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At least 1,045 records · Page 58
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DOE OSTI2015

Effect of Al{sup 3+} substitution on the structural, magnetic, and electric properties in multiferroic Bi{sub 2}Fe{sub 4}O{sub 9} ceramics

Structural, magnetic, and electric properties have been investigated in polycrystalline Bi{sub 2}(Fe{sub 1−x}Al{sub x}){sub 4}O{sub 9} (0≤x≤0.25) ceramics synthesized by a modified Pechini method. Structural analysis reveals that Al{sup 3+} doped Bi{sub 2}Fe{sub 4}O{sub 9} crystallizes in orthorhombic structure with Pbnm space group. Surface morphology of the end products is examined by scanning electron microscopy and the grain size has a tendency to decrease with increase in Al{sup 3+} doping level. Compared with pure Bi{sub 2}Fe{sub 4}O{sub 9}, room temperature coexistent multiferroic-like behavior is observed in Al{sup 3+} doped Bi{sub 2}Fe{sub 4}O{sub 9}. By analyzing magnetic properties, the Néel temperature monotonously shifts to low temperatures from ~260 K (x=0) to ~35 K (x=0.25). Moreover, the spin dynamic measured by the shift in ac magnetic susceptibility as a function of frequency provides a possibility of spin-glass-like behavior, which is further confirmed by fitting the critical slowing down power law and memory effect. - Graphical abstract: Compared with pure Bi{sub 2}Fe{sub 4}O{sub 9}, room temperature weak ferromagnetic property and enhanced ferroelectric-like behavior can be achieved simultaneously with proper Al{sup 3+} doping. - Highlights: • Bi{sub 2}(Fe{sub 1−x}Al{sub x}){sub 4}O{sub 9} (0≤x≤0.25) ceramics are fabricated via a Pechini method. • Weak ferromagnetic and ferroelectric behaviors can be achieved simultaneously. • Spin-glass-like behavior is detected with proper Al{sup 3+} doping. • The memory and aging effects are observed with proper Al{sup 3+} doping.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2016

Relationship between ferroelectric properties and local structure of Pb{sub 1−x}Ba{sub x}Zr{sub 0.40}Ti{sub 0.60}O{sub 3} ceramic materials studied by X-ray absorption and Raman spectroscopies

This paper reports on the structural characterization of Pb{sub 1−x}Ba{sub x}Zr{sub 0.40}Ti{sub 0.60}O{sub 3} (PBZT) ferroelectric ceramic compositions prepared by the conventional solid state reaction method. X-ray absorption spectroscopy (XAS) and Raman spectroscopy were used in the probing of the local structure of PBZT samples that exhibit a normal or relaxor ferroelectric behavior. They showed a considerable local disorder around Zr and Pb atoms in the samples of tetragonal or cubic long-range order symmetry. The intensity of the E(TO{sub 3}) mode in the Raman spectra of PBZT relaxor samples remains constant at temperatures lower than T{sub m}, which has proven the stabilization of the correlation process between nanodomains. - Graphical abstract: X-ray absorption measurements showed considerable local disorder around Zr and Pb atoms in the samples of tetragonal or cubic long-range order symmetry. The intensity of the E(TO{sub 3}) mode in the Raman spectra of PBZT relaxor samples remains constant at temperatures lower than T{sub m}, which has proven the stabilization of the correlation process between nanodomains. Display Omitted - Highlights: • Structural characterization of Pb{sub 1−x}Ba{sub x}Zr{sub 0.40}Ti{sub 0.60}O{sub 3} (PBZT) ferroelectric ceramic. • X-ray absorption and Raman spectroscopies were used to probe the structure of PBZT. • Dissymmetry of Zr and Pb sites was observed in samples long-range cubic symmetry. • Local disorder in all PBZT samples through the observation of Raman active modes.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2017

Mechanism of γ-irradiation induced phase transformations in nanocrystalline Mn{sub 0.5}Zn{sub 0.5}Fe{sub 2}O{sub 4} ceramics

