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At least 1,765 records · Page 98
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DOE OSTI2014

Room temperature multiferroic properties and magnetoelectric coupling in Sm and Ni substituted Bi{sub 4−x}Sm{sub x}Ti{sub 3−x}Ni{sub x}O{sub 12±δ} (x = 0, 0.02, 0.05, 0.07) ceramics

Lead free multiferroic Bi{sub 4−x}Sm{sub x}Ti{sub 3−x}Ni{sub x}O{sub 12±δ} (x = 0.02, 0.05, and 0.07) samples have been synthesized by conventional solid state route. X-ray diffraction analysis reveals single phase up to x = 0.07, and a secondary phase appears at x > 0.07. Raman spectroscopy confirms the local distortions in the crystal. Field emission scanning electron microscopy shows plate like grains. Substitution has increased the orthorhombic distortion, grain size, and hence the ferroelectric transition temperature (T{sub c}). A significant reduction in the values of dielectric constant (ε′) and loss tangent (tan δ) has been observed with the increase of Sm and Ni ions. The increase in dc resistivity at room temperature has been found with substitution. Enhancement in the values of remnant polarization (2P{sub r}) and magnetization (2M{sub r}) is observed. Magnetoelectric coupling coefficient (α) values of 0.60 mV/cm/Oe are achieved in Bi{sub 4−x}Sm{sub x}Ti{sub 3−x}Ni{sub x}O{sub 12±δ} ceramic samples. Hence, we have successfully converted the ferroelectric Bi{sub 4}Ti{sub 3}O{sub 12} into a multiferroic, which is a new lead free multiferroic material, can be useful for future electromagnetic devices.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2014

Investigation of A-site La substituted BaTi{sub 0.96}Mn{sub 0.04}O{sub 3} ceramics: Searching for ferromagnetic origin

Ba{sub 1-x}La{sub x}Ti{sub 0.96}Mn{sub 0.04}O{sub 3} ceramics (x = 0, 3%, 7%) were prepared by a modified Pechini method and the structure, morphology, magnetic and electric properties have been investigated. X-ray diffraction analysis reveals La{sup 3+} ions could suppress the formation of hexagonal phase effectively. The cell parameter c decreases firstly and then increases with the increase of La content, which indicates that La ions have been incorporated into the lattice of BaTi{sub 0.96}Mn{sub 0.04}O{sub 3}, and that Mn ions transform from high valence to low valence. The magnetization, polarization and leakage currents are also influenced by La doping greatly. Detailed analysis of magnetic variation with structural change attributes the room temperature ferromagnetism to double exchange interactions between Mn{sup 3+} and Mn{sup 4+} ions.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2014

Photoluminescence in Pb{sub 0.95}Sr{sub 0.05}(Zr{sub 1−x}Ti{sub x}){sub 1−y}Cr{sub y}O{sub 3} ferroelectric ceramic system

Over the past several years, there has been a remarkable growth and development in new ceramic and/or composite materials to be used in the electro-electronic industry. Ferroelectric materials have been recognized for their multifunctional physical properties; also, their optical properties are a subject of intense research effort due to their possible electro-optic applications. In this work, the visible photoluminescence effect is analyzed at room temperature in a sintered Pb{sub 0.95}Sr{sub 0.05}(Zr{sub 1−x}Ti{sub x}){sub 1−y}Cr{sub y}O{sub 3} perovskite-type structure system, doped with Sr and Cr. The excitation bands used were 267, 325, 373, 457, 635, and 680 nm, but the best result was obtained at 373 nm. The intensity and energy of such emission in this system have been studied by changing the molar Cr concentration (0 < y < 0.005) and the Ti content (x), with x = 0.20, 0.40, 0.53, 0.60, and 0.80, on both sides of the morphotropic phase boundary (MPB) zone. The principal emission bands are at the energies 1.73, 1.87, and 3.03 eV. The changes that were caused by Zr or Ti ions in the symmetry presented in the rhombohedral or tetragonal side of the MPB are more important. Additionally, structural and micro-structural measurements were performed by the x-ray diffraction and scanning electron microscopy techniques, respectively. The micro-Raman technique is also used in the study of this set of samples, which allows finding the Raman shift modes and the influence on the structural changes of the dopants.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2014

