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At least 1,423 records · Page 79
All sourcesNASA NTRSDOE OSTI
DOE OSTI2024

Dielectric and magnetic properties of microwave-absorbing FeAl x O y catalysts fabricated via solution combustion synthesis

Iron-based alumina (FeAl x O y ) nanocomposites are microwave-absorbers and catalysts, which makes them promising for emerging microwave-assisted thermocatalytic technologies. Solution combustion synthesis (SCS) has been used to synthesize FeAl x O y powders, and prior work has demonstrated that adjusting SCS parameters significantly changes phase composition and specific surface area of the products. However, it is unclear how synthesis parameters affect their microwave-absorbing properties, which are essential for optimizing microwave-assisted technologies. To address this challenge, in the present work, twelve different FeAl x O y products were synthesized at different combinations of the SCS parameters such as two fuels (citric acid and glycine), two heating modes (hotplate and muffle furnace), and three Fe:Al molar ratios (2:1, 1:1, 1:2). Dielectric and magnetic properties of the products were characterized using a network analyzer and a vibrating sample magnetometer. Based on the measured permittivity and permeability, penetration depth and reflection loss were calculated as a function of frequency and bed thickness. The products were heated by microwaves at 2.45 GHz and then examined with X-ray diffraction (XRD) analysis. For all products, the magnetic saturation was lower than for bulk iron oxides because of the small crystallite size and aluminum substitution. The use of glycine induced high dielectric losses and enabled fast microwave-heating rates compared to citric acid. Higher Fe:Al ratio also led to higher dielectric and magnetic losses. With glycine fuel, SCS in a furnace induced larger penetration depth and lower microwave absorption than SCS on a hotplate. The minimization of reflected power was more sensitive to the thickness of the product bed than to the frequency of the electromagnetic field. Post-heating XRD analysis revealed different phase transformations in the FeAl x O y powders depending on the SCS parameters. As a result, an FeAl x O y material, synthesized via incipient wetness impregnation, lacked magnetic losses and did not heat well as compared to the SCS products.

Combustion synthesis↗
DOE OSTI2021

A generalized distillation network synthesis model

In this report we propose a generalized superstructure-based distillation network synthesis model with improved modeling capabilities resulting in an extended solution space. The model can assign multiple mixtures to be separated (e.g., reactor network effluents) to different columns of the network while considering the interactions among different separation steps. In terms of outlets, products with general specifications, including pure components and multi-component mixtures, as well as streams without strict specifications (e.g., reactor recycle streams) can be readily handled. Furthermore, stream bypass is considered to avoid unnecessary separations, and thermal coupling is considered to yield novel solutions. The proposed model enables seamless integration with reactor network synthesis models thereby leading to solutions that are superior to the ones obtained by conventional sequential approaches.

42 ENGINEERING↗
DOE OSTI2018

A superstructure optimization approach for process synthesis under complex reaction networks

Here in this work, we present mixed integer linear programming methods for the synthesis of processes that involve complex reaction networks. Specifically, we consider the modeling of reactors and interconnecting streams in systems where the composition of the reactor inlet streams can vary substantially, thereby making the determination of the limiting component as well as the calculation of the stream heating/cooling and power requirements challenging. First, towards the modeling of reactors, we develop an extent-based method which detects the limiting reactant of each reaction occurring in parallel with others, based on the inlet flows of the reactants. Second, we develop a computationally tractable method for the calculation of the work and heating/cooling duty needed to condition any stream of a process based on simple calculations that can be performed offline. Finally, we present how the two aforementioned components can be integrated in an optimization model generated based on a process superstructure. We demonstrate the application of the developed methods for the synthesis of a biorefinery.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2019

Synthesis of operable process intensification systems: advances and challenges

Process intensification (PI) has been gaining increasing momentum in the chemical engineering research community and the chemical/energy industry. While many PI alternative technologies and their conventional counterparts exist, systematic approaches and tools to decide on the most promising intensified process solutions are currently rather lacking. Process Systems Engineering (PSE) can contribute uniquely to this challenge by leveraging process synthesis, design, analysis, and optimization tools. However, key open questions in this area still remain, including: (i) how to efficiently address the combinatorial design space and systematically deliver intensified designs, and (ii) how to ensure the operablility performances of the derived intensified structures at an early design stage. Here, this paper provides a brief review of recent progress towards the synthesis of operable process intensification systems, highlights major challenges, and discusses future research opportunities.

