Synthesis and spectroscopic investigations of Mn3O4 nanoparticles

Trimanganese tetraoxide (Mn₃O₄) nanoparticles have been synthesized via hydrothermal process. Nevertheless, homogeneous nanoparticles of Mn₃O₄ with platelet lozange shape were obtained. The crystallite size ranged from 40 to 70 nm. The Mn₃O₄ product was investigated by X-ray diffraction, transmission electron microscopy (MET), and impedance spectroscopy. Electrical conductivity measurements showed that the as-synthesized Mn₃O₄ nanomaterial has a conductivity value which goes from 1.8 10⁻⁷ Ω⁻¹ cm⁻¹ at 298 K, to 23 10⁻⁵ Ω⁻¹ cm⁻¹ at 493 K. The temperature dependence of the conductivity between 298 and 493 K obeys to Arrhenius law with an activation energy of 0.48 eV.     

Microwave assisted fast fabrication of Fe3O4-MWCNTs nanocomposites and their application as MRI contrast agents

Uniform Fe₃O₄ nanoparticles with diameters of 3-5 nm are successfully decorated onto the external walls of multiwall carbon nanotubes (MWCNTs) by in situ high-temperature decomposition of Fe(acac)₃ in polyol solution under the irradiation of microwave. With this method, reaction time of forming Fe₃O₄-MWCNTs nanocomposites has been significantly shortened to 15 min. The resulting Fe₃O₄-MWCNTs nanocomposites show superparamagnetic property at room temperature and can be remained as stable aqueous dispersion for 2 months. Longitudinal relaxivity (r₁) and transverse relaxivity (r₂) of the magnetic MWCNTs are 8.34 Fe mM⁻¹ S⁻¹ and 146 Fe mM⁻¹ S⁻¹ respectively. The much higher r₂ value and the obvious change in the gray scale of MR images confer the Fe₃O₄-MWCNTs nanocomposites as potential candidates for T₂-weighted MRI contrast agents.     

Strong adsorption of chlorotetracycline on magnetite nanoparticles

In this work, environmentally friendly magnetite nanoparticles (Fe₃O₄ MNPs) were used to adsorb chlorotetracycline (CTC) from aqueous media. Fe₃O₄ MNPs exhibit ultrahigh adsorption ability to this widely used antibiotic. The adsorption behavior of CTC on Fe₃O₄ MNPs fitted the pseudo-second-order kinetics model, and the adsorption equilibrium was achieved within 10 h. The maximum Langmuir adsorption capacity of CTC on Fe₃O₄ (476 mg g⁻¹) was obtained at pH 6.5. Thermodynamic parameters calculated from the adsorption data at different temperature showed that the adsorption reaction was endothermic and spontaneous. Low concentration of NaCl and foreign divalent cations hardly affected the adsorption. Negative effect of coexisting humic acid (HA) on CTC adsorption was also observed when the concentration of HA was lower than 20 mg L⁻¹. But high concentration of HA (>20 mg L⁻¹) increased the CTC adsorption on Fe₃O₄ MNPs. The matrix effect of several environmental water samples on CTC adsorption was not evident. Fe₃O₄ MNPs were regenerated by treatment with H₂O₂ or calcination at 400 °C in N₂ atmosphere after separation from water solution by an external magnet. This research provided a high efficient and reusable adsorbent to remove CTC selectively from aqueous media.     

Self-controlled growth of Fe3BO6 crystallites in shape of nanorods from iron-borate glass of small templates