Experimentally validated finite element model of electrocaloric multilayer ceramic structures

A novel finite element model to simulate the electrocaloric response of a multilayer ceramic capacitor (MLCC) under real environment and operational conditions has been developed. The two-dimensional transient conductive heat transfer model presented includes the electrocaloric effect as a source term, as well as accounting for radiative and convective effects. The model has been validated with experimental data obtained from the direct imaging of MLCC transient temperature variation under application of an electric field. The good agreement between simulated and experimental data, suggests that the novel experimental direct measurement methodology and the finite element model could be used to support the design of optimised electrocaloric units and operating conditions.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2014

Optical energy storage and reemission based weak localization of light and accompanying random lasing action in disordered Nd{sup 3+} doped (Pb, La)(Zr, Ti)O{sub 3} ceramics

Multi-mode random lasing action and weak localization of light were evidenced and studied in normally transparent but disordered Nd{sup 3+} doped (Pb,La)(Zr,Ti)O{sub 3} ceramics. Noticeable localized zone and multi-photon process were observed under strong pumping power. A tentative phenomenological physical picture was proposed by taking account of diffusive process, photo-induced scattering, and optical energy storage process as dominant factors in elucidating the weak localization of light observed. Both the decreased transmittance (increased reflectivity) of light and the observed long lasting fading-off phenomenon supported the physical picture proposed by us.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗
DOE OSTI2014

Ferroelectric polymer-ceramic composite thick films for energy storage applications

We have successfully fabricated large area free standing polyvinylidene fluoride -Pb(Zr{sub 0.52}Ti{sub 0.48})O{sub 3} (PVDF-PZT) ferroelectric polymer-ceramic composite (wt% 80–20, respectively) thick films with an average diameter (d) ∼0.1 meter and thickness (t) ∼50 μm. Inclusion of PZT in PVDF matrix significantly enhanced dielectric constant (from 10 to 25 at 5 kHz) and energy storage capacity (from 11 to 14 J/cm{sup 3}, using polarization loops), respectively, and almost similar leakage current and mechanical strength. Microstructural analysis revealed the presence of α and β crystalline phases and homogeneous distribution of PZT crystals in PVDF matrix. It was also found that apart from the microcrystals, well defined naturally developed PZT nanocrystals were embedded in PVDF matrix. The observed energy density indicates immense potential in PVDF-PZT composites for possible applications as green energy and power density electronic elements.

36 MATERIALS SCIENCE↗
DOE OSTI2014

Thickness dependence of magnetoelectric response for composites of Pb(Zr{sub 0.52}Ti{sub 0.48})O{sub 3} films on CoFe{sub 2}O{sub 4} ceramic substrates

Using chemical solution spin-coating we grew Pb(Zr{sub 0.52}Ti{sub 0.48})O{sub 3} films of different thicknesses on highly dense CoFe{sub 2}O{sub 4} ceramics. X-ray diffraction revealed no other phases except Pb(Zr{sub 0.52}Ti{sub 0.48})O{sub 3} and CoFe{sub 2}O{sub 4}. In many of these samples we observed typical ferroelectric hysteresis loops, butterfly-shaped piezoelectric strains, and the magnetic-field-dependent magnetostriction. These behaviors caused appreciable magnetoelectric responses based on magnetic-mechanical-electric coupling. Our results indicated that the thickness of the Pb(Zr{sub 0.52}Ti{sub 0.48})O{sub 3} film was important in obtaining strong magnetoelectric coupling.

