XRD,impedance, and Mössbauer spectroscopy study of the Li<Subscript>3</Subscript>Fe<Subscript>2</Subscript>(PO<Subscript>4</Subscript>)<Subscript>3</Subscript> + Fe<Subscript>2</Subscript>O<Subscript>3</Subscript> composite for Li ion batteries

The synthesis procedure of the Li₃Fe₂(PO₄)₃?+?Fe₂O₃ composite is presented. The monoclinic (A type) and hematite phases were detected by X-ray diffraction after the synthesis of the composite. The structural α–β (at a temperature of 460 K) and β–γ (at a temperature of 523 K) phase transitions in the composite were indicated by the anomalies of the electrical conductivity, dielectric permittivity, and changes of activation energies of conductivity. Two phase transitions have been detected in the Li₃Fe₂(PO₄)₃?+?Fe₂O₃ composite by ⁵⁷Fe Mössbauer spectroscopy: the phase transition in Li₃Fe₂(PO₄)₃ from the paramagnetic to antiferromagnetic phase at temperature T _N?=?29.5 K and the Morin phase transition in Fe₂O₃ at temperature T _M?=?235 K.     

Nanostructural inhomogeneity of EuBa<Subscript>2</Subscript>Cu<Subscript>3</Subscript>O<Subscript>6 + δ</Subscript> superconductors

Samples of high-temperature superconducting oxide EuBa₂Cu₃O_{6 + δ} (Eu-123) with total cationic composition Eu: Ba: Cu = 1: 2: 3 are investigated by means of local X-ray microanalysis and high-resolution transmission electron microscopy. The cationic nonstoichiometry of Eu-123 oxide is revealed. The particles of the studied samples are inhomogeneous in structure on the nanoscale, with two types of inhomogeneities: one with typical sizes of one to several nanometers, and one with typical sizes of 10 to 20 nm, respectively.     

Current-induced voltage oscillations in superconducting Y<Subscript>1</Subscript>Ba<Subscript>2</Subscript>Cu<Subscript>3</Subscript>O<Subscript>7-δ</Subscript>

We investigated influence of bidirectional square wave current with long periods and dc current on the evolution of the voltage-time (V - t) curves in superconducting polycrystalline bulk Y₁Ba₂Cu₃O_7-δ (YBCO) material at the temperatures near the critical temperature. In a well-defined range of amplitudes and periods of driving current, and temperatures, novel type of non-linear dynamic responses was observed by means of the V-t curves. It was seen that such a non-linear response to bidirectional square wave current sometimes reflects itself as regular sinusoidal-like voltage oscillations. The sinusoidal-like and non-sinusoidal oscillations were discussed mainly in terms of the dynamic competition between pinning and depinning and significant relaxation effects which appear in this competing process. The density fluctuations associated with the current induced self-magnetic flux (SMF) lines and semi-elastic coupling of SMF lines with the pinning centers were also considered as possible physical mechanisms in the interpretation of the experimental results.     

Current dependent reorganization in superconducting Y<Subscript>1</Subscript>Ba<Subscript>2</Subscript>Cu<Subscript>3</Subscript>O<Subscript>7-δ</Subscript>

We present strong non-linear dynamic responses developing due to magnitude and type of driving current in bulk polycrystalline superconducting Y₁Ba₂Cu₃O_7-δ sample at zero magnetic field. Several novel types of dynamic changes induced by the transport current were observed via the time evolution of the voltage (V - t curves). The physical observations appearing in V - t curves were interpreted mainly with the reorganization of driving current in a multiply connected network of weak-link structure. It was found that such a dynamic process could cause an enhancement or suppression in superconducting order parameter due to the magnitude of the driving current and coupling strength of weak link structure together with the chemical and anisotropic states of the sample. It was shown that the general behavior of decays evolving in V - t curves is consistent with an exponential relation which is analogous to the glassy state relaxation.     

