobalt ferrite. Heating at 500 °C in the air-containing atmosphere caused the nanomaterials to lose their nanochain structures. In accordance to room-temperature magnetic measurements, the as-prepared and thermally treated Fe 1–x Co x nanochains were ferromagnetic. The highest saturation magnetization (Ms) was measured for the Fe 1–x Co x nanochains treated at 400 °C in dry air (105 A*m^2/kg and 154 A*m^2/kg for Fe 0.25 Co 0.75 and Fe 0.75 Co 0.25, respectively), whereas the lowest Ms was found for the Fe 0.25 Co 0.75 heated at 500 °C in dry air (17 A*m^2/kg) and the Fe 0.75 Co 0.25 heated at 500 °C in argon (16 A*m^2/kg).

Słowa kluczowe:

nanomagnetics, FeCo nanochains, magnetic-field-induced synthesis, thermal treatment

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The main objective of this work is to study the influence of thermal oxidation on the chemical composition and magnetic properties of iron nanoparticles which were manufactured in a simple chemical reduction of Fe3+ ions coming from iron salt with sodium borohydride. The annealing processing was performed in an argon atmosphere containing the traces of oxygen to avoid spontaneous oxidation of iron at temperatures ranging from 200 °C to 800 °C. The chemical composition and magnetic properties of as-prepared and thermally-treated nanoparticles were determined by means of X-ray diffractometry, Raman spectroscopy, Mössbauer spectroscopy and vibrating sample magnetometry. Due to the magnetic interactions, the investigated iron nanoparticles tended to create the dense aggregates which were difficult to split even at low temperatures. This caused that there was no empty space between them, which led to their partial sintering at elevated temperatures. These features hindered their precise morphological observations using the electron microscopy techniques. The obtained results show that the annealing process up to 800 °C resulted in a progressive change in the chemical composition of as-prepared iron nanoparticles which was associated with their oxidation. As a consequence, their magnetic properties also depended on the annealing temperature. For instance, considering the values of saturation magnetization, its highest value was recorded for the as-prepared nanoparticles at 1 T and it equals 149 emu/g, while the saturation point for nanoparticles treated at 600 °C and higher temperatures was not reached even at the magnetic field of about 5 T. Moreover, a significant enhancement of coercivity was observed for the iron nanoparticles annealed over 600 °C.

Słowa kluczowe:

Chemical composition, Chemical reduction, Iron nanoparticle, Magnetic properties, Oxidation

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This work describes the detailed studies performed on the nanocomposite composed of chemically-modified multiwall carbon nanotubes covered by hematite nanoparticles which diameters vary from 10 nm to 70 nm. This nanomaterial was fabricated in two-steps facile chemical synthesis and was characterized with the use of several experimental techniques, such as: thermogravimetric analysis, differential thermal analysis, Raman spectroscopy, X-ray diffraction, and transmission Mössbauer spectroscopy in order to determine its structure precisely. Moreover, the investigated nanocomposite was tested as an anode material of Li-ion batteries. Its cycling performance was stable during 40 cycles, while its capacity was retained at the level of 330 and 230 mAh/g at the discharge/charge rate of 25 and 200 mA/g, respectively.

Słowa kluczowe:

anode material, hematite, Li-ion battery, multiwall carbon nanotube, nanocomposite

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This work describes an oxidation process of iron–iron oxide core–shell nanowires at temperatures between 100°C and 800°C. The studied nanomaterial was synthesized through a simple chemical reduction of iron trichloride in an external magnetic field under a constant flow of argon. The electron microscopy investigations allowed determining that the as-prepared nanowires were composed of self-assembled iron nanoparticles which were covered by a 3 nm thick oxide shell and separated from each other by a thin interface layer. Both these layers exhibited an amorphous or highly-disordered character which was traced by means of transmission electron microscopy and Mössbauer spectroscopy. The thermal oxidation was carried out under a constant flow of argon which contained the traces of oxygen. The first stage of process was related to slow transformations of amorphous Fe and amorphous iron oxides into crystalline phases and disappearance of interfaces between iron nanoparticles forming the studied nanomaterial (range: 25–300°C). After that, the crystalline iron core and iron oxide shell became oxidized and signals for different compositions of iron oxide sheath were observed (range: 300–800°C) using X-ray diffraction, Raman spectroscopy and Mössbauer spectroscopy. According to the thermal gravimetric analysis, the nanowires heated up to 800°C under argon atmosphere gained 37% of mass with respect to their initial weight. The structure of the studied nanomaterial oxidized at 800°C was mainly composed of α-Fe2O3 (∼93%). Moreover, iron nanowires treated above 600°C lost their wire-like shape due to their shrinkage and collapse caused by the void coalescence.

Słowa kluczowe:

annealing, core-shell nanostructure, iron nanoparticles, iron nanowires, oxidation, thermal treatment

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This work presents the results of high temperature annealing of iron nanowires at five different temperatures (ranging 200–800 °C) in the slightly oxidative atmosphere. Investigated nanomaterial was prepared in simple chemical reduction process from aqueous solution of iron trichloride placed in external magnetic field. Experimental results allowed determining how magnetic properties of as-prepared as well as annealed iron nanowires change in respect to their structures. They also delivered information about phase transitions occurred in as-prepared sample under thermal treatment.

Słowa kluczowe:

annealing, iron, magnetic properties, nanowires

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Streszczenie:

The aim of this work is to study the preparation and characterization of a new nanocomposite which consists of chemically-modified multiwall carbon nanotubes covered by randomly-deposited nanoparticles of hematite. The morphology, structural and physical properties of the investigated nanomaterial were determined by means of transmission electron microscopy, X-ray diffraction and vibrating sample magnetometry at ambient conditions. The presence of residual catalyst nanospheres inside multiwall carbon nanotubes was confirmed by transmission electron microscopy. The signal coming from this contamination was under the detection limit of X-ray diffractometer, therefore it was not registered.

Słowa kluczowe:

Hematite, Multiwall carbon nanotubes, CVD, TEM, XRD, VSM

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Słowa kluczowe:

magnetic-field-induced process, magnetic material, nanoalloy, wire-like nanostructure

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