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At least 433 records · Page 24
All sourcesNASA NTRSDOE OSTI
DOE OSTI2015

The down-conversion and up-conversion photoluminescence properties of Na{sub 0.5}Bi{sub 0.5}TiO{sub 3}:Yb{sup 3+}/Pr{sup 3+} ceramics

Na{sub 0.5}Bi{sub 0.5−x−y}Yb{sub x}Pr{sub y}TiO{sub 3} (NBT:xYb/yPr) ceramics with different Yb and Pr contents are prepared. Both the down-conversion (DC) and up-conversion (UC) photoluminescence (PL) of the ceramics via 453 and 980 nm excitation, respectively, are investigated. The effect of Yb{sup 3+} and Pr{sup 3+} doping contents on the DC and UC PL is significantly different from each other. Furthermore, the UC PL of the ceramics as a function of temperatures is measured to investigate the UC process in detail. Based on energy level diagram of Pr{sup 3+} and Yb{sup 3+} ions and the DC and UC PL spectra, the DC and UC PL mechanisms of Pr{sup 3+} and Yb{sup 3+} ions are discussed. Especially, the UC PL mechanism is clarified, which is different from the previously reported literature. Also, the temperature sensing properties of the ceramics are studied based on the photoluminescence ratio technique, using the thermal coupling energy levels of Pr{sup 3+}.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗
DOE OSTI2021

Phase evolution during reactive flash sintering of Li 6.25 Al 0.25 La 3 Zr 2 O 12 starting from a chemically prepared powder

Here, reactive flash sintering (RFS) of a chemically prepared multiphase precursor powder was performed to fabricate Li 6.25 Al 0.25 La 3 Zr 2 O 12 (Al-LLZO) ceramics. This approach allowed for obtaining single-phase dense samples in a remarkably short processing time of 30 s, at a furnace temperature of 600 °C, with an electric field of 50 V cm -1 and a current limit of 150 mA mm -2 . The ceramics display high bulk conductivity of 0.18 mS cm -1 at room temperature. Furthermore, phase evolution is studied by in-situ X-ray diffraction during: i) conventional heating and ii) RFS under current rate mode. As expected, the intermediate phases progressively dissolved into the Al-LLZO matrix by conventional heating. On the other hand, RFS promoted the growth of the intermediate La 2 Zr 2 O 7 , an effect that was overcome by the thermally driven formation of Al-LLZO at higher temperatures. The observed different reaction pathway suggests that RFS can be used for stabilizing phases that are not thermodynamically favored upon conventional heating.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Highly reflective polymeric substrates functionalized utilizing atomic layer deposition

Reflective surfaces are one of the key elements of solar plants to concentrate energy in the receivers of solar thermal electricity plants. Polymeric substrates are being considered as an alternative to the widely used glass mirrors due to their intrinsic and processing advantages, but optimizing both the reflectance and the physical stability of polymeric mirrors still poses technological difficulties. In this work, polymeric surfaces have been functionalized with ceramic thin-films by atomic layer deposition. The characterization and optimization of the parameters involved in the process resulted in surfaces with a reflection index of 97%, turning polymers into a real alternative to glass substrates. The solution we present here can be easily applied in further technological areas where seemingly incompatible combinations of polymeric substrates and ceramic coatings occur.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗
DOE OSTI2016

Sintering and characterization of SrBi{sub 2}Ta{sub 2}O{sub 9} obtained by high-pressure processing at low temperatures

High-pressure processing is a very attractive approach for the production of materials with new and/or improved properties. In this work, pressures in the order of 7.7 GPa and 2.5 GPa were induced in SrBi{sub 2}Ta{sub 2}O{sub 9} samples at different temperatures placed in a specific reaction cell and generated different effects on phase formation. The microstructural evolution during high-pressure processing was investigated by scanning electron microscopy in association with energy dispersion spectroscopy and with the support of an X-ray diffraction analyzer. Frequency response analysis was used to obtain the dielectric curves by electrochemical impedance spectroscopy. A SrBi{sub 2}Ta{sub 2}O{sub 9} single-phase sample, treated at 2.5 GPa and 900 °C, was used to evaluate the electrical properties, obtaining a dielectric response similar to SrBi{sub 2}Ta{sub 2}O{sub 9} samples sintered by conventional processes at temperatures above 1000 °C. In addition, by this method, it was possible to obtain ceramics with uniform microstructure and a relative density of 93%. - Highlights: • The first production of SrBi{sub 2}Ta{sub 2}O{sub 9} using the technique of high-pressure processing. • The ability to produce single-phase SrBi{sub 2}Ta{sub 2}O{sub 9} treated at 2.5 GPa and 900 °C. • The electrical properties are compatible with SBT sintered at high temperatures.

