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At least 1,783 records · Page 99
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DOE OSTI2015

Enhance D. C. resistivity of Ba{sub 0.7}Sr{sub 0.3}TiO{sub 3} ceramic by acceptor (Mn) doping

In the present work, we prepared Ba{sub 0.7}Sr{sub 0.3}TiO{sub 3} and Mn (2 and 3 at % on Ti site) doped Ba{sub 0.7}Sr{sub 0.3}TiO{sub 3} ceramic by sol- gel method. The samples were characterized by X-ray diffraction (XRD). The XRD patterns reveled that Mn ions did not change the perovskite structure of BST (70/30). The dielectric measurements proved that dielectric constant decreased with Mn doping. The dc resistivity was studied by using I-V measurements. The dc resistivity of the BST increased with Mn doping, which suppressed the leakage current.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Structural, ferroelectric and magnetic study of lead free (Na{sub 0.5}Bi{sub 0.5}){sub 1-x}La{sub x}Ti{sub 0.988}Fe{sub 0.012}O{sub 3} (x=0,0.01,0.03,0.05) ceramic

Lead free (Na{sub 0.5}Bi{sub 0.5}){sub 1-x}La{sub x}Ti{sub 0.988}Fe{sub 0.012}O{sub 3} ceramic having compositions (x=0, 0.01, 0.03, 0.05) has been prepared by sol gel method using citric acid. Structural analysis has been done by X-ray diffraction and FTIR measurements. XRD patterns have been confirmed perovskite structure for all samples. FTIR absorption band at around ∼630 cm{sup −1} is observed for all samples which confirm perovskite phase formation in samples. With increasing La concentration, shifting in XRD peaks and FTIR absorption bands is observed which suggests incorporation of La on A-site in prepared (Na{sub 0.5}Bi{sub 0.5}){sub 1-x}La{sub x}Ti{sub 0.988}Fe{sub 0.012}O{sub 3} samples. Effect of La substitution on Ferroelectric (Polarization vs. Electric field) and Magnetic (Magnetization vs. Magnetic field) properties have been studied at room temperature. All samples exhibit weak ferromagnetic order and also possess ferroelectric behavior which provides new insight to lead free single phase multiferroic materials.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Chemical and structural effects on the high-temperature mechanical behavior of (1−x)(Na{sub 1/2}Bi{sub 1/2})TiO{sub 3}-xBaTiO{sub 3} ceramics

Bismuth sodium titanate–barium titanate [(1−x)(Na{sub 1/2}Bi{sub 1/2})TiO{sub 3}-xBaTiO{sub 3}, NBT-100xBT] is one of the most well studied lead-free piezoelectric materials due in large part to the high field-induced strain attainable in compositions near the morphotropic phase boundary (x = 0.06). The BaTiO{sub 3}-rich side of the phase diagram, however, has not yet been as comprehensively studied, although it might be important for piezoelectric and positive temperature coefficient ceramic applications. In this work, we present a thorough study of BaTiO{sub 3}-rich NBT-100xBT by ferroelastic measurements, dielectric permittivity, X-ray diffraction, and Raman spectroscopy. We show that the high-temperature mechanical behavior, i.e., above the Curie temperature, T{sub C}, is influenced by local disorder, which appears also in pure BT. On the other hand, in NBT-100xBT (x < 1.0), lattice distortion, i.e., tetragonality, increases, and this impacts both the mechanical and dielectric properties. This increase in lattice distortion upon chemical substitution is counterintuitive by merely reasoning on the ionic size, and is due to the change in the A-O bond character induced by the Bi{sup 3+} electron lone pair, as indicated by Raman spectroscopy.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Structural and dielectric properties of CuO-doped SrTiO{sub 3} ceramics

Copper-doped SrTiO{sub 3} (ST) ceramic powders were processed by solid-state route diffusion (SRD) bulk preparation technique. We reported the effect of Cu{sup +2} ions on the dielectric response of ST and it established the substantial increase in dielectric constant (ε{sub r}) than undoped ST from 303K-673K and low loss (tanδ) for good dielectric applications. In respect of the electrical properties ac- activation energies were computed of range 0.089-0.319eV using lnσ Vs 1/T plots. The microstructure was examined with grain sizes 6-9µm of uniform distribution by field emission scanning electron microscope (FESEM). Some additional phases SrCu{sub 3}Ti{sub 4}O{sub 12} and TiO{sub 2} rutiles were detected by X-ray diffraction technique.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2015