Fe₃BO₆ can be an ideal compound for devising functional magnetic and dielectric properties in a single material for multiple applications such as electrodes, gas sensors, or medical tools. Useful to tailor such properties, here we report on a self-controlled Fe₃BO₆ growth in a specific shape of nanorods from a supercooled liquid precursor (an inorganic polymeric liquid or glass) of an initial composition (100 − x)B₂O₃ − xFe₂O₃, x = 40–50 mol%. B₂O₃ as a strong glass former co-bridges the Fe³⁺ ions in oxygen polygons primarily in a 2-D interconnected polymer network so that it dictates preferably a 1-D directional growth on the reaction Fe³⁺ species in form of a compound Fe₃BO₆, a favorable phase to nucleate and grow when annealing a precursor at 500–800 °C in ambient air. Distinct nanorods with a diameter ∼200 nm and 40–100 μm length have been formed on 10–15 min annealing a sample in microwave at moderate temperature 550 °C. A bonded surface B₂O₃ layer (15–25 nm thickness) has grown on the Fe₃BO₆ of the nanorods in situ in a specific structure. XPS bands in the Fe³⁺, B³⁺ and O²⁻ species confer this model structure. A local BO₃ → BO₄ conversion has incurred in the boroxol (B₃O_4.5)_n, n → ∞, rings in the surface layer, showing three distinct IR bands at 1035, 1215 and 1425 cm⁻¹.     

Preparation of Fe3O4/PVA nanofibers via combining in-situ composite with electrospinning

A novel approach, combining in-situ composite method with electrospinning, was used to prepare high magnetic Fe₃O₄/poly(vinyl alcohol) (PVA) composite nanofibers. Fe₃O₄ magnetic fluids were synthesized by chemical co-precipitation method in the presence of 6 wt.% PVA aqueous solution. PVA was used as stabilizer and polymeric matrix. The resulting Fe₃O₄/PVA composite nanofibers were characterized with field emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM) and X-ray diffractometer (XRD), respectively. These composite fibers showed a uniform and continuous morphology, with the Fe₃O₄ nanoparticles embedded in the fibers. Magnetization test confirmed that the composite fiber showed a high saturated magnetization (M_s = 2.42 emµ·g^-1) although only 4 wt.% content.     

Structural,optical and electrical properties of In4Sn3O12 films prepared by pulsed laser deposition

Highly conducting (σ ∼ 2.6 × 10³ Ω⁻¹ cm⁻¹) In₄Sn₃O₁₂ films have been deposited using pulsed laser deposition (PLD) on glass and quartz substrates held at temperatures between 350 and 550 °C under chamber pressures of between 2.5 and 15 mTorr O₂. The crystallinity and the surface roughness of the films were found to increase with increasing substrate temperature. Electron concentrations of the order of 5 × 10²⁰ cm⁻³ and mobilities as high as 30 cm² V⁻¹ s⁻¹ were determined from Hall effect measurements performed on the films. Fitting of the transmission spectral profiles in the ultra-violet–visible spectrum has allowed the determination of the refractive index and extinction coefficient for the films. A red-shift in the frequency of plasmon resonance is observed with both increasing substrate temperature and oxygen pressure. Effective masses have been derived from the plasma frequencies and have been found to increase with carrier concentration indicating a non-parabolic conduction band in the material In₄Sn₃O₁₂. The optical band-gap has been determined as 3.8 eV from the analysis of the absorption edge in the UV. These results highlight the potential of these films as lower In-content functional transparent conducting materials.     

Low temperature synthesis of Fe3O4 nanoparticles and its application in lithium ion batteries

Well dispersed Fe₃O₄ nanoparticles with mean size about 160 nm are synthesized by a simple chemical method at atmosphere pressure. The products are characterized by X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM), and Raman spectrum. Electrochemical properties of the as-synthesized Fe₃O₄ nanoparticles as anode electrodes of lithium ion batteries are studied by conventional charge/discharge tests, showing initial discharge and charge capacities of 1140 mAh g⁻¹ and 1038 mAh g⁻¹ at a current density of 0.1 mA cm⁻². The charge and discharge capacities of Fe₃O₄ electrode decrease along with the increase of cycle number, arriving at minimum values near the 70th cycle. After that, the discharge and charge capacities of Fe₃O₄ electrode begin to increase along with the increase of cycle number, arriving at 791 and 799 mAh g⁻¹ after 393 cycles. The morphology and size of the electrode after charge and discharge tests are characterized by SEM, which exhibits a large number of dispersive particles with mean size about 150 nm.     