The structural, infrared absorption and magnetic property transformations in nanocrystalline Mn{sub 0.5}Zn{sub 0.5}Fe{sub 2}O{sub 4} samples irradiated with different doses (0, 15, 25 and 50 kGy) of γ-irradiation were investigated in this work and a mechanism of phase transformation/decomposition is provided based on the metastable nature of the Mn-atoms in the spinel lattice. The nano-powder sample was prepared by solution combustion route and the pellets of the sample were exposed to γ-radiation. Up to a dose of 25 kGy of γ-radiation, the sample retained the single phase cubic spinel (Fd-3m) structure, but the disorder in the sample increased. On irradiating the sample with 50 kGy γ-radiation, the spinel phase decomposed into new stable phases such as α-Fe{sub 2}O{sub 3} and ZnFe{sub 2}O{sub 4} phases along with amorphous MnO phase, leading to a change in the surface morphology of the sample. Along with the structural transformations the magnetic properties deteriorated due to breakage of the ferrimagnetic order with higher doses of γ-irradiation. Our results are important for the understanding of the stability, durability and performance of the Mn-Zn ferrite based devices used in space applications. - Graphical abstract: The nanocrystalline Mn{sub 0.5}Zn{sub 0.5}Fe{sub 2}O{sub 4} ceramic sample transforms to crystalline α-Fe{sub 2}O{sub 3} and ZnFe{sub 2}O{sub 4} phases (and amorphous MnO phase) at a γ-irradiation dose of 50 kGy, as MnO goes out of the spinel lattice. The high energy γ-irradiation causes structural damage to the nanomaterials leading to change in morphology of the sample as seen in the SEM images. - Highlights: • Mn atoms are more unstable in the Mn-Zn ferrite spinel lattice than Zn-atoms. • Displacement of Mn atoms by γ-radiation from the lattice renders phase transformation. • In Mn{sub 0.5}Zn{sub 0.5}Fe{sub 2}O{sub 4}, Mn-ferrite cell transforms to crystalline α-Fe{sub 2}O{sub 3} and amorphous MnO. • The stable ZnFe{sub 2}O{sub 4} phase retains its structure even after 50 KGy γ-irradiation. • The γ-irradiation degrades the magnetic properties of Mn{sub 0.5}Zn{sub 0.5}Fe{sub 2}O{sub 4} ceramics.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2014

High energy X-ray diffraction study of a dental ceramics–titanium functional gradient material prepared by field assisted sintering technique

A functional gradient material with eleven layers composed of a dental ceramics and titanium was successfully consolidated using field assisted sintering technique in a two-step sintering process. High energy X-ray diffraction studies on the gradient were performed at High Energy Material Science beamline at Desy in Hamburg. Phase composition, crystal unit edges and lattice mismatch along the gradient were determined applying Rietveld refinement procedure. Phase analysis revealed that the main crystalline phase present in the gradient is α-Ti. Crystallinity increases stepwisely along the gradient with a decreasing increment between every next layer, following rather the weight fraction of titanium. The crystal unit edge a of titanium remains approximately constant with a value of 2.9686(1) Å, while c is reduced with increasing amount of titanium. In the layer with pure titanium the crystal unit edge c is constant with a value of 4.7174(2) Å. The lattice mismatch leading to an internal stress was calculated over the whole gradient. It was found that the maximal internal stress in titanium embedded in the studied gradient is significantly smaller than its yield strength, which implies that the structure of titanium along the whole gradient is mechanically stable. - Highlights: • High energy XRD studies of dental ceramics–Ti gradient material consolidated by FAST. • Phase composition, crystallinity and lattice parameters are determined. • Crystallinity increases stepwisely along the gradient following weight fraction of Ti. • Lattice mismatch leading to internal stress is calculated over the whole gradient. • Internal stress in α-Ti embedded in the gradient is smaller than its yield strength.