42 ENGINEERING↗
DOE OSTI2020

Thermodynamics and kinetics of solution combustion synthesis: Ni(NO 3 ) 2 + fuels systems

Solution combustion synthesis (SCS) utilizes exothermic self-propagating reactions to prepare nanoscale materials that can be used widely in energy, electronics, and biomedical technologies and other applications. SCS is a specific variety of a more general combustion synthesis (CS) method. Investigations of the thermodynamics, kinetics, and the mechanisms of SCS reactions, are not as well studied as the other CS processes. This work reports on a systematic study of the thermodynamics and kinetics of SCS reactions involving Ni(NO 3 ) 2 , an oxidizer, and either glycine (C 2 H 5 NO 2 ) or hexamethylenetetramine (HMT, C 6 H 12 N 4 ) as fuels. A thermodynamic modeling approach, based on the Gibbs free energy minimization principle, is applied to the simultaneous calculations of the adiabatic temperatures and compositions of the equilibrium products. Our calculations reveal the influence of fuel-to-oxidizer ratio, amount of water, and the oxygen in air on the combustion temperature under adiabatic conditions and the composition of the resulting products. We have, in turn, measured the combustion temperature and phase composition of products and compared them with the calculations. Variations of drying times for the solutions yield precursor gels with varying water contents. This approach enables the manipulation of combustion parameters and confirms the use of calculated activation energies for reactions using the Merzhanov-Khaikin method. Here, the results show that SCS reactions in fuel-lean solutions producing NiO have higher activation energy in contrast to reactions with fuel-rich solutions that form Ni. Reduction of activation energies due to the increase in the fuel-to-oxidizer ratio could be related to the observed change of the rate-limiting stages of the endothermic decomposition of the individual reactants to the exothermic decomposition of coordinate compounds formed between the reactants.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2013

Mechanistic Studies of Methanol Synthesis over Cu from CO/CO2/H2/H2O Mixtures: the Source of C in Methanol and the Role of Water

The low temperature (403 – 453K) conversions of CO:hydrogen and CO2:hydrogen mixtures (6 bar total pressure) to methanol over copper catalysts are both assisted by the presence of small amounts of water (mole fraction ~0.04%-0.5%). For CO2:hydrogen reaction mixtures, the water product from both methanol synthesis and reverse water gas shift serves to initiate both reactions in an autocatalytic manner. In the case of CO:D2 mixtures, very little methanol is produced until small amounts of water are added. The effect of water on methanol production is more immediate than in CO2:D2, yet the steady state rates are similar. Tracer experiments in 13CO:12CO2:hydrogen (with or without added water), show that the dominant source of C in the methanol product gradually shifts from CO2 to CO as the temperature is lowered. Cu-bound formate, the major IR visible surface species under CO2:hydrogen, is not visible in CO:moist hydrogen. Though formate is visible in the tracer experiments, the symmetric stretch is absent. These results, in conjunction with recent DFT calculations on Cu(111), point to carboxyl as a common intermediate for both methanol synthesis and reverse water gas shift, with formate playing a spectator co-adsorbate role.

copper catalysts↗
DOE OSTI2025

Synthesis of multicomponent oxygen evolution reaction coatings via block copolymer templating with vapor- and solution-phase precursors

