High coercivity magnetic multi-wall carbon nanotubes for low-dimensional high-density magnetic recording media

Fe-embedded multi-wall carbon nanotubes (MWCNTs) were fabricated using Fe-catalyst by the chemical deposition method. Microscopic characterizations showed that the well-aligned MWCNTs were ～ 80 mm in length, with outer diameter of 20–50 nm and inner diameter of 10–20 nm. Magnetic properties were characterized in temperatures of 5 K and 305 K, which revealed that the MWCNTs exhibited high coercivity of 2600 Oe at 5 K and 732 Oe at 305 K. These values are much higher than that of bulk iron (～ 0.9 Oe) and Fe/Co/Ni nanoparticles or nano-wire arrays (～ 200–500 Oe) at the room temperature. This high coercivity and the structure of single-domain Fe nanoparticles isolated by anti-ferromagnetic MWCNTs make it a promising candidate for low-dimensional high-density magnetic recording media.     

Synthesis of carbon nanofibers with a polygonal cross section by the catalytic decomposition of C2H2 over bi-metal catalysts

Carbon nanofibers with a polygonal cross section were synthesized using catalytic chemical vapor deposition over Fe–Sn, Ni–Sn or Co–Sn catalysts. Their morphologies were characterized by scanning and transmission electron microscopy. Edges connecting of two walls can be clearly observed and some adjacent walls have a V-shape. The lengths of the sides of the polygonal cross sections range from 150 to 500 nm over Fe–Sn or Co–Sn nanoparticles, increasing to 700–900 nm over Ni–Sn nanoparticles. Polygonal catalyst particles can be seen at the ends of the fibers.     

MnFe2O4 bulk,nanoparticles and film: A comparative study of structural and magnetic properties

MnFe₂O₄ bulk sample was synthesized by conventional solid state reaction method, at 1350 °C. Nanoparticles with mean size of 〈D〉_TEM=10.4(±1.1) nm were prepared by thermal decomposition of metal nitrates, at 350 °C. And a film sample was prepared by pulsed laser deposition of bulk ferrite on MgO(100) at substrate temperature of 600 °C. Then a comparative study of the structural and magnetic properties of the samples has been carried out using different measurements. X-ray diffraction pattern of bulk and nanoparticles samples confirmed formation of spinel phase. The film sample showed an epitaxial growth on MgO in (400) direction. Saturation magnetization of nanoparticles at 300 K, M_S=33 emu/g, was comparable with film sample, M_S=38 emu/g, both being ∼2.5 times smaller than that of bulk sample (M_S=82 emu/g). The results showed the importance of surface effects in the film sample and nanoparticles. The obtained zero coercivity of bulk sample at 300 K and the low value of 8 Oe at 5 K is attributed to soft magnetic behavior of the MnFe₂O₄. On the other hand, nanoparticles showed superparamagnetic behavior at 300 K; and blocked state with a large coercivity of 730 Oe at 5 K. The film sample showed non-zero corecivity at both 5 and 300 K which reveals higher magnetic anisotropy of film compared to the bulk ferrite.     

Morphology of cubic boron nitride crystals synthesized using (Fe,Co, Ni)–(Cr,Mo)–Al alloy solvents under pressure

The growth region of the cubic boron nitride (cBN) using (Fe, Ni)–Cr–Al and Co–(Cr, Mo)–Al solvents were presented in the pressure range of about 4–6 GPa and the temperature range between 1200 and 1700 °C. The minimum pressure for cBN formation was confirmed at about 4–4.1 GPa for both (Fe, Ni)–Cr–Al and Co–(Cr, Mo)–Al solvents. Based upon this pressure–temperature condition of the cBN growth region, the morphology of cubic boron nitride crystals was examined under various compositions of the solvents. The morphology of cBN crystals was affected by not only the reaction pressure and but also the composition of the solvents. It was found that the variation of alloy composition provides various morphologies and grain sizes of cBN crystals.     

Properties and rapid consolidation of nanostructured TiC-based hard materials with various binders by a high-frequency induction heated sintering

The densification of hard TiC–10 vol.% binder (Co, Ni, Fe) materials was accomplished within 2 min using a high-frequency induction heated sintering (HFIHS) method. The advantage of this process is not only rapid densification to almost the theoretical density but also the prevention of grain growth of the nano-structured materials. Highly dense TiC–binder (Co, Ni, Fe) composites with a relative density of up to 99.9% were obtained within 2 min by HFIHS under 80 MPa. The average grain size of TiC in the TiC–10 vol.% Ni composite was approximately 44 nm. The hardness and fracture toughness of the dense TiC–10 vol.% binder (Co, Ni, Fe) composite produced by HFIHS were also investigated.     