36 MATERIALS SCIENCE↗
DOE OSTI2014

Direct observation of Nd{sup 3+} and Tm{sup 3+} ion distributions in oxy-fluoride glass ceramics containing PbF{sub 2} nanocrystals

Nd{sup 3+} and Tm{sup 3+}, doped oxy-fluoride glasses and glass ceramics were prepared by conventional melt-quenching and subsequent heat-treatment, respectively. β-PbF{sub 2} nanocrystals with diameter 50 –100 nm formed in the glass matrix after heat treatment. The Stark splitting in absorption peaks, enhanced photoluminescence and prolonged lifetimes that β-PbF{sub 2} nanocrystal formation increased the luminescence of rare earth ions. Both Nd{sup 3+} and Tm{sup 3+} ions were incorporated into nanocrystals that were enriched in lead and fluorine, and deficient in oxygen. - Highlights: • EELS analysis for rare-earth ion distribution in oxy-fluoride glass ceramics • No significant changes in lifetimes of Nd{sup 3+}, while obvious change for Tm{sup 3+} • Direct evidence of Nd{sup 3+} and Tm{sup 3+} aggregation into fluoride nanocrystals.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Controlling the sol–gel process of nano-crystalline lithium-mica glass-ceramic by its chemical composition and synthesis parameters

This paper aims to explore the impact of the parameters such as pH of the system, refluxing temperature, water quantity and chemical composition on the sol–gel synthesis of lithium-mica glass-ceramic nano-powder. The synthesis process was accomplished using two chemical composition formula (Li{sub (1+x)}Mg{sub 3}AlSi{sub 3(1+x)}O{sub 10+6.5x}F{sub 2} and LiMg{sub 3}AlSi{sub 3(1+x)}O{sub 10+6x}F{sub 2}). X-ray diffraction, Brunauer–Emmett–Teller surface area measurement and scanning electron microscopy techniques were applied to evaluate a variety of as-synthesized samples. Consequently, a transparent homogeneous sol was obtained under the conditions as pH ≤ 4, synthesis temperature ≤ 50 °C, and mol ratio of water to chemicals ≤ 2. The prepared nano-powders under such conditions were in the range of 60–100 nm. The results also revealed that the mica glass-ceramics prepared based on the composition Li{sub (1+x)}Mg{sub 3}AlSi{sub 3(1+x)}O{sub 10+6.5x}F{sub 2} possessed finer powders due to their slow hydrolysis process. Moreover, any reduction in the stoichiometric deviation of lithium mica (x) leads to acquiring finer powders. - Highlights: • A transparent homogeneous sol leads to prepare nanopowders in the range of 60–100 nm. • The particles synthesized at lower temperatures possess finer sizes. • The acquired product which is prepared with excessive water offers larger sizes. • Any reduction in stoichiometric deviation leads to acquiring finer powders. • Taking synthesis composition as Li{sub (1+x)}Mg{sub 3}AlSi{sub 3(1+x)}O{sub 10+6.5x}F{sub 2} offers finer powders.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Densification, microstructure and properties of TiB2 ceramics fabricated by spark plasma sintering

Highlights: • Nearly full densification of in-house processed TiB{sub 2} ceramic powders at 1500 °C. • Microstructures revealing the size and shape of TiB{sub 2} grains after SPS. • The effect of sub-micron particles on the densification during SPS. • The effect of sintering pressure on the microstructure. • Microhardness and nano-indentation measurements along with oxidation studies. - Abstract: This study reports the fabrication of high-density TiB{sub 2} ceramics at reduced temperatures (1500 °C) by using field assisted sintering technology/spark plasma sintering (FAST/SPS) technique. In-house processed TiB{sub 2} powders with high purity were employed as starting materials. The effects of SPS conditions on the sintering behavior and microstructure of TiB{sub 2} were investigated. Sub-micron character of TiB{sub 2} particles has a strong influence on the densification during SPS. Microstructural analyses revealed that the high pressure affected both the grain size and the shape of TiB{sub 2} crystallites. Elongated grains with average size of 6 μm were perceived in TiB{sub 2} sample fabricated by SPS at 1500 °C under 60 MPa pressure with a relative density of 96.7%. The microhardness and elastic modulus were measured as 27.4 GPa and 685.2 GPa, respectively. This sample revealed an improved oxidation resistance due to the formation of a thin oxidation layer on the surface when heated up to 1200 °C.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Advanced ceramic components with embedded sapphire optical fiber sensors for high temperature applications