Porous mixed transition metal oxide heterostructures are promising electrocatalysts due to their high surface area. However, achieving conformal multicomponent oxide coatings with controlled nanoscale architectures remains challenging. Here, we report a synthesis strategy that integrates solution-based swelling infiltration (SBI) with gas-phase sequential infiltration synthesis (SIS) in a block copolymer template to fabricate porous, high-surface-area, conformal mixed-oxide electrocatalytic coatings. In this approach, a PS75-P4VP25 block copolymer (BCP) film is first infiltrated with transition metal acetylacetonate precursors via SBI, followed by exposure to gas phase precursors of ZnO via SIS process. Thermal annealing of the infiltrated BCP films converts them into all-inorganic Fe–ZnO, Fe–Co–ZnO, and Fe–Ni–ZnO coatings. Electrochemical testing on 70 nm thick conformal coatings demonstrates promising oxygen evolution reaction (OER) activity in alkaline media, with mass-specific current densities up to 1.0 × 10 5 mA/g at an overpotential of 330 mV (vs. RHE) at ultralow loading (~0.005 g/cm 2 ). Among the compositions, Fe–Co–ZnO and amorphous Fe–Ni–ZnO show the best OER performance, delivering current densities of 2.00 and 3.04 mA/cm 2 , respectively, compared to 1.52 mA/cm 2 for Fe–ZnO.. This work establishes SBI–SIS as a versatile route for fabricating nm-thin, high-performance multicomponent oxide heterostructures on cost-efficient supports, enabling efficient catalyst utilization in electrochemical energy conversion application.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2019

Synthesis and optimized formulation for high-capacity manganese fluoride (MnF 2 ) electrodes for lithium-ion batteries

Electrochemical activity of poorly conductive metal fluorides in Li-ion batteries is contingent on their nanostructuration to reduce diffusion lengths and increase reaction kinetics. In that regard, we optimize the synthesis and electrode formulation of MnF 2 to enable sufficient electrochemical activity required to study its electrochemical conversion reaction mechanism. Solvothermal synthesis in a water–ethanol mixture (1:1 Vol.), using Mn acetate and a slight excess of hydrofluoric acid (HF), results in pure phase, nanosized (˜30 nm diameter) rutile-type MnF 2 ( P 4 2 /mnm). High energy ball-milling of MnF2–carbon mixtures leads to an amorphization of MnF 2 and its partial phase transformation to the α-PbO 2 -type structure, without significant improvement of the electrochemical performance. Changing the electrode binder, however, from typical polyvinylidene fluoride (PVDF) to water-soluble Na-alginate, leads to a significant improvement of the reversibility of the electrochemical reaction. Here, we attribute this drastic improvement to the improved adherence and homogeneity of the electrode film prepared with Na-alginate.

25 ENERGY STORAGE↗
DOE OSTI2017

Room temperature synthesis of β-NaGdF 4 : RE 3+ (RE= Eu, Er) nanocrystallites and their luminescence

In this study, a room temperature synthesis was developed for phase pure β-NaGdF 4 nanocrystallites as well as 5, 10, and 20% Eu 3+ or 5% Er 3+ doped material. Rare earth acetates and NaCl react in a 1:2 M ratio with a variable excess of NH 4 F in ethylene glycol within 24 hours. Since the thermodynamic stability of the hexagonal phase decreases along the lanthanide series, a larger excess of NH 4 F was required for the synthesis of luminescent samples doped with the smaller Er 3+ ions than for Eu 3+ doped or pure β-NaGdF 4 . The materials were characterized by powder X-ray diffraction, electron microscopy, and luminescence spectroscopy. The Eu 3+ -doped samples show 5 D 0 → 7 F J and 5 D 1 → 7 F J luminescence after Eu 3+ excitation at 394 nm or Gd 3+ excitation at 273 nm and 308 nm. The ratio of 5 D 1 vs. 5 D 0 luminescence is influenced by the excitation wavelength and the Eu 3+ concentration. Lastly, the Er 3+ -doped samples show green and red upconversion luminescence, respectively, from the 2 H 11/2 + 4 S 3/2 → 4 I 15/2 and 4 F 9/2 → 4 I 15/2 transitions after 970 nm excitation.

