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Ionic liquid assisted microwave synthesis route towards color-tunable luminescence of lanthanide- doped BiPO 4
Ln 3+ -doped (Ln=Sm, Eu, Tb, Dy) nanoparticles of BiPO 4 with a particle size below 10 nm were synthesized in a straightforward manner from the appropriate mixture of the respective metal acetates and the task-specific ionic liquids choline or butylammonium dihydrogen-phosphate by conversion in a laboratory microwave (120 °C, 10 min). The ionic liquid acts not only as a solvent and microwave susceptor, but also as the reaction partner and nanoparticle stabilizer. The materials were thoroughly characterized not only with respect to their optical properties but also by PXRD, FT-IR, TEM techniques. Furthermore, depending on the lanthanide, the nanomaterial shows intense luminescence of different colors such as: orange (Sm 3+ ), red (Eu 3+ ), green (Tb 3+ ) or even white (Dy 3+ ).
Two convenient low-temperature routes to single crystals of plutonium dioxide
During the solvothermal synthesis of a low-dimensional borate, KB 5 O 7 (OH) 2 2H 2 O, in the presence of Pu(III), single crystals of plutonium dioxide unexpectedly formed. Single crystals of PuO 2 also formed during the hydrothermal synthesis of another borate, Na 2 B 5 O 8 (OH) 2 H2O, in the presence of Pu(III). The reactions were conducted at 170 °C and 150 °C, respectively, which are much lower temperature than previously reported preparations of crystalline PuO 2 . Yellow-green crystals with a tablet habit were characterized by single crystal X-ray diffraction and solid-state UV–vis–NIR absorption spectroscopy. The crystal structure was solved by direct methods with R 1 =1.26% for 19 unique observed reflections. PuO 2 is cubic, space group $Fm\bar{3}m$, and adopts the fluorite structure type. Finally, the lattice parameter was determined to be $a$=5.421(5)Å giving a volume of 159.3(2)Å3. The absorption spectrum is consistent with Pu(IV).
Understanding the structural and morphological effects of synthesis route on NpO 2
The availability of actinide standard materials for use in nuclear safeguard applications is critical, as is thorough characterization thereof. Although accurate trace element compositions and isotopic considerations are paramount for deployment of reference standards, structural characterization is also essential towards accurately describing the chemical form and potential matrix effects in candidate materials. Here, to this end, samples of NpO 2 were synthesized via a direct denitration (DD) method and probed with powder X-ray diffraction (PXRD), Raman spectroscopy, and scanning electron microscopy (SEM) for structural and morphological characterization and comparison with NpO 2 materials produced via modified direct denitration (MDD). PXRD confirmed the bulk identity of NpO 2 , and no additional phases were identified using this method. Analysis of Raman data collected using a 532 nm excitation wavelength indicates that samples are mostly phase pure; however, some variability in spectral features is observed. Analysis of additional spectroscopic data collected with a 785 nm excitation wavelength revealed variability in the relative intensity of spectral features. Raman spectroscopy indicates that the sample is primarily NpO 2 ; however, additional signals indicate possible structural disorder, oxidized species, or potential contributions from other Np phases. To further investigate the possibility of additional phase contributions within the sample of NpO 2 , Raman spectroscopic mapping was employed to examine the homogeneity of the sample produced via DD. From this analysis, we determined that despite variability in the intensity of Raman-active vibrational modes, consistent spectra are obtained throughout the area of the sample investigated. SEM images show aggregates with variable sizes and shapes, with rounded, primary particles possessing an average diameter of approximately 100 nm. Comparison of the results of these multimodal analyses to the literature indicates that the crystal chemical, spectroscopic, and microstructural properties of NpO 2 vary based on synthesis method, even if X-ray diffraction data indicate that the bulk phase is NpO 2 .