Novel method for synthesis of Fe core and C shell magnetic nanoparticles

Using a newly developed method, carbon-encapsulated iron (Fe) nanoparticles were synthesized by plasma due to ultrasonication in toluene. Fe core with carbon shell nanoparticles were characterized using Transmission Electron Microscopy (TEM) and High Resolution Transmission Electron Microscopy (HRTEM). Fe nanoparticles of diameter 7–115 nm are encapsulated by 7–8 nm thick carbon layers. There was no iron carbide formation observed between the Fe core and the carbon shell. The Fe nanoparticles have body centered cubic (bcc) crystal structure. Synthesized nanoparticles showed a saturation magnetization of 9 A m²/kg at room temperature. After thermal treatment crystalline order of the nanoparticles improved and saturation magnetization increased to 24 A m²/kg. We foresee that the carbon-encapsulated Fe nanoparticles are biologically friendly and could have potential applications in Magnetic Resonance Imaging (MRI) and photothermal cancer therapy.     

NiO/C nanocapsules with onion-like carbon shell as anode material for lithium ion batteries

The synthesis of NiO/C nanocapsules with NiO nanoparticles as the core and onion-like carbon layers as the shell is reported. The NiO/C nanocapsules deliver an initial discharge capacity of 1689.4 mAh g⁻¹ at 0.5 C and maintain a high reversible capacity of 1157.7 mAh g⁻¹ after 50 cycles compared to the NiO nanoparticles of 383.5 mAh g⁻¹. As an anode material for lithium ion batteries, the NiO/C nanocapsules exhibit a remarkable discharge capacity, a high rate charge–discharge capability and an excellent cycling stability. The improvements are ascribed to the fact that the onion-like carbon shells not only can provide enough voids to accommodate the volume change of NiO nanoparticles but also can prevent the formation of solid electrolyte interface (SEI) films on the surface of the NiO nanoparticles and hence the direct contact of Ni and SEI films upon lithium extraction.     

Onion-like carbon nanoparticles generated by multiple laser irradiations on laser-ablated particles

A one-step process to synthesize onion-like carbon nanoparticles at room temperature under atmospheric pressure was developed. Periodic pulsed laser irradiation of carbon nanoparticles confined in the cavity of a carbon target rod induces drastic changes to their structure, changing them from amorphous to ordered concentric graphitic shells. The size distribution of gas-borne nanoparticles measured by a scanning mobility particle sizer showed the mean mobility diameter decreased from 83 nm to 18 nm as a result of restructuring of carbon agglomerates. Polyhedral and unagglomerated nanoparticles with shell structures composed of multiple graphene sheets were observed by a transmission electron microscopy.     

Fabrication of porous carbon monoliths with a graphitic framework

Macro/mesoporous carbon monoliths with a graphitic framework were synthesized by carbonizing polymeric monoliths of poly(benzoxazine-co-resol). The overall synthesis process consists of the following steps: (a) the preparation of polymeric monoliths by co-polymerization of resorcinol and formaldehyde with a polyamine (tetraethylenepentamine), (b) doping the polymer with a metallic salt of Fe, Ni or Co, (c) carbonization and (d) the removal of inorganic nanoparticles. The metal nanoparticles (Fe, Ni or Co) formed during the carbonization step catalyse the conversion of a fraction of amorphous carbon into graphitic domains. The resulting carbon monoliths contain >50 wt.% of graphitic carbon, which considerably improves their electrical conductivity. The use of tetraethylenepentamine in the synthesis results in a nitrogen-containing framework. Textural characterization of these materials shows that they have a dual porosity made up of macropores and mesopores (∼2–10 nm), with a BET surface area in the 280–400 m² g⁻¹ range. We tested these materials as electrodes in organic electrolyte supercapacitors and found that no conductive additive is needed due to their high electrical conductivity. In addition, they show a specific capacitance of up to 35 F g⁻¹, excellent rate and cycling performance, delivering up to 10 kW kg⁻¹ at high current densities.     