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

Dense and half-dense NiZnCo ferrite ceramics: Their respective relevance for antenna downsizing, according to their dielectric and magnetic properties at microwave frequencies

Spinel ferrite Ni{sub 0.5}Zn{sub 0.3}Co{sub 0.2}Fe{sub 1.98}O{sub 4−x} nanoparticles were synthesized by co-precipitation method, and samples were realized by moulding and annealing at key temperatures (T{sub M} = 800 °C, 900 °C, 1050 °C, determined beforehand through shrinkage measurements) going with calcining and sintering processes. Annealing at 800 °C and 900 °C led to half-dense ceramics (porosity ∼50 vol. %), whereas bulky ferrite was obtained after annealing at 1050 °C. Elemental analysis, X-ray diffraction and ion chromatography analysis were performed. Complex dielectric permittivity (ε*) and magnetic permeability (μ*) were investigated up to 6 GHz. With increasing T{sub M}, a decreasing amount of Fe{sup 2+} was observed, going with increasing sample density. Coupled effects of the Fe{sup 2+} concentration and of the porosity, both on dielectric and magnetic properties, were chiefly investigated and discussed. The materials show almost constant permittivities (ε′ = 5.0, 6.0, and 14.8 for T{sub M} = 800 °C, 900 °C and 1050 °C, respectively). The bulk value at f = 1 GHz (ε′ = 14.8) can be interpreted well according to Shannon's theory. The permittivities of the half-dense ceramics are discussed on the basis of Bruggeman's Effective Medium Theory. The materials annealed at 800 °C and 900 °C show almost constant magnetic permeabilities in the frequency range from 0.2 to 1 GHz (μ′ = 3.4 and 6.0 for T{sub M} = 800 °C and 900 °C). The observed permeability behavior is typical of monodomain particles, except for the sample annealed at 1050 °C, for which domain wall contribution to μ* is suspected because of non-negligible losses at low frequency (μ″ = 1.3–1.8 at f < 0.3 GHz). This finding is supported by estimations of the upper and lower values for the critical grain size, on the basis of Brown–Van der Zaag's theory. Facing bulk ceramics, and in view of using Ni{sub 0.5}Zn{sub 0.3}Co{sub 0.2}Fe{sub 1.98}O{sub 4−x} ferrite as substrate for antenna miniaturization, the electromagnetic properties of half-dense ceramics materials seem to be very competitive at frequencies beyond 0.2 GHz, and up to 0.7–0.8 GHz.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2015

Zircaloy Cladding as Starting Precursor for Ceramic Waste-Forms - 15562

Zircaloy cladding of spent fuel is regular waste-stream related to the process of reprocessing. It remains in the apparatus after spent fuel dissolution. The most common technique of zircaloy cladding treatment is cementation and disposal in metallic containers. In view of the high cost of the cladding material (mainly zirconium), there have been a number of proposals for this material to be recovered and re-used. However, the residual contamination of the claddings following the dissolution of the fuel and the chemical stability of the zirconium militate against any proposal for a recycling process that might be economically reasonable. At the same time there is a lot of information available about synthesis of mineral-like materials based on zirconium for immobilization of long-lived radionuclides. The object of this work was to study experimentally electrochemical dissolution of fuel rod cladding for further obtaining starting precursor for the synthesis of ceramic-waste forms. The results of experiments on electrochemical dissolution of zirconium and zirconium alloy (fuel rod cladding) in nitric acid solutions are presented. The peak dissolution rate of specimens is shown to be observed in dilute nitric acid at elevated temperatures. The rate of dissolution rises with temperature, reaching ∼40-70 mg/cm{sup 2}.h at 90 deg. C. The current yield at this point is 0.6-0.7 g/A.h. The results of analysis of the surface oxide film on specimens and residues formed during dissolution are also presented. An electrochemical dissolution of zircaloy claddings is the common technique for preparation of zirconium solutions to be used for ceramic waste form synthesis. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2020

Extended Finite Element Based Approach in Additive Manufacturing Modeling for Optimizing Highly Complex Manifold in Protonic Ceramic Electrochemical Cells