Underlying limitations behind impedance rise and capacity fade of single crystalline Ni-rich cathodes synthesized via a molten-salt route
Layered oxide LiNi x Mn y Co z O 2 (NMC) cathodes are often synthesized as polycrystalline secondary particles. Due to intergranular fracture stemming from volume changes of randomly oriented primary particles during charge/discharge, the synthesis of larger single-crystalline cathodes is of high interest. In this work, molten salt assisted growth of micron-sized Ni-rich crystals is achieved with excellent crystallinity, low cation mixing, and negligible impurities. However, electrochemical performance is compromised by high surface reactivity resulting in decomposition of electrolyte and subsequent formation of a thick CEI layer. While intergranular fracture is eliminated, planar gliding and severe intragranular fracture along the (003) plane occurs in the high voltage region within the first few cycles and is associated primarily with H2 to H3 structural transitions. In addition, H2 to H3 transitions are highly irreversible with cyclic voltammograms revealing polarization growth within <5 cycles. Subsequently, the single-crystalline material exhibited markedly reduced available capacity and enhanced capacity fade from sharp impedance growth compared to its polycrystalline counterpart. Here, this work furthers a fundamental understanding into the limitations of single-crystalline Ni-rich cathodes, and the obstacles limiting the advantages offered by the single-crystalline morphology.
NMR investigation of proton transport in polybenzimidazole/polyphosphoric acid membranes prepared via novel synthesis route
Here, in this work, we present a molecular-level view of the structural changes in polybenzimidazole (PBI) membranes doped with phosphoric acid (PA) generated by a novel membrane fabrication technique. The modified PA doped membranes displayed unprecedented ionic conductivity at elevated temperatures, comparable to the starting PBI gel membranes prepared by the commonly used PPA process, while also exhibiting enhanced mechanical properties. To elucidate the cause of these effects, we used multi-nuclear ( 1 H, 13 C, 31 P) 1D PFG, MAS and CPMAS, and 2D HETCOR magnetic resonance (NMR) techniques to characterize the structure and dynamics of the modified film and the original gel PBI membranes. 1 H diffusivity measurements show significantly enhanced proton diffusivity, both in magnitude and in lower activation energy, which were consistent with its high ionic conductivity despite the lower PA content compared to the original gel membrane. CPMAS experiments further substantiated that the location of these distinct phosphate environments as being close to the polymer network. Finally, the phosphate groups in the modified membrane were revealed to be strongly bounded to each other and to the PBI polymer backbone in contrast to the combination of weakly and strongly bounded groups of the original gel membrane.
A high-pressure route to thermoelectrics with low thermal conductivity: The solid solution series AgIn{sub x}Sb{sub 1−x}Te{sub 2} (x=0.1–0.6)
Metastable rocksalt-type phases of the solid solution series AgIn{sub x}Sb{sub 1−x}Te{sub 2} (x=0.1, 0.2, 0.4, 0.5 and 0.6) were prepared by high-pressure synthesis at 2.5 GPa and 400 °C. In these structures, the coordination number of In{sup 3+} is six, in contrast to chalcopyrite ambient-pressure AgInTe{sub 2} with fourfold In{sup 3+} coordination. Transmission electron microscopy shows that real-structure phenomena and a certain degree of short-range order are present, yet not very pronounced. All three cations are statistically disordered. The high degree of disorder is probably the reason why AgIn{sub x}Sb{sub 1−x}Te{sub 2} samples with 0.4<x<0.6 exhibit very low thermal conductivities with a total κ<0.5 W/K m and a lattice contribution of κ{sub ph} ∼0.3 W/K m at room temperature. These are lower than those of other rocksalt-type tellurides at room temperature; e.g. the well-known thermoelectric AgSbTe{sub 2} (κ ∼0.6 W/K m). The highest ZT value (0.15 at 300 K) is observed for AgIn{sub 0.5}Sb{sub 0.5}Te{sub 2}, mainly due to its high Seebeck coefficient of 160 µV/K. Temperature-dependent X-ray powder patterns indicate that the solid solutions are metastable at ambient pressure. At 150 °C, the quaternary compounds decompose into chalcopyrite-type AgInTe{sub 2} and rocksalt-type AgSbTe{sub 2}. - Graphical abstract: Reaction scheme, temperature characteristics of the ZT value and a selected-area electron diffraction pattern (background) of AgIn{sub 0.5}Sb{sub 0.5}Te{sub 2}, which crystallizes in a rocksalt-type structure with statistical cation disorder. Display Omitted - Highlights: • High-pressure synthesis yields the novel solid solution series AgIn{sub x}Sb{sub 1−x}Te{sub 2}. • In contrast to AgInTe{sub 2}, the compounds are inert at ambient pressure. • HRTEM shows no pronounced short-range order in the disordered NaCl-type structure. • The metastable phases exhibit very low total thermal conductivities <0.5 W/K m. • ZT values of 0.15 at room temperature were measured for AgIn{sub 0.5}Sb{sub 0.5}Te{sub 2}.