Mössbauer studies of spatial spin-modulated structure and hyperfine interactions in multiferroic Bi<Superscript>57</Superscript>Fe<Subscript>0.10</Subscript>Fe<Subscript>0.85</Subscript>Cr<Subscript>0.05</Subscript>O<Subscript>3</Subscript>

Results of Mössbauer investigations on ⁵⁷Fe nuclei in multiferroic material Bi⁵⁷Fe_0.10Fe_0.85Cr_0.05O₃ in the temperature range from 5.2 to 300 K are presented. Bulk rhombohedral samples were obtained by solidstate synthesis at high pressure. Mössbauer spectra were analyzed using the model of spatial incommensurate spin-modulated structure of the cycloidal type. Information on the influence of substituting Cr cations for Fe cations on hyperfine spectral parameters was obtained: the shift and quadrupolar shift of a Mössbauer line, and isotropic and anisotropic contributions into the hyperfine magnetic field. The anharmonicity parameter m of the spatial spin-modulated structure increases almost 1.7 times at 5.2 K when BiFeO₃ is doped with chromium. The data on m were used for calculation of the uniaxial magnetic anisotropy constants and their temperature dependences for pure and chromium-doped BiFeO₃.     

High-Temperature Heat Capacity of Zn<Subscript>2</Subscript>V<Subscript>2</Subscript>O<Subscript>7</Subscript>–Cu<Subscript>2</Subscript>V<Subscript>2</Subscript>O<Subscript>7</Subscript> Solid Solutions

Differential scanning calorimetry has been used to study the influence of temperature on the heat capacity of synthesized vanadates Zn₂V₂O₇, (Cu_0.56Zn_1.44)V₂O₇, and (Cu_1.0Zn_1.0)V₂O₇. It is found that dependences C_p = f(T) have extremes. The thermodynamic properties of Zn₂V₂O₇ have been determined.     

Cluster spin glass and superparamagnetism in RuSr<Subscript>2</Subscript>Eu<Subscript>1.5</Subscript>Ce<Subscript>0.5</Subscript>Cu<Subscript>2</Subscript>O<Subscript>10-</Subscript><Subscript>δ</Subscript>

We investigate in detail the dc magnetization and nonlinear ac susceptibility behavior of the superconducting ferromagnet RuSr₂Eu_1.5Ce_0.5Cu₂O_{10- δ} (Ru1222) to develop a comprehensive understanding of the spin glass and superparamagnetism in this material. The structural properties of the system result in the formation of magnetic (ferromagnetic) clusters of different sizes, shapes and properties. The magnetic clustering of the system leads to observation of various features in dc magnetization and ac susceptibility consistent with superparamagnetism and cluster spin glass states, which can coexist or stand alone, depending on the temperature range considered. Experimental results of magnetic measurements in combination with their analysis have enabled us to explain and distinguish these phenomena, as well as to propose a temperature dependent scenario of the system behavior.     

Internal friction and magnetoelectric response in two-layer composites Tb<Subscript>0.12</Subscript>Dy<Subscript>0.2</Subscript>Fe<Subscript>0.68</Subscript>–PbZr<Subscript>0.53</Subscript>Ti<Subscript>0.47</Subscript>O<Subscript>3</Subscript>

The inverse magnetoelectric effect and internal friction in two-layer composites based on ferromagnetic Tb_0.12Dy_0.2Fe_0.68 and piezoelectric PbZr_0.53Ti_0.47O₃ are studied in an ac electrical field in the frequency range of 52–213 kHz at temperatures of 293 to 400 K. A correlation is found between the internal friction and the efficiency of the inverse magnetoelectric transformation at resonant frequencies.     

Preparation and characterization of organic–inorganic hybrid compound [N(C<Subscript>4</Subscript>H<Subscript>9</Subscript>)<Subscript>4</Subscript>]<Subscript>2</Subscript>Cu<Subscript>2</Subscript>Cl<Subscript>6</Subscript>

Organic–inorganic hybrid sample [N(C₄H₉)₄]₂Cu₂Cl₆ was prepared via the reaction between copper chloride and tetrabutylammonium chloride. The compound was characterized by X-ray powder diffraction, IR, Raman, differential scanning calorimetry (DSC), DTA-TGA analysis and electrical impedance spectroscopy. DSC studies indicate a presence of one-phase transition at 343 K. The complex impedance of compound [N(C₄H₉)₄]₂Cu₂Cl₆ have been investigated in temperature and frequency ranges 300–380 K and 200 Hz–5 MHz, respectively. The Z′ and Z″ versus frequency plots are well fitted to an equivalent circuit model. The circuits consist of the parallel combination of bulk resistance R _p and constant phase elements CPE. The frequency dependence of the conductivity is interpreted in term of Jonscher's law: s(w) = s_dc + Awⁿ \sigma (\omega ){ } = {\sigma_{\rm{dc}}} + { }A{\omega^n} . The conductivity follows the Arrhenius relation. The variation of the value of these elements with temperatures confirmed the availability of the phase transition at 343 K detected by DSC and electrical measurements.     

