Raman spectroscopy study of lattice dynamics of macro-, micro-, and nanostructured barium titanates

The temperature dependences of the components A ₁(2TO) and E(1TO) of the soft ferroelectric mode during phase transitions in single crystals, ceramics, polycrystalline and epitaxial thin films of barium titanate, as well as a superlattice consisting of alternating layers of barium and strontium titanates, have been studied using the Raman spectroscopy method. Abrupt changes in soft mode frequencies have been observed in the single crystal during phase transitions between tetragonal, orthorhombic, and rhombohedral phases. Smoothing of the temperature dependences of soft modes and the coexistence of phases have been observed in ceramics and polycrystalline films. In the epitaxial film, the sequence of structural transformations fundamentally differs from that observed in the single crystal; in the superlattice, the ferroelectric phase is stable to 550 K.     

Synthesis and electrical characterisation of different doped magnesium titanates

The synthesis and characterization are reported for the cubic spinel titanate Mg_(2−x)Ni_xTiO₄ (x≤0.25) and Mg_(2−x)Mn_xTiO₄ (x≤1). Single phase samples were observed for Mg_(2−x)Ni_xTiO₄ and with x≤0.4 for Mg_(2−x)Mn_xTiO₄. AC measurements were carried out on four different compositions (x=0.01, 0.03, 0.04 and 0.15) in the Mg_(2−x)Ni_xTiO₄ series and for Mg_1.9Mn_0.1TiO₄. For all these compounds, increasing conductivity with temperature and Arrhenius conductivity dependence are observed, the activation energy is around 0.28 eV for the Ni compounds and is 0.184 eV for Mg_1.9Mn_0.1TiO₄. The DC conductivity was recorded over a range of oxygen partial pressures (10⁻¹⁹ to 1 atm) at 930 °C. The Mg_(2−x)Ni_xTiO₄ compounds show a n-type behaviour whereas the Mg_(2−x)Mn_xTiO₄ show a p-type behaviour at high p(O₂) and n-type at low p(O₂). The stability under reduced conditions was checked and discussed for the different synthesized compounds. Paper presented at the 5th Euroconference onSolid State Ionics, Benalmádena, Spain, Sept. 13–20, 1998.     

Synthesis, characterization and microwave absorption properties of titania-coated barium ferrite composites

Anatase titania-coated barium ferrite composites were prepared by a heterogeneous precipitation method in the presence of barium ferrite particles. The obtained samples were characterized by ξ-pH, TEM, EDX and XRD. The complex permittivity and permeability were studied in the frequency range of 2-12 GHz. The structure and microwave response properties are investigated. The results show that the coverage of titania has a great influence on microwave response of barium ferrite. The formation of an anatase titania nano-layer on the surface of a barium ferrite particle changes the character of the frequency dispersion of the complex permittivity. Comparing the anatase titania-coated barium ferrite composites with the uncoated barium ferrite, the complex permittivity of the anatase titania-coated barium ferrite composites is higher than that of uncoated barium ferrite. The complex permeability of composites was found to decrease with an increase in frequency as well as with the molar ratio of Ti:Ba. The enhancement of the complex permittivity may be due to dipolar polarization and interfacial polarization. The maximum reflection loss was obtained at the Ti:Ba ratio of 1:10, and the peak of the maximum reflection loss shifts to a lower frequency value with increasing titania fraction. By changing the thickness of titania coverage, the frequency dependence of the complex permittivity could be adjusted, which provides us an opportunity for the synthesis of tailored particles.     

On the nature of differences in the Ni charge states in barium and strontium titanates

XAFS studies of nickel-doped solid solution Ba_1–xSr_xTiO₃ show that the Ni charge state changes from 4 in SrTiO₃ to ~2.5 in BaTiO₃ as x is varied. First-principles electronic structure calculations show that nickel creates an impurity band in the forbidden gap of BaTiO₃ and SrTiO₃. Calculations of the formation energy of the oxygen vacancies explain the difference between the Ni charge states in these compounds by the different formation energies of these vacancies.     