36 MATERIALS SCIENCE↗
DOE OSTI2023

The influence of hydrothermal synthesis temperature on the electronic structure and luminescence property of Cr-doped ZnGa 2 O 4 nanoparticles

Cr-doped ZnGa 2 O 4 (CZGO) is a near-infrared-emitting material with long-lasting persistent luminescence. This unique property makes it a great candidate in optical imaging and sensing for various biomedical applications. Nanosized CZGO can be synthesized via a hydrothermal approach, but the reaction temperatures reported in existing literature vary from 120°C to 220°C, approaching the highest temperature allowed for a standard autoclave vessel. The reason for choosing a particular hydrothermal synthesis temperature has rarely been discussed, and it is unclear whether the resulting CZGO possess the same optical properties. This work compares CZGO nanoparticles synthesized at temperatures from the lowest reported 120°C and to as high as 220°C. We find that although all the synthesized CZGO are light emitting, they exhibit different luminescence intensities and respond differently to the change of excitation energy. X-ray absorption fine structure (XAFS) analysis is employed to investigate the local chemical environment around Zn, Ga and Cr, respectively. We found synthesis temperature strongly influences the Ga species formed in these particles. The energy transfer mechanism is further elucidated using X-ray excited optical luminescence (XEOL) in combination with element-specific XAFS. Two energy transfer paths are identified, which explains the different excitation energy dependencies of the observed photoluminescence.

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

Synthesis and characterization of Gd-doped magnetite nanoparticles

There has been rising interest in the synthesis of magnetite nanoparticles due to their importance in biomedical and technological applications. Tunable magnetic properties of magnetite nanoparticles to meet specific requirements will greatly expand the spectrum of applications. Tremendous efforts have been devoted to studying and controlling the size, shape and magnetic properties of magnetite nanoparticles. We investigate gadolinium (Gd) doping to influence the growth process as well as magnetic properties of magnetite nanocrystals via a simple co-precipitation method under mild conditions in aqueous media. Gd doping was found to affect the growth process leading to synthesis of controllable particle sizes under the conditions tested (0–10 at% Gd 3+ ). Typically, undoped and 5 at% Gd-doped magnetite nanoparticles were found to have crystal sizes of about 18 and 44 nm, respectively, supported by X-ray diffraction and transmission electron microscopy. These results showed that Gd-doped nanoparticles retained the magnetite crystal structure, with Gd 3+ randomly incorporated in the crystal lattice, probably in the octahedral sites. The composition of 5 at% Gd-doped magnetite was Fe (3-x) Gd x O 4 (x=0.085±0.002), as determined by inductively coupled plasma mass spectrometry. 5 at% Gd-doped nanoparticles exhibited ferrimagnetic properties with small coercivity (~65 Oe) and slightly decreased magnetization at 260 K in contrast to the undoped, superparamagnetic magnetite nanoparticles. Templation by the bacterial biomineralization protein Mms6 did not appear to affect the growth of the Gd-doped magnetite particles synthesized by this method.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Hydrothermal synthesis of Co-free NMA cathodes for high performance Li-ion batteries

Scalable and sustainable production of high voltage cathodes is required to meet the increasing demands for Li-ion batteries. Additionally, the anticipated scarcity of critical materials like cobalt necessitates demonstration of Co-free alternatives that can match the performance metrics of conventional cathodes. Herein, a hydrothermal synthesis route for production of a new class of high-capacity, cobalt-free cathode material, LiNi 0.9 Mn 0.05 Al 0.05 O 2 (NMA9055) for next-generation Li-ion batteries is reported. In this work, the synthesized cathode material shows high crystallinity and purity with monodispersed spherical morphology. Extensive electrochemical, structural, and post-mortem characterization of this novel NMA material is carried out. NMA-Li half cells show an initial discharge capacity of 200 mAh/g with a 96% capacity retention over 100 cycles when cycled between 3.0 and 4.4 V. On the other hand, NMA full cells with Li 4 Ti 5 O 12 (LTO) electrodes as the anode, show an initial discharge capacity of 186 mAh/g with 81% capacity retention over 200 cycles. Post-mortem structural and morphological characterization show that the NMA morphology and crystal structure do not degrade significantly over 200 charge/discharge cycles. This new class of cobalt free cathode material containing nickel, manganese and aluminum synthesized by an ammonia-free synthesis route is expected to provide a facile solution towards sustainable cathode production.