Surface of underdoped YBa<Subscript>2</Subscript>Cu<Subscript>3</Subscript>O<Subscript>7-</Subscript><Subscript>δ</Subscript> as revealed by STM/STS

We performed scanning tunneling microscopy and spectroscopy on untwinned crystals of underdoped YBa₂Cu₃O_{7- δ} at δ = 0.4. A comprehensive statistical analysis of our topographic data indicates a doping dependent cleaving behavior of this material. We find in particular that at δ = 0.4 the material primarily cleaves in multiples of one unit cell along the c-axis with a high corrugation of the topmost layer. Our data suggest that the low temperature cleaving mainly results in a disruption of the CuO chain layers involving a redistribution of the layer atoms onto the two cleaving planes. In a few instances, fractional step heights (in terms of the c-axis lattice constant) are observed as well. Scanning tunneling spectroscopy reveals that such fractional steps connect surfaces which differ significantly in their tunneling conductance.     

Synthesis and characterization of Li<Subscript>3</Subscript>V<Subscript>2</Subscript>(PO<Subscript>4</Subscript>)<Subscript>3</Subscript>·LiMn<Subscript>0.33</Subscript>Fe<Subscript>0.67</Subscript>PO<Subscript>4</Subscript>/C cathode materials

A new polyanionic cathode material, Li₃V₂(PO₄)₃·LiMn_0.33Fe_0.67PO₄/C for lithium-ion batteries, was synthesized using a sol-gel method and with N,N-dimethyl formamide as a dispersion agent. The analysis of electron transmission spectroscopy and X-ray diffraction revealed that the composite contained two phases. The material has high crystallinity with a grain size of 20–50 nm. The valence states of Mn, V, and Fe in the composite were analyzed by X-ray photoelectron spectroscopy. The electrochemical kinetics in Li₃V₂(PO₄)₃ is effectively enhanced by the incorporation of LiMnPO₄ and LiFePO₄, via structure modification and reduced Li diffusion length. The Li₃V₂(PO₄)₃·LiMn_0.33Fe_0.67PO₄/C materials displayed high rate capacity and steady cycle performance with discharge capacity remained 148 mAh g^?1 after 50 cycles at the rate of 0.2C. In particular, the composite exhibited excellent reversible capacities, with the values of 157, 134, 120, 102, and 94 mAh g^?1 at charge/discharge 0.2, 0.5, 1, 2, and 5C rates, respectively.     

Superconductivity in Sr<Subscript>0.75</Subscript>Y<Subscript>0.75</Subscript>Ba<Subscript>1.5</Subscript>Cu<Subscript>3</Subscript> O<Subscript>7−<Emphasis Type="Italic">d</Emphasis></Subscript> compounds

The effect of simultaneous Sr substitution at the Ba and Y sites has been studied in the Sr_0.75Y_0.75Ba_1.5Cu₃O_7–dsystem. Attempts to replace 25% Y and 25% Ba have been successful and superconductivity was observed above 78 K for Sr_0.75Y_0.75Ba_1.5Cu₃O_7–d compound with high oxygen content, i.e., O_6.76, and having orthorhombic crystal symmetry. The compound was treated in argon gas at 800°C to reduce the oxygen content and to induce some structural changes. The Sr_0.75Y_0.75Ba_1.5Cu₃O_6.1 compound thus obtained has tetragonal symmetry and low oxygen content, O_6.1. It has also shown superconductivity at 28 K. The paper presents a careful comparison of the structural and electrical properties and infrared absorbance spectra of the two compounds with the same metallic composition, Sr_0.75Y_0.75Ba_1.5Cu₃, but with different oxygen content and crystal symmetry. The study clearly establishes the occurrence of superconductivity in tetragonal Sr-substituted (both at Y and Ba sites in) YBCO.     