XAFS studies of the local environment of Pb impurity atoms in barium,strontium, and calcium titanates

The local environment of Pb impurity atoms in BaTiO₃, SrTiO₃, and CaTiO₃ crystals was studied by XAFS technique. It is shown that, in both polar and nonpolar phases of BaTiO₃ and in SrTiO₃, the Pb atoms are displaced from the A lattice sites by ～0.15 Å; in CaTiO₃ this displacement is absent. Large values of Debye-Waller factors (0.05–0.10 Ų) for the atoms in the first shell of Pb observed in all the three crystals indicate the distortion of the oxygen environment of Pb atoms. The appearance of these features was explained by the fact that the Pb-O chemical bond has a noticeable covalent component and a Pb atom can form strong bonds only with four of the 12 surrounding oxygen atoms. The obtained data were used to determine the main factors responsible for the occurrence of ferroelectric phase transition in SrTiO₃ and CaTiO₃ and for the increase of the Curie temperature of BaTiO₃ when it is doped with Pb.     

Synthesis and characterization of hard magnetic composites—Hollow microsphere/titania/barium ferrite

Hard magnetic composites—hollow microsphere (core)/titania (intermediate layer)/barium ferrite (magnetic shell) (M/T/B) were prepared by wet-chemical method. Barium ferrite nanoparticles were directly coated on the rutile titania-coated hollow microsphere forming light hard magnetic composites using sol-gel technique. The prepared composites were characterized with FESEM, EDS, XRD and vibrating sample magnetometry. The composites are composed of barium ferrite, hematite, titania and mullite. For the samples with 40 wt.% barium ferrite, its specific saturation magnetization with titania is increased to 17.88 emu/g in comparison with 9.6 emu/g without titania. The function of titania in the composites is also discussed.     

Synthesis and characterization of a nano-scaled barium cerate perovskite powder using starch as polymerization agent

The preparation of nano-sized BaCeO₃ powder using starch as a polymerization agent is described herein. Phase evolution during the decomposition process of a (BaCe)-gel was monitored by XRD. A phase-pure nano-sized BaCeO₃ powder was obtained after calcining of the (BaCe)-gel at 920 °C. The resulting powder has a specific surface area of 15.4 m²/g. TEM investigations reveal particles mainly in the size range of 30 to 65 nm. The shrinkage and sintering behavior of resulting powder compacts were studied in comparison to a coarse-grained mixed-oxide BaCeO₃ powder (S_BET = 2.1 m²/g). Dilatometric measurements show that the beginning of shrinkage of compacts from the nano-sized powder is downshifted by 300 °C compared to mixed-oxide powder. Compacts from the nano-sized powder reach a relative density of 91% after sintering at 1450 °C for 10 h.     

Synthesis and characterization of barium strontium titanate nano powders by low temperature ambient pressure sol process

Journal of Nanoparticle Research - Crystalline (Ba x Sr1?x TiO3) (x = 0, 0.5 0.8 and 1) nanosized powders is synthesized by an ambient pressure and low temperature sol...     

Elaboration and characterization of barium silicate thin films

Room temperature depositions of barium on a thermal silicon oxide layer were performed in ultra high vacuum (UHV). In-situ X-ray photoelectron spectroscopy (XPS) analyses were carried out as well after exposure to air as after subsequent annealings. These analyses were ex-situ completed by secondary ion mass spectrometry (SIMS) profiles and transmission electron microscopy (TEM) cross-sectional images. The results showed that after air exposure, the barium went carbonated. Annealing at sufficient temperature permitted to decompose the carbonate to benefit of a barium silicate. The silicate layer was formed by interdiffusion of barium with the initial SiO₂ layer.     