Enhanced thermoelectric properties of NaCo2O4 by adding ZnO

The primary phase present in the as-sintered Na(Co_1 − xZn_x)₂O₄ (0 ≤ x ≤ 0.1) bodies was the solid solution of the constituent oxides with a bronze-type layered structure. The electrical conductivity of the Na(Co_1 − xZn_x)₂O₄ samples significantly increased with an increase in ZnO content. The sign of the Seebeck coefficient for all samples was positive over the whole temperature range (723-1073 K), i.e., p-type conduction. The power factor of Na(Co_0.95Zn_0.05)₂O₄ showed an outstanding power factor (1.7 × 10^− 3Wm^− 1 K^− 2) at 1073 K. The power factor was above four times superior to that of ZnO-free NaCo₂O₄ (0.4 × 10^− 3Wm^− 1 K^− 2). This originates from an unusually large Seebeck coefficient (415 μVK^− 1) accompanied with high conductivity (127Ω^− 1 cm^− 1) at 1073 K.     

An easy fabrication of monodisperse oleic acid-coated Fe3O4 nanoparticles

An easy route is described for the synthesis of monodisperse oleic acid-coated Fe₃O₄ nanoparticles with uniform size and shape via a thermal decomposition of Fe(acac)₃ in the presence of oleic acid (OA). The prepared Fe₃O₄ samples are characterized by X-ray diffraction, transmission electron microscopy, Fourier transform infrared spectrometry, and vibrating sample magnetometer. The results show that the resulting OA-coated Fe₃O₄ nanoparticles have an average diameter of about 24 nm and an OA layer, around 3 nm in thickness. The magnetic saturation value of the prepared OA-coated Fe₃O₄ nanoparticles is determined to be 78.68 emu/g, indicating a well-established superparamagnetic property.     

Effect of chromium substitution on structure and magnetic properties of Bi2Fe4O9

Orthorhombic Bi₂Fe_4 − xCr_xO₉ (x = 0.0, 0.25, and 0.75) nanoplatelets were synthesized by a simple hydrothermal method. The structure, morphology, and magnetic properties of the obtained powders have been characterized. Calculation of the lattice parameters of Bi₂Fe_4 − xCr_xO₉, as well as bond lengths and angles, was carried out by X-ray diffraction Rietveld refinement. The volumes of the metal-oxygen tetrahedra and octahedra were calculated to be sequentially increasing as the Cr doping level increases. The samples undergo an antiferromagnetic transition at 250 ± 5 K. The magnetic moments of the samples increase with higher Cr doping level. The 3d electron spin state for Fe³⁺ in the as-prepared samples is different, which is possibly due to the distortion of Fe-O tetrahedra and octahedra in the crystal structure after chromium substitution.     

New heat generation material in AC magnetic field for Y3Fe5O12-based powder material synthesized by reverse coprecipitation method

We found the most promising powder material for the application of the thermal coagulation therapy for the treatment of cancerous tissues. The maximum heat generation ability (ΔT = 40-77 °C, 370 kHz, 1.77 kA·m^− 1) was obtained for the powder materials by the calcination at 1100 °C for the Y_3 − XGd_XFe₅O₁₂ system. This ΔT value is higher than ca. ΔT = 30 °C in same magnetic field for fine FeFe₂O₄ particles as the candidate material for this type of therapy. The particle growth with the formation of the cubic single phase might influence to the high heat generation. As an unexpected result, the Gd₃Fe₅O₁₂ (X = 3) has no heat generation ability in an AC magnetic field.     

Synthesis and electrochemical properties of Ti doped Li3 − xFe2 − xTix(PO4)3/C cathode materials

Li_3 − xFe_2 − xTi_x(PO₄)₃/C (x = 0-0.4) cathodes designed with Fe doped by Ti was studied. Both Li₃Fe₂(PO₄)₃/C (x = 0) and Li_2.8Fe_1.8Ti_0.2(PO₄)₃/C (x = 0.2) possess two plateau potentials of Fe³⁺/Fe²⁺ couple (around 2.8 V and 2.7 V vs. Li⁺/Li) upon discharge observed from galvanostatic charge/discharge and cyclic voltammetry. Li_2.8Fe_1.8Ti_0.2(PO₄)₃/C has higher reversibility and better capacity retention than that of the undoped Li₃Fe₂(PO₄)₃/C. A much higher specific capacity of 122.3 mAh/g was obtained at C/20 in the first cycle, approaching the theoretical capacity of 128 mAh/g, and a capacity of 100.1 mAh/g was held at C/2 after the 20th cycle.     