Phase formation in the BaCO<Subscript>3</Subscript>–PbO–Fe<Subscript>2</Subscript>O<Subscript>3</Subscript>–Nb<Subscript>2</Subscript>O<Subscript>5</Subscript> system

Features of the formation of lead-ferroniobate compounds in the xBaCO₃–(1 – x)PbO–Fe₂O₃–Nb₂O₅ system by solid-phase synthesis are investigated. For perovskite-type lead-ferroniobate solid solution, a single-phase concentration region is revealed at 1233 K. The crystalline structures of the synthesized compounds are refined using Rietveld analysis and the Pm3?m and R3m space groups. Ceramic samples of lead ferroniobate are studied by scanning electron microscopy.     

Microwave characterization of Pb<Subscript>1−x</Subscript>Ca<Subscript>x</Subscript>Fe<Subscript>0.5</Subscript>Nb<Subscript>0.5</Subscript>O<Subscript>3</Subscript> multiferroics at X-band

The microwave characteristics of Pb_1?x Ca _x Fe_0.5Nb_0.5O₃ multiferroics (x = 0.0, 0.4, 0.45, 0.5, 0.55, 0.6), have been investigated as a function of frequency and substitution. The results depict ?13.99 dB reflection loss at 11.65 GHz in composition x = 0.6. Microwave absorption is enhanced with substitution of Ca²⁺ ions and undoped composition 0.0 behaves as electromagnetic shield. The model governing microwave absorption is discussed and different compositions for electromagnetic applications have been suggested.     

Magnetorefractive effect in (Co<Subscript>50</Subscript>Fe<Subscript>50</Subscript>)<Subscript>x</Subscript>(Al<Subscript>2</Subscript>O<Subscript>3</Subscript>)<Subscript>1−<Emphasis Type="Italic">x</Emphasis></Subscript> granular films

The reflectivity spectra and the magnetorefractive effect (MRE) of (Co₅₀Fe₅₀)_x(Al₂O₃)_1?x metal-dielectric granular films (0.07<x<0.52) are analyzed in the IR spectral range λ=2.5–25 µm. It is revealed that the specific features observed in the spectra at λ≈8.5 and 20 µm are associated with the excitation of phonon modes in the dielectric matrix. The magnetorefractive effect in the films is observed below the percolation thresh-old only in p-polarized light and above the percolation threshold for both the p and s polarizations. It is demonstrated that the optical properties of (Co₅₀Fe₅₀)_x(Al₂O₃)_1?x films in the IR spectral range, to a first approximation, can be interpreted in the framework of the effective-medium theory and the magnetorefractive effect can be explained in terms of the modified Hagen-Rubens relation.     

Fractal magnetic microstructure in the (Co<Subscript>41</Subscript>Fe<Subscript>39</Subscript>B<Subscript>20</Subscript>)<Subscript>x</Subscript>(SiO<Subscript>2</Subscript>)<Subscript>1−<Emphasis Type="Italic">x</Emphasis></Subscript> nanocomposite films

Magnetostructural methods are applied to determine the exchange bond percolation limit in (Co₄₁Fe₃₉B₂₀)_x(SiO₂)_1?x nanocomposites (x _c = 0.30 ± 0.02), which separates the phase plane along the metal concentration axis into a superparamagnetic region and a ferromagnetic region. It is shown that, with respect to the singularities of the magnetization up to the magnetization saturation curves, the ferromagnetic region is further subdivided into three regions differing in the character of the spatial propagation of the magnetization ripples or in the magnetic correlation function characteristics. The fractal dimension of the nanocomposite magnetic microstructure near the percolation threshold is determined.     

Effect of hydrostatic pressure on the superconductivity in fluorinated Hg<Subscript>0.8</Subscript>Ba<Subscript>2</Subscript>Ca<Subscript>2</Subscript>Cu<Subscript>3.2</Subscript>O<Subscript>8+δ</Subscript>

The effect of hydrostatic pressure on the superconducting transition temperature was measured for the Hg-1223 phase of a fluorinated mercury cuprate high-temperature superconductor with T_c(optim)=38 K. The value of the T_c derivative with respect to pressure was found to be rather high (11.0 K/GPa); at P=1.5 GPa, T_c=153.5 K. The results obtained are discussed in connection with works on the synthesis of such samples.     