掺杂钛酸钡薄膜的合成及性能研究

通过化学溶液沉积法制备的BiFeO3-BaTiO3薄膜在室温下能够同时显现铁电性及铁磁性。在600-700℃的条件下,以Pt/TiOx/SiO2/Si为载体,能够成功得到钙钛矿单相0.7BiFeO3-0.3BaTiO3薄膜。随着结晶温度上升,晶粒持续增长,最终在700℃到达更高的结晶度。由于0.7BiFeO3-0.3BaTiO3薄膜的绝缘电阻较低,它所显现的极化（P）-电场（E）磁滞回线较弱。尽管如此,由于在0.7BiFeO3-0.3BaTiO3薄膜铁的位置上添加锰,高作用场的漏电流有效地减少,最终铁电性质得到了提高。在室温下,添加了摩尔分数5%的锰的0.7BiFeO3-0.3BaTiO3薄膜同时显现铁电极化和铁磁磁化磁滞回线。     

掺杂钛酸钡薄膜的合成及性能研究

通过化学溶液沉积法制备的BiFeO3-BaTiO3薄膜在室温下能够同时显现铁电性及铁磁性。在600-700℃的条件下,以Pt/TiOx/SiO2/Si为载体,能够成功得到钙钛矿单相0.7BiFeO3-0.3BaTiO3薄膜。随着结晶温度上升,晶粒持续增长,最终在700℃到达更高的结晶度。由于0.7BiFeO3-0.3BaTiO3薄膜的绝缘电阻较低,它所显现的极化（P）-电场（E）磁滞回线较弱。尽管如此,由于在0.7BiFeO3-0.3BaTiO3薄膜铁的位置上添加锰,高作用场的漏电流有效地减少,最终铁电性质得到了提高。在室温下,添加了摩尔分数5%的锰的0.7BiFeO3-0.3BaTiO3薄膜同时显现铁电极化和铁磁磁化磁滞回线。     

掺杂钛酸钡薄膜的合成及性能研究

通过化学溶液沉积法制备的BiFeO3-BaTiO3薄膜在室温下能够同时显现铁电性及铁磁性。在600-700℃的条件下,以Pt/TiOx/SiO2/Si为载体,能够成功得到钙钛矿单相0.7BiFeO3-0.3BaTiO3薄膜。随着结晶温度上升,晶粒持续增长,最终在700℃到达更高的结晶度。由于0.7BiFeO3-0.3BaTiO3薄膜的绝缘电阻较低,它所显现的极化（P）-电场（E）磁滞回线较弱。尽管如此,由于在0.7BiFeO3-0.3BaTiO3薄膜铁的位置上添加锰,高作用场的漏电流有效地减少,最终铁电性质得到了提高。在室温下,添加了摩尔分数5%的锰的0.7BiFeO3-0.3BaTiO3薄膜同时显现铁电极化和铁磁磁化磁滞回线。     

Preparation and characterization of ZnSn-substituted barium ferrite thin films

The preparation of ZnSn-substituted barium ferrite films by sputtering deposition was studied. The as-sputtered films were amorphous, and annealing at a minimum of 750 °C was required to crystallize the films, based on the X-ray diffraction analysis and the magnetic measurements. Scanning electron microscopy combined with energy-dispersive X-ray spectroscopic microanalysis confirmed that the films were single phase with the composition BaZn_xSn_xFe_12−2xO₁₉, x=0.2−0.3, and their thicknesses were 0.4-1.0 μm when annealed at 750-900 °C. Atomic and magnetic force microscopy studies showed no significant grain growth upon annealing and that the films consisted of single-domain grains forming interaction-cluster-type domains. The natural ferromagnetic resonance frequency was determined at around 4 GHz, together with substantial magnetic losses that make these films promising candidates for microwave absorbers.     

Synthesis and surface properties of submicron barium sulfate particles

Barium sulfate particles were synthesized in the presence of EDTA at room temperature. X-ray diffractometry (XRD), Fourier transform infrared resonance (FTIR) and scanning electron microscopy (SEM) were used to characterize the structure and morphology of BaSO₄ particles. The effect of the preparation parameters on the particle size distribution and morphology was investigated. The conditional formation constants of Ba-EDTA at different pH values were calculated. The results show that the size and morphology of BaSO₄ particles can be effectively controlled by adding EDTA in the precipitation process. Among all the operation conditions, the pH value has significant effect on the particle size. The obtained barium sulfate particles are spherical and well dispersed at pH = 9-10. Zeta potentials of BaSO₄ were measured at different pH. The isoelectric point (IEP) of barium sulfate colloid appears at pH 6.92. The model of the solid-solution interface at a particle of BaSO₄ was presented. The FTIR result indicates that the surface of the prepared BaSO₄ absorbs the functional groups of EDTA, which lower the IEP of the barium sulfate particles.     