25 ENERGY STORAGE↗
DOE OSTI2012

Hydrothermal synthesis map of bismuth titanates

The hydrothermal synthesis of four bismuth titanate materials from common bismuth and titanium precursors under hydrothermal conditions is described. Reaction of NaBiO{sub 3}{center_dot}2H{sub 2}O and anatase TiO{sub 2} in concentrated NaOH solution at 240 Degree-Sign C is shown to produce perovskite and sillenite phases Na{sub 0.5}Bi{sub 0.5}TiO{sub 3} and Bi{sub 12}TiO{sub 20}, depending on the ratio of metal precursors used. When KOH solution is used and a 1:1 ratio of the same precursors, a pyrochlore Bi{sub 1.43}Ti{sub 2}O{sub 6}(OH){sub 0.29}(H{sub 2}O){sub 0.66} is formed. The use of a mixture of HNO{sub 3} and NaOH is shown to facilitate the formation of the Aurivillius-type bismuth titanate Bi{sub 4}Ti{sub 3}O{sub 12}. The phases have been isolated separately as phase-pure powders and profile refinement of powder X-ray diffraction data allows comparisons with comparable materials reported in the literature. Analysis of Bi L{sub III}-edge X-ray absorption near edge structure (XANES) spectra of the materials shows the oxidation state of bismuth is +3 in all of the hydrothermally derived products. - Graphical abstract: Use of NaBiO{sub 3}{center_dot}2H{sub 2}O and TiO{sub 2} as reagents under hydrothermal conditions allows the phase-pure preparation of four crystalline bismuth titanate materials. Highlights: Black-Right-Pointing-Pointer NaBiO{sub 3} and TiO{sub 2} under hydrothermal conditions allow formation of bismuth titanates. Black-Right-Pointing-Pointer Synthesis of four distint phases has been mapped. Black-Right-Pointing-Pointer Bi LIII-edge XANES shows Bi is reduced to oxidation state +3 in all materials. Black-Right-Pointing-Pointer A new hydrated bismuth titanate pyrochlore has been isolated.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2012

Controlled synthesis, formation mechanism and upconversion luminescence of NaYF{sub 4}: Yb, Er nano-/submicrocrystals via ionothermal approach

In order to deepen the fundamental understanding of IL-mediated synthesis of nano-/submicrostructure, hydrophilic ILs ([Emim][BF{sub 4}], [Bmim][BF{sub 4}] and [Omim][BF{sub 4}]), which act as solvents, templates, as well as fluorine source, have been employed to synthesize rare earth doped NaYF{sub 4} upconversion nano-/submicrocrystals (UC-NMCs). The imidazolium cations provide the capping reagent to prevent the nucleation centers from aggregation and growing, while the tetrafluoroborate anions introduce a new fluorine source according to partial hydrolysis. It is demonstrated that the properties of IL, such as viscosity, polarity, solvency and interfacial tension, extremely affect the dissolution, diffusion and nucleation process of lanthanide ions in IL. Morphology and size of the final products can thus be tailored by synthetical parameters, like imidazolium cations, cosolvents, Ln{sup 3+} and fluoride concentrations, as well as ionothermal time. Based on the experimental results, the possible mechanism of the nucleation and growth of UC-NMCs in IL is discussed. - Graphical abstract: The upconversion nano-/submicrocrystals with diverse morphologies and sizes have been synthesized through ionothermal approach. The possible mechanism is concluded, which strengthens the fundamental understanding of IL-mediated synthesis of nano-/submicrostructure. Highlights: Black-Right-Pointing-Pointer The upconversion nano-/submicrocrystals were synthesized through ionothermal approach. Black-Right-Pointing-Pointer The as-prepared products exhibited diverse morphologies and sizes. Black-Right-Pointing-Pointer The possible mechanism of the nucleation and growth process in ILs is concluded.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2012