Investigation of some new hydro(solvo)thermal synthesis routes to nanostructured mixed-metal oxides
We present a study of two new solvothermal synthesis approaches to mixed-metal oxide materials and structural characterisation of the products formed. The solvothermal oxidation of metallic gallium by a diethanolamine solution of iron(II) chloride at 240 °C produces a crystalline sample of a spinel-structured material, made up of nano-scale particles typically 20 nm in dimension. XANES spectroscopy at the K-edge shows that the material contains predominantly Fe{sup 2+} in an octahedral environment, but that a small amount of Fe{sup 3+} is also present. Careful analysis using transmission electron microscopy and powder neutron diffraction shows that the sample is actually a mixture of two spinel materials: predominantly (>97%) an Fe{sup 2+} phase Ga{sub 1.8}Fe{sub 1.2}O{sub 3.9}, but with a minor impurity phase that is iron-rich. In contrast, the hydrothermal reaction of titanium bis(ammonium lactato)dihydroxide in water with increasing amounts of Sn(IV) acetate allows nanocrystalline samples of the SnO{sub 2}–TiO{sub 2} solid solution to be prepared directly, as proved by powder XRD and Raman spectroscopy. - Graphical abstract: New solvothermal synthesis approaches to spinel and rutile mixed-metal oxides are reported. - Highlights: • Solvothermal oxidation of gallium metal in organic iron(II) solution gives a novel iron gallate spinel. • Hydrothermal reaction of titanium(IV) complex and tin(IV) acetate produces the complete SnO{sub 2}–TiO{sub 2} solid solution. • Nanostructured mixed-metal oxide phases are produced directly from solution.
Hierarchical Na-doped cubic ZrO{sub 2} synthesis by a simple hydrothermal route and its application in biodiesel production
Hierarchical growth of cubic ZrO{sub 2} phase was successfully synthesized via a simple hydrothermal process in the presence of different surfactants (cationic, non-ionic and anionic) and sodium hydroxide. The structural and microstructural characterizations of different ZrO{sub 2} powders were performed using various techniques, such as X-ray diffraction, transmission electron microscopy, N{sub 2} adsorption–desorption, scanning electron microscopy and infrared. Results indicated that sodium addition stabilized the cubic ZrO{sub 2} phase by a Na-doping process, independently of the surfactant used. In contrast, microstructural characteristics varied as a function of the surfactant and sodium presence. In addition, water vapor (H{sub 2}O) and carbon dioxide (CO{sub 2}) sorption properties were evaluated on ZrO{sub 2} samples. Results evidenced that sample surface reactivity changed as a function of the sodium content. Finally, this surface reactivity was evaluated on the biodiesel transesterification reaction using the different synthesized samples, obtaining yields of 93%. - Graphical abstract: Hierarchical growth of cubic Na-ZrO{sub 2} phase was synthesized by hydrothermal processes in the presence of surfactants and sodium. Sodium addition stabilized the cubic phase by a Na-doping process, while the microstructural characteristics varied with surfactants. Finally, this surface reactivity was evaluated on the biodiesel transesterification reaction. - Highlights: • Cubic-ZrO{sub 2} phase was synthesized via a simple hydrothermal process. • ZrO{sub 2} structure and microstructures changed as a function of the surfactant. • Cubic-ZrO{sub 2} phase was evaluated on the biodiesel transesterification reaction.