36 MATERIALS SCIENCE↗
DOE OSTI2014

Electro-caloric effect in lead-free Sn doped BaTiO{sub 3} ceramics at room temperature and low applied fields

Structural, dielectric, ferroelectric (FE), {sup 119}Sn Mössbauer, and specific heat measurements of polycrystalline BaTi{sub 1–x}Sn{sub x}O{sub 3} (x = 0% to 15%) ceramics are reported. Phase purity and homogeneous phase formation with Sn doping is confirmed from x-ray diffraction and {sup 119}Sn Mössbauer measurements. With Sn doping, the microstructure is found to change significantly. Better ferroelectric properties at room temperature, i.e., increased remnant polarization (38% more) and very low field switchability (225% less) are observed for x = 5% sample as compared to other samples and the results are explained in terms of grain size effects. With Sn doping, merging of all the phase transitions into a single one is observed for x ≥ 10% and for x = 5%, the tetragonal to orthorhombic transition temperature is found close to room temperature. As a consequence better electro-caloric effects are observed for x = 5% sample and therefore is expected to satisfy the requirements for non-toxic, low energy (field) and room temperature based applications.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2014

High temperature dielectric relaxation anomaly of Y³⁺ and Mn²⁺ doped barium strontium titanate ceramics

Relaxation like dielectric anomaly is observed in Y³⁺ and Mn²⁺ doped barium strontium titanate ceramics when the temperature is over 450 K. Apart from the conventional dielectric relaxation analysis method with Debye or modified Debye equations, which is hard to give exact temperature dependence of the relaxation process, dielectric response in the form of complex impedance, assisted with Cole-Cole impedance model corrected equivalent circuits, is adopted to solve this problem and chase the polarization mechanism in this paper. Through this method, an excellent description to temperature dependence of the dielectric relaxation anomaly and its dominated factors are achieved. Further analysis reveals that the exponential decay of the Cole distribution parameter n with temperature is confirmed to be induced by the microscopic lattice distortion due to ions doping and the interaction between the defects. At last, a clear sight to polarization mechanism containing both the intrinsic dipolar polarization and extrinsic distributed oxygen vacancies hopping response under different temperature is obtained.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2014

Influence of secondary phases on phase and microwave dielectric properties of new Ca{sub 2}Ce{sub 2}Ti{sub 5}O{sub 16} ceramics

Ca{sub 2}Ce{sub 2}Ti{sub 5}O{sub 16} ceramics processed via mix oxide route was investigated. Phase composition and microwave dielectric properties were measured using X-ray diffraction and a cavity method, respectively. CeO{sub 2} and another unidentified phase (that vanishes at ≥1400°C) existed as secondary phases along with the parent Ca{sub 2}Ce{sub 2}Ti{sub 5}O{sub 16} phase. The amount of the parent Ca{sub 2}Ce{sub 2}Ti{sub 5}O{sub 16} phase increased with increasing sintering temperature from 1350°C to 1450 °C accompanied by a decrease in the apparent density. The density decreased but ε{sub r} and Qufo increased with sintering temperature. An ε{sub r} ∼87.2, Qufo ∼5915 GHz and τ{sub f} ∼219 GHz was achieved for the sample sintered at 1450°C.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2014

Manufacturing techniques studies of ceramics by neutron and γ-ray radiography

In this study, the aim was to evaluate capabilities and constraints of radiographic imagery using thermal neutrons and gamma-rays as tools to identify the type of technique employed in ceramics manufacturing especially that used in prehistoric Brazilian pottery from Acre state. For this purpose, radiographic images of test objects made with clay of this region using both techniques - palette and rollers - have been acquired with a system comprised of a source of gamma-rays or thermal neutrons and a corresponding X-ray or neutron-sensitive Imaging Plate as detector. For the neutrongraphy samples were exposed to a thermal neutron flux of order of 10{sup 5}n.cm{sup −2}.s{sup −1} for 3 minutes at main port of Argonauta research reactor of the Instituto de Engenharia Nuclear - IEN/CNEN. The radiographic images using γ-rays from {sup 165}Dy (95 keV) and {sup 198}Au (412 keV) both produced at this reactor, have been acquired under an exposure time of a couple of hours. After acquisition, images have undergone a treatment to improve their quality through enhancement of their contrast, a procedure involving corrections of the beam divergence, sample shape and averaging of the attenuation map profile. Preliminary results show that difference between manufacturing techniques is better identified by radiography using low energy γ-rays from {sup 165}Dy rather than neutrongraphy or γ-rays from {sup 198}Au. Nevertheless, disregarding the kind of employed radiation, it should be stressed that feasibility to apply the technique is tightly tied to homogeneity of the clay itself and tempers due to their different attenuation.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗
DOE OSTI2014