Here this paper describes an extrusion-based additive manufacturing process that has been developed to enable embedment of sapphire optical fiber sensors in ceramic components during the part fabrication. In this process, an aqueous paste of ceramic particles is extruded through a moving nozzle to build the part layer-by-layer. In the case of sensor embedment, the fabrication process is halted after a certain number of layers have been deposited; the sensors are placed in their predetermined locations, and the remaining layers are deposited until the part fabrication is completed. Because the sensors are embedded during the fabrication process, they are fully integrated with the part and the problems of traditional sensor embedment can be eliminated. Scanning electron microscopy was used to observe the embedded sensors and to detect any possible flaws in the part or embedded sensor. Attenuation of the sensors was measured in near-infrared region (1500–1600 nm wavelength). Standard test methods were employed to examine the effect of embedded fibers on the strength and hardness of the parts. The results indicated that the sapphire fiber sensors with diameters smaller than 250 micrometers were able to endure the freeform extrusion fabrication process and the post-processing without compromising the part properties.

36 MATERIALS SCIENCE↗
DOE OSTI2013

Structural evolution, sintering behavior and microwave dielectric properties of (1−x)Li{sub 2}TiO{sub 3} + xLiF ceramics

Graphical abstract: - Highlights: • Structure, sinterability and dielectric properties of LiF-doped Li{sub 2}TiO{sub 3} were studied. • Li{sub 2}TiO{sub 3} can be densitied (TD 98%) at lower sintering temperature by LiF additions. • Excellent microwave dielectric properties could be obtained. - Abstract: Structural evolution, sintering behavior, and microwave dielectric properties of (1−x)Li{sub 2}TiO{sub 3} + xLiF (0.05 ≤ x ≤ 0.70) ceramics have been studied by X-ray diffraction (XRD), Scanning Electron Microscopy (SEM), Raman spectra, thermal dilatometry and microwave resonant measurement at the frequency of about 7–11 GHz. The results show that Li{sub 2}TiO{sub 3} can form limited solid solution with LiF (x ≤ 0.4) and LiF second phase appeared when x{sup 3}0.5. The structure of the solid solution transformed from ordered monoclinic phase (β-Li{sub 2}TiO{sub 3} (ss)) to disordered cubic rock salt (α-Li{sub 2}TiO{sub 3} (ss)) when x{sup 3}0.15. The presence of short range ordering was confirmed for the cubic phase. The sinterability was considerably improved by doping with LiF. Densified ceramics with about 95–98% theoretical density could be obtained for the doped compositions after sintering at 900–1150 °C/2 h. An optimized microwave dielectric properties with ε{sub r} of ∼23.6, Q × f of ∼108,000 GHz and τ{sub f} of ∼4.2 ppm/°C could be obtained for the x = 0.1 composition after sintering at 1100 °C/2 h.

36 MATERIALS SCIENCE↗
DOE OSTI2013

Blocking effect of crystal–glass interface in lanthanum doped barium strontium titanate glass–ceramics

Graphical abstract: The blocking effect of the crystal–glass interface on the carrier transport behavior in the lanthanum doped barium strontium titanate glass–ceramics: preparation and characterization. - Highlights: • La{sub 2}O{sub 3} addition promotes the crystallization of the major crystalline phase. • The Z″ and M″ peaks exist a significant mismatch for 0.5 mol% La{sub 2}O{sub 3} addition. • The Z″ and M″ peaks separate obviously for 1.0 mol% La{sub 2}O{sub 3} addition. • Crystallite impedance decreases while crystal–glass interface impedance increases. • La{sub 2}O{sub 3} addition increases blocking factor of the crystal–glass interface. - Abstract: The microstructures and dielectric properties in La{sub 2}O{sub 3}-doped barium strontium titanate glass–ceramics have been investigated by scanning electron microscopy (SEM) and impedance spectroscopy. SEM analysis indicated that La{sub 2}O{sub 3} additive decreases the average crystallite size. Impedance spectroscopy revealed that the positions of Z″ and M″ peaks are close for undoped samples. When La{sub 2}O{sub 3} concentration is 0.5 mol%, the Z″ and M″ peaks show a significant mismatch. Furthermore, these peaks separate obviously for 1.0 mol% La{sub 2}O{sub 3} addition. With increasing La{sub 2}O{sub 3} concentration, the contribution of the crystallite impedance becomes smaller, while the contribution of the crystal–glass interface impedance becomes larger. More interestingly, it was found that La{sub 2}O{sub 3} additive increases blocking factor of the crystal–glass interface in the temperature range of 250–450 °C. This may be attributed to a decrease of activation energy of the crystallite and an increase of the crystal–glass interface area.