Comparative investigation on the structural,morphological, optical,and magnetic properties of CoFe2O4 nanoparticles

Herein, we report a sustainable production of magnetic cobalt ferrite nanoparticles by conventional (CHM) and microwave heating (MHM) method. Hibiscus rosa-sinensis extract was used as both reducing and stabilizing agent. Using plant extracts to synthesize nanoparticles has been considered as an eco-friendly method, since it avoids noxious chemicals. The plethora of plant extract mediated nanoparticles were compared by techniques, such as XRD, Rietveld, FT-IR, SEM, EDX, UV-Visible DRS, PL and VSM were carried out to analyze and understand their crystallite size, functional groups, morphology, optical and magnetic properties. The crystalline structure of cobalt ferrite nanoparticles revealed the cubic structure and the microwave heating of nanoparticles showed smaller crystallite size compared to the conventional heating, which was then confirmed by XRD analysis. To analyze the presence of functional groups and the phytochemical involvement of the plant extract was confirmed by FT-IR studies. Spherical morphology with less than 100 nm sized particles was confirmed by SEM and EDX analysis confirm the existence of Co, O, and Fe elements present in the samples. UV-Visible DRS studies were carried out to calculate the band gap of the as-synthesized nanoparticles, estimated from the Kubelka-Munk function, as 2.06, and 1.87 eV for CHM and MHM, respectively. Photoluminescence emission spectrum of the nanoparticles showed two different bands at 494 and 620 nm, which explores the optical properties of the nanoparticles, due to the quantum confinement effect. VSM analysis showed better ferromagnetic behavior, which can be used for magnetic applications.     

High-pressure synthesis of cubic BN using Fe–Mo–Al and Co–Mo–Al alloy solvents

The pressure and temperature regions of cubic BN formation were determined using Fe–Mo–Al and Co–Mo–Al ternary alloys as synthetic solvents of cubic BN. The alloy compositions employed in the present study were (in weight percent) Fe60.14–Mo36.86–Al3 and Co57.6–Mo38.4–Al4. The cubic BN was successfully synthesized at minimum pressure of about 4.4 GPa and temperature of about 1250 °C. Pressure and temperature of cubic BN synthesis were decreased drastically by small amount of Al addition into Fe–Mo or Co–Mo alloy solvents. The growth of cubic BN was started at the interface between the molten alloy and the source hexagonal BN. In the present study, we proposed that Fe–Mo and Co–Mo work as solvent of B and N atoms and Al acts as a nucleation agent of cubic BN.     

Synthesis,structure and magnetic properties of spinel ferrite (Ni,Cu, Co)Fe2O4 from low nickel matte

Spinel ferrite (Ni, Cu, Co)Fe₂O₄ was synthesized from the low nickel matte by using a co-precipitation-calcination method for the first time. The influences of the added amount of NiCl₂·6H₂O, calcination temperature and time on the structure and magnetic properties of the as-prepared ferrites were studied in detail by X-ray diffraction (XRD), Scanning electron microscopy (SEM), Raman spectroscopy, and Vibrating sample magnetometer (VSM). It is indicated that pure (Ni, Cu, Co)Fe₂O₄ with cubic phase could be obtained under the experimental conditions (NiCl₂·6H₂O added amount of 3.0: 100 g mL⁻¹, calcination temperature from 800 to 1000 °C and calcination time from 1 to 3 h). With increasing calcination temperature and time, saturation magnetization (M_S) of the synthesized (Ni, Cu, Co)Fe₂O₄ increased and the coercivity (H_C) decreased. Under the optimum conditions (i.e. NiCl₂·6H₂O added amount of 3.0: 100 g mL⁻¹, 1000 °C, 3 h), the M_S and H_C values of the product were approximately 46.1 emu g⁻¹ and 51.0 Oe, respectively, which were competitive to those of other nickel ferrites synthesized from pure chemical reagents. This method explores a novel pathway for efficient and comprehensive utilization of the low nickel matte.     

Re-formation of metastable ε-Fe2O3 in post-annealing of Fe2O3/SiO2 nanostructure: Synthesis,computational particle shape analysis in micrographs and magnetic properties

Several Fe₂O₃/SiO₂ nanostructures were synthesized by the combination of the microemulsion and a sol-gel methods. Based on X-ray powder diffraction (XRD) and magnetic measurements (giant coercivity ~2.13 T) we identified ε-Fe₂O₃ (hard magnet) as the dominant crystalline phase. TEM analysis showed a wide size distribution of iron oxide nanoparticles (from 4 to 50 nm) with various morphologies (spherical, ellipsoidal and rod-like). We quantitatively described (computational analysis, MATLAB code) morphological properties of nanoparticles using the ellipticity of the shapes. The as-synthesized hard magnetic material was subjected to a post-annealing treatment at different temperatures (200, 500, 750, 1000 and 1100 °C) in order to investigate stability, formation and transformation of the ε-Fe₂O₃ polymorph. We found decreasing coercivity in the thermally treated samples up to the temperature of 750 °C (H_c=1245 Oe), followed by an observation of a surprising jump in coercivity H_C~1.5 T after post-annealing at 1000 °C. We conclude that the re-formation of the ε-Fe₂O₃ structure during post-annealing at 1000 °C is the origin of the observed phenomena. The phase transformation ε-Fe₂O₃→α-Fe₂O₃ and crystallization of amorphous silica in quartz and cristobalite were observed in the sample treated at 1100 °C.     