Controlled flame synthesis of αFe<Subscript>2</Subscript>O<Subscript>3</Subscript> and Fe<Subscript>3</Subscript>O<Subscript>4</Subscript> nanoparticles: effect of flame configuration,flame temperature,and additive loading

Superparamagnetic iron oxide nanoparticles are used in diverse applications, including optical magnetic recording, catalysts, gas sensors, targeted drug delivery, magnetic resonance imaging, and hyperthermic malignant cell therapy. Combustion synthesis of nanoparticles has significant advantages, including improved nanoparticle property control and commercial production rate capability with minimal post-processing. In the current study, superparamagnetic iron oxide nanoparticles were produced by flame synthesis using a coflow flame. The effect of flame configuration (diffusion and inverse diffusion), flame temperature, and additive loading on the final iron oxide nanoparticle morphology, elemental composition, and particle size were analyzed by transmission electron microscopy (TEM), high-resolution TEM (HR-TEM), energy dispersive spectroscopy (EDS), and Raman spectroscopy. The synthesized nanoparticles were primarily composed of two well known forms of iron oxide, namely hematite αFe₂O₃ and magnetite Fe₃O₄. We found that the synthesized nanoparticles were smaller (6–12 nm) for an inverse diffusion flame as compared to a diffusion flame configuration (50–60 nm) when CH₄, O₂, Ar, and N₂ gas flow rates were kept constant. In order to investigate the effect of flame temperature, CH₄, O₂, Ar gas flow rates were kept constant, and N₂ gas was added as a coolant to the system. TEM analysis of iron oxide nanoparticles synthesized using an inverse diffusion flame configuration with N₂ cooling demonstrated that particles no larger than 50–60 nm in diameter can be grown, indicating that nanoparticles did not coalesce in the cooler flame. Raman spectroscopy showed that these nanoparticles were primarily magnetite, as opposed to the primarily hematite nanoparticles produced in the hot flame configuration. In order to understand the effect of additive loading on iron oxide nanoparticle morphology, an Ar stream carrying titanium-tetra-isopropoxide (TTIP) was flowed through the outer annulus along with the CH₄ in the inverse diffusion flame configuration. When particles were synthesized in the presence of the TTIP additive, larger monodispersed individual particles (50–90 nm) were synthesized as observed by TEM. In this article, we show that iron oxide nanoparticles of varied morphology, composition, and size can be synthesized and controlled by varying flame configuration, flame temperature, and additive loading.     

A structural,magnetostrictive and Mössbauer study of Tb<Subscript>0.3</Subscript>Dy<Subscript>0.7</Subscript>(Fe<Subscript>0.9</Subscript><Emphasis Type="Italic">T</Emphasis><Subscript>0.1</Subscript>)<Subscript>1.95</Subscript> alloys

The effect of IIIA metal and transition metalT substitution for Fe on crystal structure, magnetostriction and spontaneous magnetostriction, anisotropy and spin reorientation of a series of polycrystalline Tb_0.3 Dy_0.7 (Fe_0.9 T _0.1)_1.95 (T=Mn, Fe, Co, B, Al, Ga) alloys at room temperature were investigated systematically. It was found that the primary phase of the Tb_0.3 Dy_0.7 (Fe_0.9 T _0.1)_1.95 alloys is the MgCu₂-type cubic Laves phase structure for different substitution. The magnetostrictionλ _s decrases greatly for the substitution of IIIA metal, B, Al and Ga, but is saturated more easily for Al and Ga substitution, showing that the Al and Ga substitution is beneficial to a decrease in the magnetocrystalline anisotropy of Tb_0.3 Dy_0.7 (Fe_0.9 T _0.1)_1.95 alloys. However, the substitution of transition metal Mn and Co decreases slightly the magnetostrictionλ _s . It was also found that the effect of different substitutions on the spontaneous magnetostrictionλ ₁₁₁ is distinct. The analysis of the Mössbauer spectra indicates that the easy magnetization direction in the {110} plane deviates slightly from the main axis of symmetry for Al and Ga substitution, namely spin reorientation, but it does not change evidently for B, Mn and Co substitution.     

Spectroscopic study of magnetic phase transitions in Nd<Subscript>x</Subscript>Gd<Subscript>1−<Emphasis Type="Italic">x</Emphasis></Subscript>Fe<Subscript>3</Subscript>(BO<Subscript>3</Subscript>)<Subscript>4</Subscript>

Magnetic ordering and spin reorientation in iron borates Nd_xGd_1?xFe₃(BO₃)₄ (x = 0.01, 0.04, 0.25, 1.0) are studied using a rare-earth spectroscopic probe.