Isotropic octupolar second harmonic generation response in LaBGeO{sub 5} glass-ceramic with spherulitic precipitation

A spherulitic crystallization of the crystalline phase LaBGeO{sub 5} is generated in the 25La{sub 2}O{sub 3}-25B{sub 2}O{sub 3}-50 GeO{sub 2} glass system. Linear and nonlinear optical properties of lanthanum borogermanate glass-ceramic have been investigated at both macroscopic and microscopic scales. Polarized μ-Raman analysis has evidenced a radial distribution of the crystallites along the c-axis inside spherulites, whereas polarized μ-Second Harmonic Generation (SHG) analysis revealed intensity maxima perpendicularly to the c-axis crystallites orientation. Polarized SHG mapping of a spherulite indicate that no dipolar response along the c-axis oriented crystallites occurs despite the individual dipolar symmetry C{sub 3} of the crystallites. At a larger mm scale, the isotropic scattering of spherulites recorded from macroscopic SHG experiment in the forward direction is consistent with an average coherent octupolar response per spherulite. These SHG analyses at different scale are both in accordance with radial antiferroelectric orientation along the c-axis of crystallites inside each spherulite.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2015

Revisiting the blocking force test on ferroelectric ceramics using high energy x-ray diffraction

The blocking force test is a standard test to characterise the properties of piezoelectric actuators. The aim of this study is to understand the various contributions to the macroscopic behaviour observed during this experiment that involves the intrinsic piezoelectric effect, ferroelectric domain switching, and internal stress development. For this purpose, a high energy diffraction experiment is performed in-situ during a blocking force test on a tetragonal lead zirconate titanate (PZT) ceramic (Pb{sub 0.98}Ba{sub 0.01}(Zr{sub 0.51}Ti{sub 0.49}){sub 0.98}Nb{sub 0.02}O{sub 3}). It is shown that the usual macroscopic linear interpretation of the test can also be performed at the single crystal scale, allowing the identification of local apparent piezoelectric and elastic properties. It is also shown that despite this apparent linearity, the blocking force test involves significant non-linear behaviour mostly due to domain switching under electric field and stress. Although affecting a limited volume fraction of the material, domain switching is responsible for a large part of the macroscopic strain and explains the high level of inter- and intra-granular stresses observed during the course of the experiment. The study shows that if apparent piezoelectric and elastic properties can be identified for PZT single crystals from blocking stress curves, they may be very different from the actual properties of polycrystalline materials due to the multiplicity of the physical mechanisms involved. These apparent properties can be used for macroscopic modelling purposes but should be considered with caution if a local analysis is aimed at.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗
DOE OSTI2015

Reduced leakage current and improved ferroelectricity in magneto-electric composite ceramics prepared with microwave assisted radiant hybrid sintering

Structural, electrical and magnetic properties of magneto-electric composite ceramics viz., 0.9 BaTi{sub 0.95}Sn{sub 0.05}O{sub 3} (BTSO)- 0.1 Ni{sub 0.8}Zn{sub 0.2}Fe{sub 2}O{sub 4} (NZFO) prepared with microwave assisted radiant hybrid sintering (MARH) are reported. Phase purity and isovalent substitution of Ti{sup 4+} by Sn{sup 4+} of the samples is confirmed from x-ray diffraction and {sup 119}Sn Mossbauer measurements respectively. Significant suppression of leakage current and improvement of ferroelectricity is observed for the composites prepared with MARH. The observed results are explained in terms of uniform dispersion of ferrite (NZFO) phase in the ferroelectric (BTSO) matrix as evidenced from back-scattered scanning electron micrographs.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Fire resistance properties of ceramic wool fiber reinforced intumescent coatings