The objective of this project is to develop a novel numerical approach based on the extended finite element method (XFEM) for modeling moving boundaries of material deposited in additive manufacturing (AM) process with improved accuracy and reduced computational cost. One of the major challenges in simulating AM processes is that the boundaries of the computational domain need to change as material is deposited. Previous approaches have achieved this by activating new finite elements, but this requires a high level of mesh refinement to capture small movement of the boundary. XFEM allows the solution boundary to move independently of the mesh, permitting smooth representation of the evolution of the boundary as material is deposited. As a result, this new method will significantly improve the simulation accuracy while reducing the computational cost compared with existing approaches. Furthermore, this project will bring significant improvements for the design and AM process optimization in an iterative fashion among numerical simuation, parameter optimization, and experimental validation. Specifically, this project will support the protonic ceramic electrochemical cells (PCEC) stack development at INL by providing insights into the density, residual stress, thermal and mechanical properties of the PCEC manifold and interconnect, which is critical in enhancing the system lifetime and reducing the overall cost. Upon the success of proposed development and validation of the proposed approach, simulation will be applied to determine an optimal set of AM process parameters for the PCEC manifold production. This project will consolidate Idaho National Laboratory (INL)’s simulation capabilities provided by the MOOSE framework and the Valhalla AM simulation application, with encouraging expansion to emerging PCEC applications and AM technologies at INL and beyond.

97 MATHEMATICS AND COMPUTING↗
DOE OSTI2018

Lithium-ion conductive ceramic textile: A new architecture for flexible solid-state lithium metal batteries

Designing solid-state lithium metal batteries requires fast lithium-ion conductors, good electrochemical stability, and scalable processing approaches to device integration. In this work, we demonstrate a unique design for a flexible lithium-ion conducting ceramic textile with the above features for use in solid-state batteries. The ceramic textile was based on the garnet-type conductor Li 7 La 3 Zr 2 O 12 and exhibited a range of desirable chemical and structural properties, including: lithium-ion conducting cubic structure, low density, multi-scale porosity, high surface area/volume ratio, and good flexibility. The solid garnet textile enabled reinforcement of a solid polymer electrolyte to achieve high lithium-ion conductivity and stable long-term Li cycling over 500 h without failure. The textile also provided an electrolyte framework when designing a 3D electrode to realize ultrahigh cathode loading (10.8 g/cm 2 sulfur) for high-performance Li-metal batteries.

25 ENERGY STORAGE↗
DOE OSTI2021

Coupling of Spark Plasma Sintering with Advanced Modeling to Enable Process Scale-Up: LDRD Final Project Poster

Electric-field assisted sintering (EFAS) manufacturing techniques reduce energy usage requirements, fabricate near-net-shape parts, and produce bulk nanostructured materials through rapid heating and cooling rates achievable through Joule heating. Process parameters of pulsed DC voltage and constant pressure are applied through stainless steel rams and graphite tooling to the ceramic yttrium oxide powder to be sintered. Our high-fidelity modeling code application advances manufacturing for extreme environments by enabling process-informed design and improving microstructure consistency through multiphysics multiscale process-structure-property-performance correlation simulations.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Refractory Issues Related to the Use of Hydrogen as An Alternative Fuel

With the increased interest and funding to investigate hydrogen as an alternative fuel to reduce carbon dioxide emissions, considerations may also be necessary to evaluate the effects of fuel substitutions on industrial processes and process vessels. One area that has not received significant attention is the effects on refractory ceramic lining systems when industrial furnaces are fired on hydrogen in place of or in addition to traditional fuels. Examples of changes in burner design and implementation when firing hydrogen can be found in the literature, but much less is documented regarding the effects on processes and process vessels. As such, this article attempts to present some of the issues encountered when substituting hydrogen as an alternative industrial fuel source and to highlight some examples of where this is occurring. Additionally, the possible ramifications of these issues on refractory ceramic lining systems are discussed.