Synthesis of Co-Zr doped nanocrystalline strontium hexaferrites by sol-gel auto-combustion route using sucrose as fuel and study of their structural,magnetic and electrical properties

Sol-gel auto-combustion route using sucrose as fuel has been employed to synthesize nanocrystalline particles of SrZr_xCo_xFe_(12−2x)O₁₉ (0.0≤ x ≤1.0). The characterization of these materials has been done by TGA-DTA, FT-IR, XRD and EDS. SEM and TEM techniques have been used to study the structure and morphology. Magnetic properties have been investigated by VSM and Mössbauer spectroscopy (MS). The influence of calcination temperature on morphology and magnetic properties of samples is studied in a wide temperature range of 500–1100 °C. XRD analysis indicates the formation of pure single phase hexagonal ferrites at 900 °C. The crystallite size calculated using Scherrer equation lies in a narrow range of 21–33 nm. The crystallite size is small enough to obtain a suitable signal to noise ratio in high density recording medium. Substitution of Zr and Co for Fe has been found to have a profound effect on the structural, magnetic and electrical properties. Upon substitution saturation magnetization (M_S) first increases from 62.67 emu/g to 64.84 emu/g (up to x=0.4) followed by a decrease to 49.71 emu/g at x=1.0. There is a slow fall in coercivity (H_C) from 5785.74 (x=0.0) to 1796.51 Oe (x=1.0). Dielectric constant, dielectric loss tangent and AC conductivity in the frequency range 20 Hz to 120 MHz have been studied for all the compositions (x=0–1.0). The composition and frequency dependence of these dielectric parameters has been qualitatively explained.     

Synthesis of (Ni,Mn,Co)O4 nanopowder with single cubic spinel phase via combustion method

(Ni,Mn,Co)O₄ nanopowders with single cubic phase were successfully synthesized using combustion methods. Particle size of the as-burnt nanopowders after combustion was about 20 nm. Crystallization behavior of the NMC was investigated using various techniques such as X-ray diffraction (XRD), thermogravimetric (TG), Fourier transform infrared (FT-IR) spectroscopy, and transmission electron microscopy (TEM). Calcination at different temperature from 400 °C to 700 °C provides the powders with increased crystallinity and grain size. However, further increasing temperature above 800 °C for calcination, cubic spinel phase of NMC partly transformed to tetragonal spinel phase, which implies that cubic spinel phase of NMC nanopowder synthesized by combustion method becomes unstable above 800 °C.     

Synthesis and characterization of NiO and Ni nanoparticles using nanocrystalline cellulose (NCC) as a template

In this study, nanosized nickel oxide (NiO) and nickel (Ni) powders were synthesised via glycine-nitrate (GN) combustion process, assisted by nanocrystalline cellulose (NCC) as a template. Despite the unique morphology of NCC, it has yet to be applied as a sacrificial bio-template for GN combustion process. In addition, NiO and Ni nanoparticles were obtained at relatively low temperatures in this study, whereby the calcination temperatures were varied from 400 °C to 600 °C, with calcination durations of 2, 4, and 6 h. The morphological analysis of the resulting products were conducted using FESEM, which showed uniformly dispersed NiO and Ni particles with average crystallite size of 25 nm and 27 nm, respectively. These results were confirmed using X-ray diffraction (XRD) technique. The Raman and Fourier transform infrared (FTIR) spectra revealed that the molecular fingerprints of the samples were in agreement with each other. Further analyses revealed that samples calcined at 600 °C for 4 h showed the lowest particle size for pure NiO, whereas the lowest particle size for pure Ni was obtained at 400 °C for 4 h. The TGA results were also consistent with the XRD analysis, whereby pure Ni was initially formed and upon heating, had gradually converted into NiO.     