This research studied the effects of varied weight percentage and length of ceramic wool fiber (CWF) reinforcement to fire retardant performance of epoxy-based intumescent coating. Ten formulations were developed using ammonium polyphosphate (APP), expandable graphite (EG), melamine (MEL) and boric acid (BA). The mixing was conducted in two stages; powdered materials were grinded in Rocklabs mortar grinder and epoxy-mixed using Caframo mixer at low speed mixing. The samples were applied on mild steel substrate and exposed to 500°C heat inside Carbolite electric furnace. The char expansion and its physical properties were observed. Scanning electron microscopy (SEM) analyses were conducted to inspect the fiber dispersion, fiber condition and the cell structure of both coatings and chars produced. Thermogravimetric analyses (TGA) were conducted to study the thermal properties of the coating such as degradation temperature and residual weight. Fire retardant performance was determined by measuring backside temperature of substrate in 1-hour, 1000°C Bunsen burner test according to UL 1709 fire regime. The results showed that intumescent coating reinforced with CWF produced better fire resistance performance. When compared to unreinforced coating, formulation S6-15 significantly reduced steel temperature at approximately 34.7% to around 175°C. However, higher fiber weight percentage had slightly decreased fire retardant performance of the coating.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Improvement of the piezoelectric properties in (K,Na)NbO{sub 3}-based lead-free piezoelectric ceramic with two-phase co-existing state

Two phases of (K,Na)NbO{sub 3} (KNN) co-exist in a KNN-based composite lead-free piezoelectric ceramic 0.910(K{sub 1−x}Na{sub x}){sub 0.86}Ca{sub 0.04}Li{sub 0.02}Nb{sub 0.85}O{sub 3−δ}–0.042K{sub 0.85}Ti{sub 0.85}Nb{sub 1.15}O{sub 5} –0.036BaZrO{sub 3}–0.0016Co{sub 3}O{sub 4}– 0.0025Fe{sub 2}O{sub 3}–0.0069ZnO system, over a wide range of Na fractions, where 0.56 ≤ x ≤ 0.75. The crystal systems of the two KNN phases are identified to tetragonal and orthorhombic by analyzing the synchrotron powder X-ray diffraction (XRD) data, high-resolution transmission electron microscopy (HR-TEM), and selected-area electron diffraction (SAD). In the range 0.33 ≤ x ≤ 0.50, the main component of the composite system is found to be single-phase KNN with a tetragonal structure. Granular nanodomains of the orthorhombic phase dispersed in the tetragonal matrix have been identified by HR-TEM and SAD for 0.56 ≤ x ≤ 0.75. Only a trace amount of the orthorhombic phase has been found in the SAD patterns at the composition x = 0.56. However, the number of orthorhombic nanodomains gradually increases with increasing Na content up to x < 0.75, as observed from the HR-TEM images. An abrupt increase and agglomeration of the nanodomains are observed at x = 0.75, where weak diffraction peaks of the orthorhombic phase have also become detectable from the XRD data. The maximum value of the electromechanical coupling coefficient, k{sub p} = 0.56, has been observed at the composition x = 0.56.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2015

The gas phase emitter effect of lanthanum within ceramic metal halide lamps and its dependence on the La vapor pressure and operating frequency

The gas phase emitter effect increases the lamp lifetime by lowering the work function and, with it, the temperature of the tungsten electrodes of metal halide lamps especially for lamps in ceramic vessels due to their high rare earth pressures. It is generated by a monolayer on the electrode surface of electropositive atoms of certain emitter elements, which are inserted into the lamp bulb by metal iodide salts. They are vaporized, dissociated, ionized, and deposited by an emitter ion current onto the electrode surface within the cathodic phase of lamp operation with a switched-dc or ac-current. The gas phase emitter effect of La and the influence of Na on the emitter effect of La are studied by spatially and phase-resolved pyrometric measurements of the electrode tip temperature, La atom, and ion densities by optical emission spectroscopy as well as optical broadband absorption spectroscopy and arc attachment images by short time photography. An addition of Na to the lamp filling increases the La vapor pressure within the lamp considerably, resulting in an improved gas phase emitter effect of La. Furthermore, the La vapor pressure is raised by a heating of the cold spot. In this way, conditions depending on the La vapor pressure and operating frequency are identified, at which the temperature of the electrodes becomes a minimum.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2015

Structural, electrical and electrochemical properties of Li{sub 4}Zr{sub x}Si{sub 1-x}O{sub 4} (0.02 ≤ x ≤ 0.06) ceramic electrolytes