Hydrothermal synthesis of new rare earth silicate fluorides: A novel class of polar materials

Polar crystals provide an interesting avenue for materials research both in the structures they form and the properties they possess. This work describes the hydrothermal synthesis and structural characterization of three novel silicate fluorides. Compound (1), LiY{sub 3}(SiO{sub 4}){sub 2}F{sub 2} crystallizes in space group C2/c, with a=17.651(4) A, b=4.8868(10) A, c=11.625(2) A and {beta}=131.13(3) Degree-Sign . BaY{sub 2}(Si{sub 2}O{sub 7})F{sub 2} (2) crystallizes in space group P-1, with a=5.1576(10) A, b=6.8389(14) A, c=11.786(2) A, {alpha}=93.02(3) Degree-Sign , {beta}=102.05(3) Degree-Sign and {gamma}=111.55(3) Degree-Sign . Finally, the structure of Ba{sub 2}Y{sub 3}(SiO{sub 4}){sub 2}F{sub 5} (3) was determined in the polar orthorhombic space group Pba2, having unit cell parameters a=8.8864(18) A, b=12.764(3) A and c=5.0843(10) A. The structures are compared based on their building blocks and long range polarities. Aligned silicate tetrahedra segregated into a single layer in (3) impart the observed polarity. - Graphical abstract: The polar structure of Ba{sub 2}Y{sub 3}(SiO{sub 4}){sub 2}F{sub 5}. Highlights: Black-Right-Pointing-Pointer Natural yttrium silicate fluoride minerals are briefly reviewed. Black-Right-Pointing-Pointer The synthesis and structures of LiY{sub 3}(SiO{sub 4}){sub 2}F{sub 2}, BaY{sub 2}(Si{sub 2}O{sub 7})F{sub 2} and Ba{sub 2}Y{sub 3}(SiO{sub 4}){sub 2}F{sub 5} are discussed. Black-Right-Pointing-Pointer Ba{sub 2}Y{sub 3}(SiO{sub 4}){sub 2}F{sub 5} crystallizes in the polar space group Pba2. Black-Right-Pointing-Pointer Polarity occurs primarily through aligned silicate tetrahedra in a segregated layer.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2012

Synthesis of YAG nanopowder by the co-precipitation method: Influence of pH and study of the reaction mechanisms

YAG nanopowders with an average grain size of 30 nm have been successfully synthesized by the co-precipitation method using nitrates with precipitant of ammonium hydrogen carbonate. The influence of precipitation conditions such as pH, aging time and calcination temperature on the formation of secondary phases has been studied. The accurate control of pH value at every stage of precipitation process is crucial to avoid the presence of YAM (Yttrium Aluminium Monoclinic, Y{sub 4}Al{sub 2}O{sub 9}) and yttrium oxide (Y{sub 2}O{sub 3}) after calcination. The reaction mechanisms have been investigated using different techniques such as infrared spectroscopy, x-ray diffraction and thermal analyses. The YAG phase is formed around 1050 Degree-Sign C passing through an intermediate phase called YAP (Yttrium Aluminium Perovskite, YAlO{sub 3}). Local chemical heterogeneities are responsible for the deviation of the Y:Al ratio and the formation of YAP during heat treatment. - Graphical abstract: Synthesis of YAG nanopowder by the co-precipitation method: Influence of pH and study of the reaction mechanisms, Marlot et al. Highlights: Black-Right-Pointing-Pointer Synthesis of pure YAG nanoparticles by the co-precipitation method. Black-Right-Pointing-Pointer Influence of pH value on the formation of secondary phases all along the process. Black-Right-Pointing-Pointer Study of the importance of pH using titration method. Black-Right-Pointing-Pointer Chemical evolution of the precursor during calcinations. Black-Right-Pointing-Pointer Proposition for reaction mechanisms.