Crystal structure and ferroelectric properties of Ca(Cu3−xMx)Ti4O12 (M = Fe and Ni) ceramics

M-substituted Ca(Cu_3−xM_x)Ti₄O₁₂ (CCMTO) ceramics, where M = Fe and Ni, were synthesized and the influence of M substitutions for Cu on the crystal structure and ferroelectric properties of CCMTO ceramics were investigated in this study. From the variations in the lattice parameters of CCMTO ceramics, the solubility limit of Ni substitution for Cu in CaCu_3−xNi_xTi₄O₁₂ (CCNTO) ceramics was x = 0.2, whereas that of CaCu_3−xFe_xTi₄O₁₂ (CCFTO) ceramics was x = 0.05. The crystal structural analysis of CCMTO ceramics revealed that the single phase of CCMTO ceramics belongs to the I23 non-centrosymmetric space group of I23; as a result, the P_r and E_c values of CCFTO ceramics at x = 0.05 were 1.8 μC/cm² and 40 kV/cm, respectively. The ferroelectric behavior of CCMTO ceramics by the M substitutions for Cu may be related to the displacement of a Ti⁴⁺ cation in the TiO₆ octahedra and tilting of the Ti–O–Ti angle because of the non-centrosymmetric space group.     

Facile synthesis and electrochemical properties of Mn3O4 nanoparticles with a large surface area

Mn₃O₄ nanoparticles were prepared by a novel oxidation-precipitation method at a low temperature. The crystal phase, microstructure, surface area and electrochemical properties of the products were characterized by X-ray diffraction (XRD), high-resolution transmission electron microscopy (HRTEM), N₂ adsorption-desorption isotherms and cyclic voltammetry (CV). The results indicate that the addition of citric acid and tartaric acid remarkably reduced the particle size and increased the specific surface area of Mn₃O₄ nanoparticles. The samples prepared by the addition of citric acid and tartaric acid have a narrow particle size distribution of 5-10 nm, a surface area of 119 and 122 m²/g, and a capacitance of 171 and 172 F g⁻¹, respectively.     

Observation of broadband infrared luminescence in a novel Bi-doped P2O5-B2O3-Al2O3 glass

A novel Bi-doped P₂O₅-B₂O₃-Al₂O₃ glass was investigated, and strong broadband NIR (near infrared) luminescence was observed when the sample was excited by 445 nm, 532 nm, 808 nm and 980 nm lasers, respectively. The max FWHM with 312 nm, the lifetime with 580 μs and the σ_emτ product with 5.3 × 10^− 24 cm² s were obtained which indicates that this glass is a promising material for broadband optical amplifier and tunable laser. The effect of the introduction of B₂O₃ on the glass structure and Bi-ions illuminant mechanism were discussed and analyzed. It is suggested that the introduction of B₂O₃ makes the glass structure closer, and the broadband NIR emission derives from Bi⁰:²D_3/2 → ⁴S_3/2 and Bi⁺:³P₁ → ³P₀ transitions.     

A true nanocomposite: Single crystalline Au nanoparticles on single crystalline Fe3O4 nanoparticles

An Au/Fe₃O₄ nanocomposite catalyst was fabricated through a simple deposition-precipitation method. The Au/Fe₃O₄ nanocomposite is a true nanocomposite that has single crystalline Au nanoparticles supported on single crystalline Fe₃O₄ nanoparticles. Lattice fringes from both Au and Fe₃O₄ single nanoparticles were simultaneously observed by transmission electron microscope (TEM). This nanocomposite catalyst showed much high activity in low temperature CO oxidation reaction. The Au/Fe₃O₄ nanocomposite catalyst reaches 100% CO conversion at 40 °C. In comparison, Au/commercial Fe₃O₄ catalyst needs 375 °C to convert CO. This Au/Fe₃O₄ nanocomposite is an ideal sample to study synergetic effect between the catalyst and the support at nanoscale.     