Synthesis and characterization of magnetite nanopowders

We have synthesized the iron oxide nanoparticles using the newly developed mechanical ultrasonication method with the FeSO₄ · 7H₂O. We have also investigated the crystallographic structural properties, morphology, and magnetic properties of the nanopowders. According to the high resolution X-ray diffraction result, the as-synthesized iron oxide nanoparticles were magnetite (Fe₃O₄). The particle size of the magnetite nanoparticles was about 6 nm confirmed by transmission electron microscopy image. The particle shape was almost a sphere confirmed by scanning electron microscopy image. The coercivity and saturation magnetization of the as-synthesized iron oxide nanopowders were 114 Oe, and 3.7 emu/g, respectively.     

铜基氧化物气凝胶的制备与表征

以CuCl2·2H2O为前躯体,环氧丙烷为凝胶促进剂,制得了铜基氧化物气凝胶。通过场发射扫描电镜、高分辨透射电镜、X射线衍射、红外谱图及N2吸附等方法,对气凝胶的结构进行了表征。结果表明：室温下合成的铜基氧化物气凝胶呈现3维网络状结构,其骨架由大量微小晶粒组成,颗粒粒径为几nm;随处理温度的升高,体系中的有机相逐渐被灼烧完全,气凝胶也由3维网络状结构转变为致密结构;气凝胶随温度升高不断变化,并最终生成氧化铜气凝胶。N2吸附结果表明气凝胶具有较高的比表面积,为386 m2/g。     

Synthesis and magnetic properties of ordered barium ferrite nanowire arrays in AAO template

BaFe₁₂O₁₉ nanowire arrays having single magnetic domain size (≤460 nm) in anodic aluminum oxide (AAO) templates were prepared by sol-gel and self-propagating high-temperature synthesis techniques. The diameter of the nanowire arrays is approximately 70 nm and the length is about 2-4 μm. The specimens were characterized using X-ray diffraction, vibrating sample magnetometer, field emission scan electron microscope, atomic force microscopy and microwave vector network analyzer. The magnetic properties of BaFe₁₂O₁₉ nanowire arrays embedded in AAO templates were measured by VSM with a field up to 1274 KA/m at room temperature. The results indicate that the nanowire arrays exhibit large saturation magnetization and high coercivity in the range of 6000 Oe and an obvious magnetic anisotropy with the easy magnetizing axis along the length of the nanowire arrays, probably due to the shape anisotropy and magneto-crystalline anisotropy. Finally the microwave absorption properties of the nanowires were discussed.     

Optical characterization of Er3+and Yb3+ co-doped barium fluorotellurite glass

Spectroscopic studies of Er³⁺/Yb³⁺ co-doped (Ba,La)-fluorotellurite glass composition have been carried out using standard experimental and theoretical methods. Quantitative analyses of the room temperature absorption and emission spectra as well as the emission lifetimes yield various important spectroscopic parameters such as the radiative decay rates, fluorescence branching ratios, and emission/absorption cross sections. In addition, internal radiative quantum yields have been determined for the infrared emission at 1571 nm and for the upconversion emission at 547 nm. The influence of various non-radiative properties such as multiphonon relaxation, concentration quenching, and quenching by hydroxyl radicals have also been quantitatively estimated and correlated with the observed spectral properties. The comparative studies with the other composition of tellurite and different glasses showed that present glass composition could be a potential candidate for the broadband amplifier.     

Magnetic properties of barium holmium fluoride, barium erbium fluoride and barium thulium fluoride

A range of properties is surveyed for three barium lanthanum fluoride compounds, where the lanthanum ion may be holmium, erbium or thulium. The experimental methods include magnetic resonance, and optical absorption spectroscopy, together with measurements of heat capacity and magnetic susceptibility.