The aim of this work was to investigate the structural, electrical and electrochemical properties of Li{sub 4}Zr{sub x}Si{sub 1-x}O{sub 4} (0.02 ≤ x ≤ 0.06) compounds prepared via sol gel method. The X-ray Diffraction results showed that all compounds can be indexed to monoclinic structure in space group P2{sub 1/m}. The Li{sub 4}Zr{sub 0.06}Si{sub 0.94}O{sub 4} compound showed highest bulk, grain boundary and total conductivity values of 1.19 × 10{sup −4} S cm{sup −1}, 4.75 × 10{sup −5} S cm{sup −1} and 3.41 × 10{sup −5} S cm{sup −1} respectively. The insertion of Zr{sup 4+} is found to enhance conductivity of the parent sample Li{sub 4}SiO{sub 4}. Linear sweep voltammetry results showed that Li{sub 4}Zr{sub 0.06}Si{sub 0.94}O{sub 4} ceramic electrolytes was electrochemically stable up to 5.07 V versus a Li{sup +}/Li{sup +} reference electrode.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2015

Strong domain configuration dependence of the nonlinear dielectric response in (K,Na)NbO{sub 3}-based ceramics

The nonlinear dielectric response in (Na{sub 0.52}K{sub 0.4425}Li{sub 0.0375})(Nb{sub 0.92−x}Ta{sub x}Sb{sub 0.08})O{sub 3} ceramics with different amounts of Ta was measured using subcoercive electric fields and quantified by the Rayleigh model. The irreversible extrinsic contribution, mainly caused by the irreversible domain wall translation, was strongly dependent on the domain configuration. The irreversible extrinsic contributions remained approximately the same within the single-phase regions, either orthorhombic or tetragonal, due to the similar domain morphology. However, in the polymorphic phase transition region, the domain wall density was increased by minimized domain size, as observed by transmission electron microscopy. This resulted in constrained domain wall motion due to self-clamping and reduced the irreversible extrinsic contribution.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗
DOE OSTI2015

Atomic-scale microstructure underneath nanoindentation in Al-Cr-N ceramic films

In this work, Al-Cr-N ceramic films deformed by nanoindentation were peeled off from silicon substrates and their atomic-scale microstructures underneath the indenter were investigated by high resolution transmission electron microscope (HR-TEM). Dislocations were formed underneath the indenter and they accumulated along nano-grain boundaries. The accumulative dislocations triggered the crack initiation along grain boundaries, and further resulted in the crack propagation. Dislocations were also observed in nano-grains on the lateral contact area. A model was proposed to describe the variation of microstructures under nanoindentation.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Strain profiles in ion implanted ceramic polycrystals: An approach based on reciprocal-space crystal selection

The determination of the state of strain in implanted materials is a key issue in the study of their mechanical stability. Whereas this question is nowadays relatively easily solved in the case of single crystals, it remains a challenging task in the case of polycrystalline materials. In this paper, we take benefit of the intense and parallel beams provided by third generation synchrotron sources combined with a two-dimensional detection system to analyze individual grains in polycrystals, hence obtaining “single crystal-like” data. The feasibility of the approach is demonstrated with implanted UO{sub 2} polycrystals where the in-depth strain profile is extracted for individual grains using numerical simulations of the diffracted signal. The influence of the implantation dose is precisely analyzed for several diffracting planes and grains. This work suggests that, at low fluences, the development of strain is mainly due to ballistic effects with little effect from He ions, independently from the crystallographic orientation. At higher fluences, the evolution of the strain profiles suggests a partial and anisotropic plastic relaxation. With the present approach, robust and reliable structural information can be obtained, even from complex polycrystalline ceramic materials.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗
DOE OSTI2016

Short range ferromagnetic, magneto-electric, and magneto-dielectric effect in ceramic Co{sub 3}TeO{sub 6}

We report observation of magneto-electric and magneto-dielectric couplings along with short range ferromagnetic order in ceramic Cobalt Tellurate (Co{sub 3}TeO{sub 6}, CTO) using magnetic, structural, dielectric, pyroelectric, and polarization studies. DC magnetization along with dielectric constant measurements indicate a coupling between magnetic order and electrical polarization. A strong anomaly in the dielectric constant at ∼17.4 K in zero magnetic field indicates spontaneous electric polarization, consistent with a recent neutron diffraction study. Observation of weak short range ferromagnetic order at lower temperatures is attributed to the Griffiths-like ferromagnetism. Furthermore, magnetic field dependence of the ferroelectric transition follows earlier theoretical predictions, applicable to single crystal CTO. Finally, combined dielectric, pyroelectric, and polarization measurements suggest that the ground state of CTO may possess spontaneous symmetry breaking in the absence of magnetic field.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗
DOE OSTI2016