36 MATERIALS SCIENCE↗
DOE OSTI2014

Dielectric behavior of samarium-doped BaZr{sub 0.2}Ti{sub 0.8}O{sub 3} ceramics

Graphical abstract: - Highlights: • We investigate dielectric properties and phase transition of Sm{sup 3+}-doped BaZr{sub 0.2}Ti{sub 0.8}O{sub 3} ceramics. • The additive amount of Sm{sub 2}O{sub 3} can greatly affect the dielectric properties. • The materials undergo a diffuse type ferroelectric phase transition. • There is an alternation of substitution preference of Sm{sup 3+} ion for the host cations in perovskite lattice. - Abstract: The dielectric properties and phase transition of Sm{sup 3+}-doped BaZr{sub 0.2}Ti{sub 0.8}O{sub 3} (BZT20) ceramics were investigated. Room temperature X-ray diffraction study suggested that the compositions had single-phase cubic symmetry. Microstructure studies showed that the grain size decreased and that the Sm{sub 2}O{sub 3} amount markedly affected the dielectric properties of BZT20. A dielectric constant of 5700 at 0.2 mol% Sm{sub 2}O{sub 3} and a dissipation factor of only 0.0011 at 2 mol% Sm{sub 2}O{sub 3} were observed, indicating that BZT20 had significant potential applications. Moreover, the dielectric constant, dissipation factor, phase-transition temperature, and maximum dielectric constant increased with increased Sm{sub 2}O{sub 3} amount at ≤0.2 mol% Sm{sub 2}O{sub 3} but decreased with increased Sm{sub 2}O{sub 3} amount at >0.2 mol% Sm{sub 2}O{sub 3}.

36 MATERIALS SCIENCE↗
DOE OSTI2014

Dielectric and electrical studies of Pr{sup 3+} doped nano CaSiO{sub 3} perovskite ceramics

Highlights: • CaSiO{sub 3}:Pr{sup 3+} was prepared by facile low temperature solution combustion method. • The crystalline phase of the product is obtained by adopting sintering method. • Samples prepared at 500 °C and calcined at 900 °C for 3 h showed β-phase. • The Pr{sup 3+} doped CaSiO{sub 3} shows “unusual results”. • The electrical microstructure has been accepted to be of internal barrier layer capacitor. - Abstract: CaSiO{sub 3} nano-ceramic powder doped with Pr{sup 3+} has been prepared by solution combustion method. The powder Ca{sub 0.95}Pr{sub 0.05}SiO{sub 3} is investigated for its dielectric and electrical properties at room temperature to study the effect of doping. The sample is characterized by X-ray diffraction and infrared spectroscopy. The size of either of volume elements of CaSiO{sub 3}:Pr{sup 3+} estimated from transmission electron microscopy is about 180–200 nm. The sample shows colossal dielectric response at room temperature. This colossal dielectric behaviour follows Debye-type relaxation and can be explained by Maxwell–Wagner (MW) polarization. However, analysis of impedance and electric modulus data using Cole–Cole plot shows that it deviates from ideal Debye behaviour resulting from the distribution of relaxation times. The distribution in the relaxation times may be attributed to existence of electrically heterogeneous grains, insulating grain boundary, and electrode contact regions. Doping, thus, results in substantial modifications in the dielectric and electrical properties of the nano-ceramic CaSiO{sub 3}.