08 HYDROGEN↗
DOE OSTI2015

Effect of synthesis methods on the Ca{sub 3}Co{sub 4}O{sub 9} thermoelectric ceramic performances

Three different synthesis methods producing nanometric grain sizes, coprecipitation with ammonium carbonate, oxalic acid, and by attrition milling have been studied to produce Ca{sub 3}Co{sub 4}O{sub 9} ceramics and compared with the classical solid state route. These three processes have produced high reactive precursors and all the organic material and CaCO{sub 3}·have been decomposed in a single thermal treatment. Coprecipitation leads to pure Ca{sub 3}Co{sub 4}O{sub 9} phase, while attrition milling and classical solid state produce small amounts of Ca{sub 3}Co{sub 2}O{sub 6} secondary phase. Power factor values are similar for all three samples, being slightly lower for the ones produced by attrition milling. These values are much higher than the obtained in samples prepared by the classical solid state method, used as reference. The maximum power factor values determined at 800 °C (∼0.43 mW/K{sup 2} m) are slightly higher than the best reported values obtained in textured ones which also show much higher density values. - Graphical abstract: Impressive raise of PF in Ca{sub 3}Co{sub 4}O{sub 9} thermoelectric materials obtained from nanometric grains. - Highlights: • Ca{sub 3}Co{sub 4}O{sub 9} has been produced by four different methods. • Precursors particle sizes influences on the final performances. • Coprecipitation methods produce single Ca{sub 3}Co{sub 4}O{sub 9} phase. • Power factor reaches values comparable to high density textured materials.

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

Selective recovery of silver from waste low-temperature co-fired ceramic and valorization through silver nanoparticle synthesis

Highlights: • Silver rich LTCC an e-waste has been recycled and valorized. • Selectively, Ag was leached and recovered as nanopowder. • The process can circulate the Ag within the industry in a close loop. • Brings back the material to production stream and address the circular economy. • Can be part of cradle-to-cradle technology and lower the futuristic carbon economy. - Abstract: Considering the value of silver metal and silver nanoparticles, the waste generated during manufacturing of low temperature co-fired ceramic (LTCC) were recycled through the simple yet cost effective process by chemical-metallurgy. Followed by leaching optimization, silver was selectively recovered through precipitation. The precipitated silver chloride was valorized though silver nanoparticle synthesis by a simple one-pot greener synthesis route. Through leaching-precipitation optimization, quantitative selective recovery of silver chloride was achieved, followed by homogeneous pure silver nanoparticle about 100 nm size were synthesized. The reported recycling process is a simple process, versatile, easy to implement, requires minimum facilities and no specialty chemicals, through which semiconductor manufacturing industry can treat the waste generated during manufacturing of LTCC and reutilize the valorized silver nanoparticles in manufacturing in a close loop process. Our reported process can address issues like; (i) waste disposal, as well as value-added silver recovery, (ii) brings back the material to production stream and address the circular economy, and (iii) can be part of lower the futuristic carbon economy and cradle-to-cradle technology management, simultaneously.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2024

Utilization of Novel (KNbO 3 ) 1− x (Ba 2 FeNbO 6 ) x ( x = 0.1, 0.2, 0.3) Solid Solutions for Efficient Photo‐Assisted Fenton Degradation of Methylene Blue Dye

Novel (KNbO 3 ) 1− x (Ba 2 FeNbO 6 ) x ( x = 0.1, 0.2, 0.3) solid solutions corresponding to K 0.82 Ba 0.18 Fe 0.09 Nb 0.91 O 3 , K 0.64 Ba 0.36 Fe 0.18 Nb 0.82 O 3 , and K 0.46 Ba 0.54 Fe 0.27 Nb 0.73 O 3 compounds have been synthesized via molten salt method. X‐ray diffraction confirms the formation of solid solutions, while transmission electron microscopy combined with energy‐dispersive spectroscopy results demonstrates a homogeneous distribution of elements. The obtained solid solutions crystallized in a cubic crystal structure, whereas the parent KNbO 3 possesses an orthorhombic structure. The wide bandgap semiconductor KNbO 3 transformed into a visible‐light‐active material, with its bandgap energy reduced from 3.56 eV to ≈2.4 eV. The substitution of K in KNbO 3 with Ba is responsible for structural modification from orthorhombic to cubic symmetry, whereas both structural modification and the substitution of Nb with Fe correlated with optical properties. The photocatalytic activities of all obtained solid solutions are improved compared with the parent KNbO 3 and Ba 2 FeNbO 6 compounds for photocatalytic degradation of methylene blue (MB) dye. Among the series of solid solutions, K 0.82 Ba 0.18 Fe 0.09 Nb 0.91 O 3 photocatalysts show the highest MB removal efficiency owing to its relatively higher surface area, suppressed charge carrier recombination, and more negative conduction band edge. Moreover, K 0.82 Ba 0.18 Fe 0.09 Nb 0.91 O 3 photocatalyst (0.1 g) combined with hydrogen peroxide (H 2 O 2 ) to form a novel photo‐Fenton system, achieving almost complete degradation of 100 mL of 10 mg L −1 MB dye in 30 min.