High thermal behavior of a new glass ceramic developed from silica xerogel/SnO{sub 2} composite

In this investigation, a new glass ceramics have been produced by mixing SnO{sub 2} and amorphous silica xerogel (ASX) extracted from sago waste ash. The composition has been prepared by adding 10 mol% of SnO{sub 2} into SX. The samples have been dry pressed and sintered in the temperature range between 800 °C and 1500 °C. The effects of temperature on the crystallization of silica xerogel after adding SnO{sub 2} and their relationship to bulk density have been studied. The crystallization process of the silica xerogel/SnO{sub 2} composite has been examined by an X-ray diffraction (XRD) and the bulk density has been characterized on the basis of the experimental data obtained using Archimedes′ principle. It has been found that an addition of SnO{sub 2} confers an appreciable effect on the grain and from the interpretation of XRD patterns allow one to explain the increase in the density by an increased crystallite size of SnO{sub 2} in the composite.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Effect of crystal structure and cationic order on phonon modes across ferroelectric phase transformation in Pb(Fe{sub 0.5-x}Sc{sub x}Nb{sub 0.5})O{sub 3} bulk ceramics

Pb(Fe{sub 0.5-x}Sc{sub x}Nb{sub 0.5})O{sub 3} [(PFSN) (0 ≤ x ≤ 0.5)] multiferroic relaxors were synthesized and the temperature dependence of phonon modes across ferroelectric to paraelectric transition was studied. With varying Sc content from x = 0 to 0.25 the structure remains monoclinic and with further addition (x = 0.3 - 0.5) the structure transforms into rhombohedral symmetry. Structural refinement studies showed that the change in crystal structure from monoclinic to rhombohedral symmetry involves a volume increment of 34-36%. Associated changes in the tolerance factor (1.024 ≤ t ≤ 0.976) and bond angles were observed. Structure assisted B′-B″ cation ordering was confirmed through the superlattice reflections in selected area electron diffraction (SAED) pattern of Pb(Sc{sub 0.5}Nb{sub 0.5})O{sub 3} (x = 0.5). Cation ordering is also evident from the evolution of Pb-O phonon mode in Raman spectra of compositions with rhombohedral symmetry (x ≥ 0.3). The high temperature Raman scattering studies show that the B-localized mode [F{sub 1u}, ∼250 cm{sup −1}] and BO{sub 6} octahedral rotational mode [F{sub 1g}, ∼200 cm{sup −1}], both originating from polar nano regions (PNRs) behave like coupled phonon modes in rhombohedral symmetry. However, in monoclinic symmetry they behave independently across the transition. Softening of B localized mode across the transition followed by the hardening for all compositions confirms the diffusive nature of the ferroelectric transformation. The presence of correlation between the B localized and BO{sub 6} rotational modes introduces a weak relaxor feature for systems with rhombohedral symmetry in PFSN ceramics, which was confirmed from the macroscopic dielectric studies.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Cubic to tetragonal phase transition of Tm{sup 3+} doped nanocrystals in oxyfluoride glass ceramics

Tm{sup 3+} ions doped β-PbF{sub 2} nanocrystals in oxyfluoride glass ceramics with different doping concentrations and thermal temperatures are prepared by a traditional melt-quenching and thermal treatment method to investigate the structure and the phase transition of Tm{sup 3+} doped nanocrystals. The structures are characterized by X-ray diffraction Rietveld analysis and confirmed with numerical simulation. The phase transitions are proved further by the emission spectra. Both of the doping concentration and thermal temperature can induce an O{sub h} to D{sub 4h} site symmetry distortion and a cubic to tetragonal phase transition. The luminescence of Tm{sup 3+} doped nanocrystals at 800 nm was modulated by the phase transition of the surrounding crystal field.

36 MATERIALS SCIENCE↗