36 MATERIALS SCIENCE↗
DOE OSTI2014

Piezo-/dielectric properties of perovskite-structure high-temperature relaxor ferroelectrics: The Pb(Lu{sub 1/2}Nb{sub 1/2})O{sub 3}–Pb(Zn{sub 1/3}Nb{sub 2/3})O{sub 3}–PbTiO{sub 3} ternary ceramics

Graphical abstract: - Highlights: • Pb(Zn{sub 1/3}Nb{sub 2/3})O{sub 3}-based ternary ferroelectric ceramics were prepared by solid-state synthesis method. • Morphotropic phase boundary region has been determined by XRD, di-/piezoelectric properties. • The compositions near MPB region exhibit excellent piezoelectric properties. - Abstract: A new compositional system of relaxor ferroelectrics was investigated based on the high piezoelectricity Pb(Zn{sub 1/3}Nb{sub 2/3})O{sub 3}–PbTiO{sub 3} ferroelectric perovskite family. Compositions were fabricated near an estimated morphotropic phase boundary (MPB) of the Pb(Lu{sub 1/2}Nb{sub 1/2})O{sub 3}–Pb(Zn{sub 1/3}Nb{sub 2/3})O{sub 3}–PbTiO{sub 3} (PLZNT) ternary system by a two-step synthetic process. Their structures have been analyzed by means of X-ray diffraction technique. On the basis of X-ray powder diffraction, the morphotropic phase boundary (MPB) region for the ternary system was obtained. The Curie temperature T{sub C} of ternary system varied from 240 °C to 330 °C and the coercive fields E{sub c}s > 10 kV/cm. The values of piezoelectric coefficients d{sub 33} vary in the range of 260–450 pC/N with different PZN contents. It is worth noting that the optimum compositions were located at MPB region but near the tetragonal phase. The new PLZNT ceramics exhibit wider range of T{sub C}s and E{sub c}s, making it a promising material for high-powder ultrasound transducers using in a large temperature range.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Structure, sintering behavior, and microwave dielectric properties of (1 − x) CaWO{sub 4}–xYLiF{sub 4} (0.02 ≤ x ≤ 0.10) ceramics

Highlights: • Structure, sinterability, and dielectric properties of CaWO{sub 4}–YLiF{sub 4} were studied. • CaWO{sub 4} can be densified (TD 97%) at 750 °C/2 h by YLiF{sub 4} doping. • Excellent microwave dielectric properties could be obtained. - Abstract: Structures and sintering behaviors of (1 − x) CaWO{sub 4}–xYLiF{sub 4} (0.02 ≤ x ≤ 0.10) ceramic have been investigated by X-ray powder diffraction (XRD), dilatometry, scanning electron microscopy (SEM) in this work. The microwave dielectric properties were measured with a network analyzer at the frequency of about 8–15 GHz. Limited solid solution could be formed within the compositional range of x < 0.1. The sintering temperature of CaWO{sub 4} could successfully be reduced to ∼750 °C/2 h by doping with small amount of YLiF{sub 4}. An optimized microwave dielectric properties with ϵ{sub r} = 10.5, Q × f = 73 000 GHz and τ{sub f} = −37.7 ppm/°C could be obtained after sintered at the 750 °C for 2 h for x = 0.04 compositions. XRD and back scattering SEM analysis indicated that the (1 − x) CaWO{sub 4}–xYLiF{sub 4} (x = 0.04) ceramic could be chemically compatible with Ag after sintering at 750 °C/2 h.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Photoluminescence, enhanced ferroelectric, and dielectric properties of Pr{sup 3+}-doped SrBi{sub 2}Nb{sub 2}O{sub 9} multifunctional ceramics

Pr{sup 3+}-doped SrBi{sub 2}Nb{sub 2}O{sub 9} (SBN) multifunctional ceramics were synthesized by the conventional solid state method. The photoluminescence (PL) excitation and emission spectra, enhanced ferroelectric and dielectric properties were investigated. The X-ray diffraction (XRD) and FESEM analyses indicated that the samples were simple phase and uniform flake-structure. Under the 250–350 nm ultraviolet (UV) excitations, the red emission was obtained and the optimal emission intensity was investigated when Pr doping level was 0.005 mol. With the increasing of the Pr{sup 3+} ion contents, the ferroelectric properties were enhanced obviously. As a new multifunctional material, the Pr{sup 3+}-doped SBN ceramics could be used for a wide range of application, such as integrated electro-optical devices.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2015

Effects of rare earth ionic doping on microstructures and electrical properties of CaCu{sub 3}Ti{sub 4}O{sub 12} ceramics