Exchange bias effect in Bi{sub 2}Fe{sub 3}AlO{sub 9} ceramics

The exchange bias (EB) effect is observed in Bi{sub 2}Fe{sub 3}AlO{sub 9} polycrystalline ceramics. The EB field (H{sub EB}), vertical magnetization shift, and coercive field show a strong dependence on the cooling fields. When a larger applied field is used to measure the hysteresis loop, the EB effect is suppressed. The induced spin-glass-like phase via Al{sup 3+} doping is responsible for the EB effect below the spin-glass temperature (T{sub SG}) of ∼25 K. Moreover, the H{sub EB} varies nonmonotonically with temperature above T{sub SG}, which is interpreted using a random field model with the exchange coupling between ferromagnetic clusters and an antiferromagnetic phase.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗
DOE OSTI2014

Observation of high-spin mixed oxidation state of cobalt in ceramic Co{sub 3}TeO{sub 6}

We report coexistence of high spin Co{sup 3+} and Co{sup 2+} in ceramic Co{sub 3}TeO{sub 6} using X-ray Absorption Near Edge Structure (XANES), DC magnetization, and first principles ab-initio calculations. The main absorption line of cobalt Co K-edge XANES spectra, along with a linear combination fit, led us to estimate relative concentration of Co{sup 2+} and Co{sup 3+}as 60:40. The pre edge feature of XANES spectrum shows crystal field splitting of ∼1.26 eV between e{sub g} and t{sub 2g} states, suggesting a mixture of high spin states of both Co{sup 2+} and Co{sup 3+}. Temperature dependent high field DC magnetization measurements reveal dominant antiferromagnetic order with two Neel temperatures (T{sub N1} ∼ 29 K and T{sub N2} ∼ 18 K), consistent with single crystal study. A larger effective magnetic moment is observed in comparison to that reported for single crystal (which contains only Co{sup 2+}), supports our inference that Co{sup 3+} exists in high spin state. Furthermore, we show that both Co{sup 2+} and Co{sup 3+} being in high spin states constitute a favorable ground state through first principles ab-initio calculations, where Rietveld refined synchrotron X-ray diffraction data are used as input.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗
DOE OSTI2014

Terbium gallium garnet ceramic-based Faraday isolator with compensation of thermally induced depolarization for high-energy pulsed lasers with kilowatt average power

A scalable aperture Faraday isolator for high-energy pulsed lasers with kW-level average power was demonstrated using terbium gallium garnet ceramics with water cooling and compensation of thermally induced depolarization in a magnetic field. An isolation ratio of 35 dB (depolarization ratio γ of 3.4 × 10{sup −4}) was experimentally observed at a maximum laser power of 740 W. By using this result, we estimated that this isolator maintains an isolation ratio of 30 dB for laser powers of up to 2.7 kW. Our results provide the solution for achieving optical isolation in high-energy (100 J to kJ) laser systems with a repetition rate greater than 10 Hz.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗
DOE OSTI2015

Mechanism of photochromic effect in Pb(Zr,Ti)O{sub 3} and (Pb,La)(Zr,Ti)O{sub 3} ceramics under violet/infrared light illumination

Obvious photochromic effects were observed in Pb(Zr,Ti)O{sub 3} and (Pb,La)(Zr,Ti)O{sub 3} (PLZT) ceramics, along with exponential responses to illumination power in both darkening and bleaching processes. An interesting anomalous dispersion in the transparent PLZT was observed and discussed. A tentative physical picture based on photoinduced electron stimulated processes and on structural change was proposed to explain all the interesting observations. Rate equations were established and solved in verifying the validity of the proposed model. This work may serve as guidance in designing tunable achromatic lenses, UV and IR light detectors and sensors.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗
DOE OSTI2015

Lead-free Ba{sub 0.8}Ca{sub 0.2}(Zr{sub x}Ti{sub 1−x})O{sub 3} ceramics with large electrocaloric effect