Rapid solid-state metathesis route to transition-metal doped titanias
Rapid solid-state metathesis (SSM) reactions are often short-lived highly exothermic reactions that yield a molten alkali halide salt that aids in product growth and crystallization. SSM reactions may also produce kinetically stabilized structures due to the short (seconds) reaction times. This report describes the investigation of rapid SSM reactions in the synthesis of transition-metal doped titanias (M–TiO{sub 2}). The dopant targeted compositions were ten mol percent and based on elemental analysis, many of the M–TiO{sub 2} samples were close to this targeted level. Based on surface analysis, some samples showed large enrichment in surface dopant content, particularly chromium and manganese doped samples. Due to the highly exothermic nature of these reactions, rutile structured TiO{sub 2} was observed in all cases. The M–TiO{sub 2} samples are visible colored and show magnetic and optical properties consistent with the dopant in an oxide environment. UV and visible photocatalytic experiments with these visibly colored rutile M–TiO{sub 2} powders showed that many of them are strongly absorbent for methylene blue dye and degrade the dye under both UV and visible light illumination. This work may open up SSM reactions as an alternate non-thermodynamic reaction strategy for dopant incorporation into a wide range of oxide and non-oxides.
A chemical bath deposition route to facet-controlled Ag{sub 3}PO{sub 4} thin films with improved visible light photocatalytic activity
A facile, economic, and reproducible chemical bath deposition (CBD) method is developed for the fabrication of facet-controlled Ag{sub 3}PO{sub 4} thin films with enhanced visible light photocatalytic activity. The fine-control of bath temperature, precursor, complexing agent, substrate, and solution pH is fairly crucial in preparing the facet-selective thin film of Ag{sub 3}PO{sub 4} nanocrystal. The change of precursor from silver nitrate to silver acetate makes possible the tailoring of the crystal shape of Ag{sub 3}PO{sub 4} from cube to rhombic dodecahedron and also the bandgap tuning of the deposited films. The control of [Ag{sup +}]/[phosphate] ratio enables to maximize the loading amount of Ag{sub 3}PO{sub 4} crystals per the unit area of the deposited film. All the fabricated Ag{sub 3}PO{sub 4} thin films show high photocatalytic activity for visible light-induced degradation of organic molecules, which can be optimized by tailoring the crystal shape of the deposited crystals. This CBD method is also useful in preparing the facet-controlled hybrid film of Ag{sub 3}PO{sub 4}–ZnO photocatalyst. The present study clearly demonstrates the usefulness of the present CBD method for fabricating facet-controlled thin films of metal oxosalt and its nanohybrid. - Highlights: • The crystal facet of Ag{sub 3}PO{sub 4} films can be tuned by chemical bath deposition. • The crystal shape of Ag{sub 3}PO{sub 4} is tailorable from cube to rhombic dodecahedron. • Facet-tuned Ag{sub 3}PO{sub 4} film shows enhanced visible light photocatalyst activity.
A fresnoite-structure-related mixed valent titanium(III/IV) chlorosilicate, Ba{sub 3}Ti{sub 2}Si{sub 4}O{sub 14}Cl: A flux crystal growth route to Ti(III) containing oxides
Single crystals of mixed valent barium titanium(III/IV) chlorosilicate, Ba{sub 3}Ti{sub 2}Si{sub 4}O{sub 14}Cl{sub 0.91}O{sub 0.09}, were grown in a high temperature molten chloride flux involving an in situ reduction step. The fresnoite structure related Ba{sub 3}Ti{sub 2}Si{sub 4}O{sub 14}Cl{sub 0.91}O{sub 0.09} crystallizes in the tetragonal space group P4/mbm with lattice parameters of a=8.6717(2) Å, c=18.6492(5) Å. The title compound exhibits a 3D structure consisting of 2D layers of fused Ti{sub 2}O{sub 9} and Si{sub 4}O{sub 12} groups and 2D layers of fused Ti{sub 2}O{sub 9}Cl{sub 2} and Si{sub 2}O{sub 7} groups that are linked via barium atoms. The in situ reduction of Ti(IV) to Ti(III) is achieved via the addition of metallic Mg to the flux to function as the reducing agent. The temperature dependence of the magnetic susceptibility shows simple paramagnetism above 100 K. There is a discontinuity in the susceptibility data below 100 K, which might be due to a structural change that takes place resulting in charge ordering. - Graphical abstract: The fresnoite structure related novel reduced barium titanium chlorosilicate, Ba{sub 3}Ti{sub 2}Si{sub 4}O{sub 14}Cl{sub 0.91}O{sub 0.09}, were synthesized via flux method. An in situ reduction of Ti(IV) to Ti(III) achieved using Mg metal. The 3D structure consists 2D layers of fused Ti{sub 2}O{sub 9} and Si{sub 4}O{sub 12} and 2D layers of fused Ti{sub 2}O{sub 9}Cl{sub 2} and Si{sub 2}O{sub 7} connected via barium atoms. Compound shows simple paramagnetism above 100 K. - Highlights: • The fresnoite related Ba{sub 3}Ti{sub 2}Si{sub 4}O{sub 14}Cl{sub 0.91}O{sub 0.09} were grown via molten flux method. • The in situ reduction of Ti(IV) to Ti(III) is achieved using metallic Mg. • 2D layers of Ti{sub 2}O{sub 9} and Si{sub 4}O{sub 12} and Ti{sub 2}O{sub 9}Cl{sub 2} and Si{sub 2}O{sub 7} connect via Ba atoms. • The magnetic susceptibility shows simple paramagnetism above 100 K.