36 MATERIALS SCIENCE↗
DOE OSTI2012

Monodisperse spindle-like FeWO{sub 4} nanoparticles: Controlled hydrothermal synthesis and enhanced optical properties

Monodisperse FeWO{sub 4} nanoparticles with specific spindle-like morphology have been synthesized in the presence of citric acid through hydrothermal process. In the synthesis route, citric acid played four roles such as the reducing agent, chelating regents, structure-directing agent and stabilizing agents. In addition, the morphology of FeWO{sub 4} was dramatically tuned by the pH value of the precursor medium. The optical properties of FeWO{sub 4} were investigated with UV-Vis spectra and photoluminescence spectroscopy. The photocatalytic experiments demonstrated that the decomposition efficiency of the monodisperse spindle-like FeWO{sub 4} nanoparticles is 74% after 30 min of UV irradiation, which displayed remarkable enhanced photodegradation activity compared with ordinary FeWO{sub 4} sample (57%) and normal TiO{sub 2} photocatalysts P-25 (56%). - Monodisperse spindle-like FeWO{sub 4} nanoparticles with enhanced photocatalytic activities. Highlights: Black-Right-Pointing-Pointer Monodisperse spindle-like FeWO{sub 4} were synthesized with hydrothermal method. Black-Right-Pointing-Pointer Citric acid plays key roles in the hydrothermal synthesis. Black-Right-Pointing-Pointer Their morphology can be tuned with pH value of the precursor medium. Black-Right-Pointing-Pointer They show enhanced photocatalytic activities with irradiation of UV light.

36 MATERIALS SCIENCE↗
DOE OSTI2013

Synthesis of Sr{sub 0.9}K{sub 0.1}FeO{sub 3-{delta}} electrocatalysts by mechanical activation

Potassium-substituted SrFeO{sub 3-{delta}} for possible application as oxygen evolution electrode in alkaline or molten salt media was prepared by mechanical activation and characterized by X-ray diffraction, dilatometric and thermogravimetric analysis, Moessbauer spectroscopy, and electrical conductivity measurements. Room temperature mechanical activation of a mixture of oxide precursors with subsequent thermal treatments at 700-900 Degree-Sign C results in the formation of Sr{sub 0.9}K{sub 0.1}FeO{sub 3-{delta}} with tetragonal perovskite-like structure. Such allows to decrease the synthesis temperature, if compared to the conventional solid-state route, and to prevent possible volatilization of potassium. The results of Moessbauer spectroscopy studies indicate that the oxygen nonstoichiometry in the samples annealed in air at 900-1100 Degree-Sign C with subsequent rapid cooling vary in the range {delta}=0.30-0.32. The electrical conductivity in air exhibits a metal-like behaviour at temperatures above 400 Degree-Sign C and semiconductor behaviour in the low-temperature range, reaching 13-30 S/cm under prospective operation conditions for alkaline electrolyzers ({<=}90 Degree-Sign C). - graphical abstract: XRD patterns of Sr{sub 0.9}K{sub 0.1}FeO{sub 3-{delta}} powders, as-prepared and after annealing at different temperatures. Log({sigma}{center_dot}T) vs. 1000/T plot of the electrical conductivity of Sr{sub 0.9}K{sub 0.1}FeO{sub 3-{delta}}. The inset shows the thermal variation of {sigma}. Ceramics used were prepared by mechanical activation followed by a two-step sintering process at 900 Degree-Sign C for 1 h and 1000 Degree-Sign C for 5 h (82% densification). Highlights: Black-Right-Pointing-Pointer Sr{sub 0.9}K{sub 0.1}FeO{sub 3-{delta}} was successfully obtained by mechanical activation of oxide precursors. Black-Right-Pointing-Pointer Synthesis temperature is significantly lower when compared to a conventional solid-state route. Black-Right-Pointing-Pointer Oxygen nonstoichiometry of annealed samples at 900-1100 Degree-Sign C vary in the range {delta}=0.30-0.32. Black-Right-Pointing-Pointer Sr{sub 0.9}K{sub 0.1}FeO{sub 3-{delta}} shows metal and semiconductor behaviour above and below 400 Degree-Sign C, respectively.

36 MATERIALS SCIENCE↗