The electrocaloric effect was investigated in lead-free Zr doped Ba{sub 0.8}Ca{sub 0.2}(Zr{sub x}Ti{sub 1−x})O{sub 3} (BCTZ) ceramics synthesized by a conventional sintering process. Room-temperature x-ray diffraction analysis showed that the tetragonal structure is obtained in BCTZ for x ≤ 0.08 and a pseudo cubic phase for x > 0.08. The dielectric spectroscopy and calorimetry revealed that the Curie temperature decreases as a consequence of Zr doping and that the BCTZ exhibits a first order ferroelectric phase transition. The electrocaloric effect was determined by the calculation of the electrocaloric change of temperature (ΔT) using the Maxwell relation based on the P–E hysteresis loops measured at different temperatures. A large electrocaloric responsivity ΔT/ΔE = 0.34 × 10{sup −6 }Km/V was found for x = 0.04, which significantly exceeds of values found so far in other lead-free electrocaloric materials.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Lattice dynamics and broad-band dielectric properties of multiferroic Pb(Fe{sub 1/2}Nb{sub 1/2})O{sub 3} ceramics

Complex dielectric properties of Pb(Fe{sub 1/2}Nb{sub 1/2})O{sub 3} ceramics were investigated in a broad frequency range from 100 Hz up to 90 THz. A broad dielectric anomaly was observed near the temperature of the ferroelectric phase transition (T{sub C1} = 376 K). Below 1 MHz, the anomaly is strongly influenced by conductivity of the sample, but higher frequency data taken up to 81 MHz reveal a broad and frequency independent peak at T{sub C1} typical for a diffuse ferroelectric phase transition. Surprisingly, dielectric permittivity measured at 37 GHz exhibits a peak shifted by 25 K above T{sub C1}, which indicates polar nanoregions with dynamics in microwave frequency region. A dielectric relaxation, which appears in THz region below 700 K, slows down towards T{sub C1} and again hardens below T{sub C2} = 356 K. This central mode drives both phase transitions, so they belong to order–disorder type, although the polar phonons exhibit anomalies near both phase transitions. In the paraelectric phase, infrared reflectivity spectra correspond to local Fm3{sup ¯}m structure due to short-range chemical ordering of Fe and Nb cations on the B perovskite sites. Moreover, each polar phonon is split due to two different cations on the B sites. Recently, Manley et al. [Nat. Commun. 5, 3683 (2014)] proposed a new mechanism of creation of polar nanoregions in relaxor ferroelectrics. They argued, based on their inelastic neutron scattering studies of PMN–PT, that the TO1 phonon is split and interaction of both components gives rise to so called Anderson phonon localization, which can produce regions of trapped standing waves and these waves induce polar nanoregions in relaxors. We cannot exclude or confirm this mechanism, but we show that the splitting of polar phonons is a common feature for all complex perovskites with relaxor ferroelectric behavior and it can be also observed in canonical ferroelectric BaTiO{sub 3}, where the soft mode is split in paraelectric phase due to a strong lattice anharmonicity.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2015

Large piezoelectricity in Pb-free 0.96(K{sub 0.5}Na{sub 0.5}){sub 0.95}Li{sub 0.05}Nb{sub 0.93}Sb{sub 0.07}O{sub 3}−0.04BaZrO{sub 3} ceramic: A perspective from microstructure

We employ transmission electron microscopy to explore the reason for large piezoelectricity (d{sub 33}≈400pC/N) in a Pb-free 0.96(K{sub 0.5}Na{sub 0.5}){sub 0.95}Li{sub 0.05}Nb{sub 0.93}Sb{sub 0.07}O{sub 3} −0.04BaZrO{sub 3} ceramic from microstructure. The result shows that the high piezoelectricity corresponds to a miniaturized nanodomain configuration in a domain hierarchy. The nanodomains disappear on heating accompanied by a reduction in d{sub 33} value. Further convergent beam electron diffraction study reveals a coexistence of tetragonal and orthorhombic phase, which indicates that large piezoelectricity of KNLNS{sub 0.07}-BZ may stem from easy polarization rotation due to low polarization anisotropy on the tetragonal-orthorhombic phase boundary.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