Avcıoğlu, Celal [Technische Universität Berlin, Fa↗
DOE OSTI2017

Structure-processing correlations and mechanical properties in freeze-cast Ti-6Al-4V with highly aligned porosity and a lightweight Ti-6Al-4V-PMMA composite with excellent energy absorption capability

In contrast to freeze-cast ceramics and polymers, few freeze-cast metals have been described, to date. This systematic study on structure-processing correlations in freeze-cast Ti-6Al-4V scaffolds reports how processing parameters determine the architecture formed during the directional solidification of water-based metal slurries and after sintering. Additionally, sedimentation in the slurry during freezing and volume shrinkage during burnout and sintering were found to significantly affect both structure and properties of the scaffolds. In using two freezing rates, 1 and 10 °C min -1 , two water-based polymer solutions as binders (chitosan and carboxymethyl cellulose) and two different metal volume fractions in the slurry, 20 and 30 vol%, Ti-6Al-4V scaffolds could be prepared with pore length, width, and porosity ranging from 41 to 523 μm, 14.5–76.5 μm, and 65 to 34%, respectively. Their compressive strength, stiffness, and toughness (work to 20% strain) fall in the range of 83–412 MPa, 7–29 GPa, and 14–122 MJ m -3 , respectively. In order to improve the properties a select composition was infiltrated with poly(methyl methacrylate). This increased the average yield strength by a factor of 2.3 from 83 to 193 MPa and the average toughness (work to 50% strain) by a factor of 2.7 from 28.1 to 76.8 MJ m -3 .

36 MATERIALS SCIENCE↗
DOE OSTI2025

Dynamic Atomistic Polar Structure Underpins Ultrahigh Linear Electro-Optic Coefficient in Transparent Ferroelectric Ceramics

Transparent ferroelectrics with high linear electro-optic (EO) coefficients are critical for advanced electro-optical devices. However, achieving optical transparency in ferroelectric ceramics remains challenging due to visible light scattering caused by defects such as domain walls, grain boundaries, and pores. Here, we report the successful fabrication of transparent ferroelectric ceramics through innovative chemical composition design and an advanced two-step sintering process in the La-doped Pb(Mg 1/3 Nb 2/3 )O 3 –PbTiO 3 system. The optical transparency, which is near the theoretical upper limit, can be attributed to the wide band gap and the minimization of light scattering of defects. By minimizing porosity and engineering grain/domain sizes to differ significantly from the wavelengths of visible light, we suppress scattering, achieving optical transparency near the theoretical upper limit. Strikingly, these ceramics exhibit an ultrahigh linear EO coefficient of ∼1417 pm/V, over 65 times greater than that of LiNbO 3 single crystals, the current industry standard. We attribute this exceptional performance to dynamic atomistic polar structures within switchable, thermally stable domains, which enhance electronic polarization sensitivity. This mechanism is corroborated by dielectric spectroscopy, high-resolution transmission electron microscopy and simulation. Our findings offer insights into the design of cost-effective transparent materials with exceptional EO properties, paving the way for next-generation electro-optical devices.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Atomistic modeling of metal–nonmetal interphase boundary diffusion

Atomistic computer simulations are applied to investigate the atomic structure, thermal stability, and diffusion processes in Al–Si interphase boundaries as a prototype of metal–ceramic interfaces in composite materials. Some of the most stable orientation relationships between the phases found in this work were previously observed in epitaxy experiments. Here, a non-equilibrium interface can transform to a more stable state by a mechanism that we call interface-induced recrystallization. Diffusion of both Al and Si atoms in stable Al–Si interfaces is surprisingly slow compared with diffusion of both elements in Al grain boundaries but can be accelerated in the presence of interface disconnections. A qualitative explanation of the sluggish interphase boundary diffusion is proposed. Atomic mechanisms of interphase boundary diffusion are similar to those in metallic grain boundaries and are dominated by correlated atomic rearrangements in the form of strings and rings of collectively moving atoms.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Estimation of abatement potentials and costs of air pollution emissions in China