Chemical synthesis of TiO2 nanoparticles and their inclusion in Ni–P electroless coatings

The work addresses the preparation of Ni3P3TiO₂ nanocomposite coatings on mild steel substrate by the electroless technique. Nanosized TiO₂ particles were first synthesized by the precipitation method and then were codeposited (4 g/l) into the Ni3P matrix using alkaline hypophosphite reduced EL bath. The surface morphology, particle size, elemental composition and phase analysis of as-synthesized TiO₂ nanoparticles and the coatings were characterized by field emission scanning electron microscopy (FESEM), energy-dispersive analysis of X-ray (EDAX) and X-ray diffraction (XRD). Coatings with 20 µm thickness were heat treated at 400 °C for 1 h in argon atmosphere. The morphology, microhardness, wear resistance and friction coefficient characteristics (ball on disc) of electroless Ni3P3TiO₂ nanocomposite coatings were determined and compared with Ni3P coatings. The results show that as-synthesized TiO₂ nanoparticles are spherical in shape with a size of about12 nm. After heat treatment, the microhardness and wear resistance of the coatings are improved significantly. Superior microhardness and wear resistance are observed for Ni3P3TiO₂ nanocomposite coatings over Ni3P coatings.     

Synthesis of La1−xSrxMO3 (M = Mn,Fe, Co,Ni) nanopowders by alanine-combustion technique

La_1?xSr_xMO₃ (M = Mn, Fe, Co, Ni, x = 0–0.3) powders were obtained by solution combustion technique using metal nitrates and α-alanine. The as-prepared powders, resulted by the combustion reaction, were annealed at different temperatures to investigate the evolution of crystalline phases. For the strontium-doped lanthanum-based perovskites, higher annealing temperatures than for the corresponding pure lanthanum-based perovskites are needed to obtain single-phase compounds depending on M-site metal and strontium content. The oxide powders were investigated by FT-IR spectra, X-ray diffraction (XRD), scanning electron microscopy (SEM) and specific area measurements. Based on our results we propose different mechanisms for La_1?xSr_xMO₃ (M = Mn, Fe, Ni, x = 0–0.3) obtaining, depending on the intermediary compounds formed in the combustion reaction or during the thermal treatment of the as-prepared powders.     

Easy synthesis of ordered mesoporous carbon containing nickel nanoparticles by a low temperature hydrothermal method

Ordered mesoporous carbons (OMCs) with embedded metallic nickel (Ni) nanoparticles have been directly synthesized by a simple and low temperature (50 °C) hydrothermal method. The synthesis involved the use of a triblock copolymer Pluronic F127 as the mesostructure directing agent, resorcinol (R) and formaldehyde (F) as carbon precursors, and Ni(NO₃)₂·6H₂O as nickel source. It consisted in the self-assembly of F127, Ni²⁺ salt and RF polymer in an acidic medium and further carbonization, where the Ni²⁺ was captured by the network of F127/RF and further reduced into metallic Ni nanoparticles. The resultant Ni/carbon materials were characterised by X-ray diffraction, thermogravimetric analysis, transmission electron microscopy and nitrogen sorption. Ni/carbon materials with a highly ordered mesostructure were obtained using equal moles of resorcinol and formaldehyde molar ratio (R/F = 1/1), whereas an excess amount of formaldehyde (R/F = 1/2) was found to not form an ordered carbon structure. The results showed that nickel particles, with sizes of ∼10–50 nm, were homogeneously dispersed in the carbon matrices, while the pore mesostructure remained intact. The homogeneous Ni/carbon composites synthesized by this easy hydrothermal route have been demonstrated to be effective molecular adsorbents for magnetic separation.     

Hydrogenation of carbon monoxide to methane over mesoporous nickel-M-alumina (M = Fe,Ni, Co,Ce, and La) xerogel catalysts

Mesoporous nickel(30 wt%)-M(10 wt%)-alumina xerogel (30Ni10MAX) catalysts with different second metal (M = Fe, Ni, Co, Ce, and La) were prepared by a single-step sol–gel method for use in the methane production from carbon monoxide and hydrogen. In the methanation reaction, yield for CH₄ decreased in the order of 30Ni10FeAX > 30Ni10NiAX > 30Ni10CoAX > 30Ni10CeAX > 30Ni10LaAX. Experimental results revealed that CO dissociation energy of the catalyst and H₂ adsorption ability of the catalyst played a key role in determining the catalytic performance of 30Ni10MAX catalyst in the methanation reaction. Optimal CO dissociation energy of the catalyst and large H₂ adsorption ability of the catalyst were favorable for methane production. Among the catalysts tested, 30Ni10FeAX catalyst with the most optimal CO dissociation energy and the largest H₂ adsorption ability exhibited the best catalytic performance in terms of conversion of CO and yield for CH₄ in the methanation reaction. The enhanced catalytic performance of 30Ni10FeAX was also due to a formation of nickel–iron alloy and a facile reduction.