A rapid shift in the sediment routing system of Lower-Upper Oligocene strata in the Qiongdongnnan Basin (Xisha Trough), Northwest South China Sea
Not Available
MgO:Dy{sup 3+} nanophosphor: Self ignition route, characterization and its photoluminescence properties
For the first time series of MgO phosphors doped with different concentrations of Dy{sup 3+} (1–9 mol%) were prepared by solution combustion method using glycine as a fuel. The final products were well characterized by powder X-ray diffraction, Fourier transform infrared spectroscopy, scanning electron microscopy and transmission electron microscopy. The powder X-ray diffraction patterns of the as-formed product show single cubic phase. The crystallite size estimated using Scherrer's method was found to be in the range 5–15 nm and the same was confirmed by transmission electron microscopy result. Photoluminescence properties of Dy{sup 3+} (1–9 mol%) doped MgO for near ultra violet excitation (325 nm) was studied in order to investigate the possibility of its use in white light emitting diode applications. The emission spectra consists of intra 4f transitions of Dy{sup 3+}, namely {sup 4}F{sub 9/2} → {sup 6}H{sub 15/2} (483 nm), and {sup 4}F{sub 9/2} → {sup 6}H{sub 13/2} (573 nm). Further, the emission at 573 nm shows strong yellow emission and can be applied to the yellow emission of phosphor for the application for near ultraviolet excitation. The intensity of yellow emission was attributed to intrinsic defects, especially oxygen-vacancies, which could assist the energy transfer from the MgO host to the Dy{sup 3+} ions. The Commission International De I-Eclairage chromaticity co-ordinates were calculated from emission spectra, the values (x,y) were very close to the National Television System Committee standard value of white emission. Therefore, the present phosphor was highly useful for display applications. - Graphical Abstract: PL emission spectra and CIE diagram of MgO:Dy{sup 3+} nanophosphor. - Highlights: • MgO:Dy{sup 3+} prepared by simple and low cost LCS method at low temperature (400 °C). • Characteristic emission peaks of Dy{sup 3+} ion at ∼ 483 and 573 nm are recorded. • CIE co-ordinate values located in the white region. • Present phosphor was quite useful for display applications.
A new route for the synthesis of submicron-sized LaB{sub 6}
Submicron crystalline LaB{sub 6} has been successfully synthesized by a solid-state reaction of La{sub 2}O{sub 3} with NaBH{sub 4} at 1200 °C. The effects of reaction temperature on the crystal structure, grain size and morphology were investigated by X-ray diffraction, scanning electron microscope and transmission electron microscope. It is found that when the reaction temperature is in the range of 1000–1100 °C, there are ultrafine nanoparticles and nanocrystals that coexist. When the reaction temperature elevated to 1200 °C, the grain morphology transformed from ultrafine nanoparticle to submicron crystals completely. High resolution transmission electron microscope images fully confirm the formation of LaB{sub 6} cubic structure. - Highlights: • Single-phased LaB{sub 6} have been synthesized by a solid-state reaction in a continuous evacuating process. • The reaction temperature has a important effect on the phase composition. • The grain size increase from nano-size to submicron with increasing reaction temperature.