Understanding the air pollution emission abatement potential and associated control cost is a prerequisite to design cost ef?cient control policies. In this study, a linear programming algorithm model, International Control Cost Estimate Tool, was updated with cost data for applications of 56 types of end-of-pipe technologies and ?ve types of renewable energy in 10 major sectors namely power generation, industry combustion, cement pro-duction, iron and steel production, other industry processes, domestic combustion, transportation, solvent use, livestock rearing, and fertilizer use. The updated model was implemented to estimate the abatement potential and marginal cost of multiple pollutants in China. The total maximum abatement potentials of sulfur dioxide (SO2), nitrogen oxides (NOx), primary particulate matter (PM2.5), non-volatile organic compounds (NMVOCs), and ammonia (NH3) in China were estimated to be 19.2, 20.8, 9.1, 17.2 and 8.6 Mt, respectively, which accounted for 89.7%, 89.9%, 94.6%, 74.0%, and 80.2% of their total emissions in 2014, respectively. The associated control cost of such reductions was estimated as 92.5, 469.7, 75.7, 449.0, and 361.8 billion CNY in SO2, NOx, primary PM2.5, NMVOCs and NH3, respectively. Shandong, Jiangsu, Henan, Zhejiang, and Guangdong provinces exhibited large abatement potentials for all pollutants. Provincial disparity analysis shows that high GDP regions tend to have higher reduction potential and total abatement costs. End-of-pipe technologies tended be a cost-ef?cient way to control pollution in industries processes (i.e., cement plants, iron and steel plants, lime production, building ceramic production, glass and brick production), whereas such technologies were less cost- effective in fossil fuel-related sectors (i.e., power plants, industry combustion, domestic combustion, and transportation) compared with renewable energy. The abatement potentials and marginal abatement cost curves developed in this study can further be used as a crucial component in an integrated model to design optimized cost-ef?cient control policies.

Zhang, Fenfen↗
DOE OSTI2015

The formation and structure of mechano-synthesized nanocrystalline Sr{sub 3}Fe{sub 2}O{sub 6.4}: XRD Rietveld, Mössabuer and XPS analyses

Highlights: • The formation of mechano-synthesized nanocrystalline Sr{sub 3}Fe{sub 2}O{sub 7−δ} is investigated. • Pre-milling the reactants substantially lowers the formation temperature. • The core and surface structures were studied. • XRD and {sup 57}Fe Mössbauer spectroscopic analyses indicate the δ-value to be 0.60. • XPS shows a complex surface structure for the mechanosynthesized Sr{sub 3}Fe{sub 2}O{sub 7−δ} nanoparticles. - Abstract: The influence of ball milling and subsequent sintering of a 3:1 molar mixture of SrCO{sub 3} and α-Fe{sub 2}O{sub 3} on the formation of Sr{sub 3}Fe{sub 2}O{sub 7−δ} double perovskite is investigated with different analytical techniques. Milling the mixture for 110 h leads to the formation of SrCO{sub 3}-α-Fe{sub 2}O{sub 3} nanocomposites and the structural deformation of α-Fe{sub 2}O{sub 3} via the incorporation of Sr{sup 2+} ions. Subsequent sintering of the pre-milled reactants’ mixture has led to the partial formation of an SrFeO{sub 3} perovskite-related phase in the temperature range 400–600 °C. This was followed by the progressive development of an Sr{sub 3}Fe{sub 2}O{sub 7−δ} phase that continued to increase with increasing sintering temperature until a single-phased nanocrystalline Sr{sub 3}Fe{sub 2}O{sub 7−δ} phase was attained at 950 °C (12 h). This temperature is ∼350 °C lower than the temperature at which the material is prepared conventionally using the ceramic method. The evolution of different structural phases during the reaction process is discussed. Rietveld refinement of the X-ray diffraction data shows a value of 0.60 for the oxygen deficiency δ, in consistency with the Fe{sup 3+}/Fe{sup 4+} ratio derived from the {sup 57}Fe Mössbauer data recorded at both 300 K and 78 K. The Mössbauer data suggests that the Sr{sub 3}Fe{sub 2}O{sub 6.4} nanoparticles are superparamagnetic with blocking temperatures below 78 K. The surfaces of the Sr{sub 3}Fe{sub 2}O{sub 6.4} nanoparticles were shown to have a complex structure and composition relative to those of their cores with traces of SrCO{sub 3}, SrO and SrFeO{sub 3−δ} being detected.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