Graphical abstract: The dielectric constant decreases monotonically with reduced RE doping ion radius and is more frequency independent compared with that of pure CCTO sample. - Highlights: • The mean grain sizes decrease monotonically with reduced RE doping ionic radius. • Doping gives rise to the monotonic decrease of ϵ{sub r} with reduced RE ionic radius. • The nonlinear coefficient and breakdown field increase with RE ionic doping. • α of all the samples is associated with the potential barrier width rather than Φ{sub b}. - Abstract: Ca{sub 1–x}R{sub x}Cu{sub 3}Ti{sub 4}O{sub 12}(R = La, Nd, Eu, Gd, Er; x = 0 and 0.005) ceramics were prepared by the conventional solid-state method. The influences of rare earth (RE) ion doping on the microstructure, dielectric and electrical properties of CaCu{sub 3}Ti{sub 4}O{sub 12} (CCTO) ceramics were investigated systematically. Single-phase formation is confirmed by XRD analyses. The mean grain size decreases monotonically with reduced RE ion radius. The EDS results reveal that RE ionic doping reduces Cu-rich phase segregation at the grain boundaries (GBs). Doping gives rise to the monotonic decrease of dielectric constant with reduced RE ionic radius but significantly improves stability with frequency. The lower dielectric loss of doped samples is obtained due to the increase of GB resistance. In addition, the nonlinear coefficient and breakdown field increase with RE ionic doping. Both the fine grains and the enhancement of potential barrier at GBs are responsible for the improvement of the nonlinear current–voltage properties in doped CCTO samples.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Correlation among far-infrared reflection modes, crystal structures and dielectric properties of Ba(Zn{sub 1/3}Nb{sub 2/3})O{sub 3}–CaTiO{sub 3} ceramics

Highlights: • Crystal symmetry decreases with CT concentration from cubic to hexagonal structure. • Lattice constants as well as the ordered degree change with CT concentration. • Ordered structures turn from 1:1 to 1:2 ordering with change of crystal structures. • There is a correlation between FIR phonon modes and dielectric properties. • There is a correlation between FIR phonon modes and crystal structures. - Abstract: Ba(Zn{sub 1/3}Nb{sub 2/3})O{sub 3} (BZN)–CaTiO{sub 3} (CT) microwave dielectric ceramics were synthesized at 1395 °C for 4 h using conventional solid-state sintering technique with different CT contents. The ceramics were characterized by X-ray diffraction (XRD) and far-infrared reflection (FIR) spectroscopy to evaluate correlations among crystal structures, dielectric properties, and infrared modes. XRD results showed that crystal symmetry decreased with increased CT concentration from cubic to hexagonal structure, and lattice constants and ordered degree changed accordingly. Ordered phases transformed from 1:1 to 1:2 ordered structure with crystal-structure change. FIR results demonstrated that two new IR active modes appeared at 300 cm{sup −1}, and another new mode appeared at 600 cm{sup −1} for the x ≥ 0.60 sample, which agreed with the change in crystal structures as confirmed by XRD results. Correlations between FIR modes and dielectric properties were established.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Scintillation, dosimeter and optical properties of MgF2 transparent ceramics doped with Gd3+

Highlights: • We have developed MgF{sub 2}:Gd{sup 3+} transparent ceramics by SPS. • The samples showed luminescence due to the 4f-4f transitions of Gd{sup 3+}. • The 1% Gd-doped sample has high TSL sensitivity equivalent to commercial personal dosimeters. - Abstract: In this study, we have developed MgF{sub 2}:Gd transparent ceramics by spark plasma sintering (SPS) and evaluated the scintillation, dosimeter and optical properties. All the sample were successfully synthesized in a transparent form with relative densities over 99% to that of the single crystal. The samples were confirmed to show scintillation, thermally-stimulated luminescence (TSL) and optically-stimulated luminescence (OSL). The origin of these emissions was due to the 4f-4f transitions of Gd{sup 3+} appearing as a single peak at 310 nm. In particular, the TSL was very sensitive to X-rays, and especially the 1% Gd-doped sample showed a sensitivity as low as 0.1 mGy. The TSL response increases monotonically with the irradiation dose, and the dynamic range was confirmed to be over 0.1–1000 mGy, which was equivalent sensitivity to that of commercial personal dosimeters.

61 RADIATION PROTECTION AND DOSIMETRY↗