Chemical diffusion coefficient of lithium ion in Li3V2(PO4)3 cathode material

The kinetic properties of monoclinic lithium vanadium phosphate were investigated by potential step chronoamperometry (PSCA) and electrochemical impedance spectroscopy (EIS) method. The PSCA results show that there exists a linear relationship between the current and the square root of the time. The D?_Li values of lithium ion in Li_3-xV₂(PO₄)₃ under various initial potentials of 3.41, 3.67, 3.91 and 4.07 V (vs Li/Li⁺) obtained from PSCA are 1.26 × 10^− 9, 2.38 × 10^− 9, 2.27 × 10^− 9 and 2.22 × 10^− 9 cm²·s^− 1, respectively. Over the measuring temperature range 15-65 °C, the diffusion coefficient increased from 2.67 × 10^− 8 cm²·s^− 1 (at 15 °C) to 1.80 × 10^− 7 cm²·s^− 1 (at 65 °C) as the measuring temperature increased.     

Properties of La-substituted Na0.5Bi4.5Ti4O15 ferroelectric thin films

Ferroelectric Na_0.5La_0.5Bi₄Ti₄O₁₅ (NaLaBTi) thin films were prepared by a chemical solution deposition method. The NaLaBTi thin films annealed at 750 °C under oxygen atmosphere were randomly oriented polycrystalline. Electrical properties of the NaLaBTi thin films were compared to Na_0.5Bi_4.5Ti₄O₁₅ thin films and better properties were observed in the NaLaBTi thin films. Remnant polarization (2P_r) and coercive electric field (2E_c) were 43 µC/cm² and 204 kV/cm at an applied electric field of 478 kV/cm, respectively. Leakage current density was 1.95 × 10^− 6 A/cm² at 100 kV/cm. Dielectric constant and dielectric loss were 805 and 0.05 at 1 kHz, respectively. Switchable polarization was suppressed by 15% after 1.44 × 10¹⁰ switching cycles.     

Growth and spectral properties of Cr:KAl(MoO4)2 crystal

The Cr³⁺:KAl(MoO₄)₂ single crystal was grown by top seeding solution growth method (TSSG). Based on the absorption and emission spectra, the crystal field strength Dq, the Racah parameters B and C, the effective phonon energy ?ω and the Huang-Rhys factor S were calculated: Dq = 1494.8 cm^− 1, B = 585.5 cm^− 1 and C = 3049 cm^− 1, ?ω = 373.8 cm^− 1 and the Huang-Rhys factor S = 3.74, respectively. The value Dq/B = 2.55 indicates that Cr³⁺ ion occupies the strong crystal field site in KAl(MoO₄)₂ crystal. A comparison of crystal field parameters for Cr³⁺:KAl(MoO₄)₂ with other Cr³⁺-doped crystals was presented. The results of spectral measurement show that Cr³⁺:KAl(MoO₄)₂ may be a potential candidate for broadband laser applications.     

Synthesis and characteristics of the C12A7-O nanoparticles by citric acid sol-gel combustion method

In this study, the O⁻-containing nanocrystal 12CaO·7Al₂O₃ (C12A7-O⁻) was synthesized by the citric acid sol-gel combustion method. The formation of the C12A7-O⁻ material was investigated via X-ray diffraction, thermogravimetric analysis, differential thermal analysis, electron paramagnetic resonance, field emission-scanning electron microscopy, and time of flight mass spectroscopy. The C12A7-O⁻ material was formed at a lower synthesis temperature (900-1150 °C), with a narrower particle size (33-74 nm). The anionic species stored in the C12A7 material was dominated by the active atomic oxygen anions (O⁻) with a concentration of (1.2 ± 0.3) × 10²⁰ cm^− 3, and the emission current density of O⁻ was about 0.89 ± 0.15 μA/cm² at T_{(sample surface)} = 800 °C and E_{(extraction field)} = 800 V/cm.