Abstract Characterization of material structure with X-ray or neutron scattering using e.g. Pair Distribution Function (PDF) analysis most often rely on refining a model against an experimental dataset. However, identifying suitable is bottleneck. Recently, automated approaches have made it possible to test thousands models for each dataset, but these methods are computationally expensive and analysing the output, i.e. extracting structural information from resulting fits in meaningful way,...

Understanding nucleation mechanisms of the solid state on an atomic scale is crucial in order to develop new synthesis methods for tailored materials. Here, we use situ X-ray total scattering follow structural rearrangements that take place formation tungsten oxide, all way from ionic precursor clusters solution final crystalline nanoparticles. The reaction was performed water and oleylamine study influence solvent, both cases, present adopted well-known α-Keggin polyoxometalate structure....

The combination of in situ pair distribution function (PDF) analysis and small-angle X-ray scattering (SAXS) enables the formation mechanism metal oxido nanoclusters cluster-solvent interactions as they take place. Herein, we demonstrate method for clusters with a [Bi

Nanosizing of metal oxide particles is a common strategy for improving materials properties; however, small often take structures different from the bulk material. MoO2 nanoparticles show structure that distinct distorted rutile and which has not yet been determined. Here, we present model nanostructured obtained through detailed atomic pair distribution function analysis combined with high-resolution electron microscopy. Defects occur in arrangement [MoO6] octahedra, both large (40-100 nm)...

Molybdenum oxides and sulfides on various low-cost high-surface-area supports are excellent catalysts for several industrially relevant reactions. The surface layer structure of these materials is, however, difficult to characterize due small disordered MoO

The structure of lanthanide(III) ions in solutions high nitrate has been debated since the early days lanthanide coordination chemistry. and properties lanthanides these are essential industrial rare-earth separation, as well fundamental solution chemistry elements. Pending decades debate, it was established that is bidentate coordinates inner sphere, complexes have observed with many four nitrates coordinated to a single center nonaqueous solutions. We revisit interactions between...

The properties of functional materials are intrinsically linked to their atomic structure. When going the nanoscale, size-induced structural changes in structure often occur, however these rarely well-understood. Here, we systematically investigate tungsten oxide nanoparticles as a function nanoparticle size and observe drastic when particles smaller than 5 nm, where amorphous. synthesized by thermal decomposition ammonium metatungstate hydrate oleylamine varying concentration, size, shape...

Layered manganese oxide materials are widely used in sodium and lithium ion batteries, but significant discrepancies encountered the literature with respect to their electrochemical properties. This could be due difficulties establishing exact phase compositions crystal structures (typically P2, P3, O2, O3, distorted analogues, e.g., P'2, hydrated - PH2, or carbonated PC2, phases) of a given synthesis product, especially when only crude crystallographic indexing is without structural...

Hydrothermal synthesis offers an environmentally benign method for of LiMn₂O₄anode material, but characterization is challenging due to structurally related impurity phases such as Li_xMn_yO₂and Mn₃O₄, whose presence may explain the inconsistent properties in published literature.

Amphoteric oxides can be challenging to produce in phase pure form due their sensitivity the pH of reaction mixture. The high-pressure, high-temperature conditions hydrothermal processes make difficult control. Here we report a simple approach obtain nanoparticles amphoteric oxides, where cheap metal nitrate precursors are reacted alcohol (2-propanol) water mixtures (25 vol%:75 vol%) maintain neutral under solvothermal conditions. Phase SnO2 were synthesized continuous flow reactor at 250...

Platinum nanocrystals with a fine control of the crystal domain size in range 1.0-2.2 nm are produced by tuning NaOH concentration during UV-induced reduction H2PtCl6 surfactant-free alkaline ethylene glycol. The colloidal solutions obtained characterized transmission electron microscopy and pair distribution function analysis, allowing analysis both atomic nanoscale structures. nanoparticles exhibit face-centered cubic structure even for smallest nanoparticles, unit cell parameter is...

Understanding material nucleation processes is crucial for the development of synthesis pathways tailormade materials. However, we currently have little knowledge influence precursor solution structure on formation pathway We here use in situ total scattering to show how influences which crystal formed during hydrothermal tungsten oxides. investigate oxide from two polyoxometalate salts, ammonium metatungstate, and paratungstate. In both cases, a hexagonal bronze (NH4)0.25WO3 as final...

Abstract Molybdenum oxide (5 to 20 wt.%) supported on calcium or strontium hydroxyapatite were investigated as catalysts for selective oxidation of methanol formaldehyde. These both active and selective, with a maximum yield achieved at 95 % conversion 96 selectivity. The main byproducts CO (3.2 %) dimethyl ether (DME, 0.7 %). catalytic performance the was measured up 600 h 350 °C. Compared an industrial iron molybdate catalyst, based deactivated slower. species found be surface layer MoO x...

In situ measurements of the hydrothermal formation LiMn2O4 (LMO) nanocrystallites reveal that reaction progresses in steps, each creating a different crystalline phase. The route is summarized as KMnO4→disordered δ-MnO2→(ordered δ-MnO2)→LiMn2O4→(γ-Mn2O3)→Mn3O4. phase purity LMO can be controlled by time and temperature where pure obtained after 150–210 seconds at 220 °C or 45–140 260 °C. It also concluded production this method comes price reduced yield. From observed an alternative way to...

Mapping of MWO 4 metal tungstate formation pathways via pair distribution function analysis shows that disorder in the initial precursor structure affects crystallization process.

Abstract The combination of in situ pair distribution function (PDF) analysis and small‐angle X‐ray scattering (SAXS) enables the formation mechanism metal oxido nanoclusters cluster–solvent interactions as they take place. Herein, we demonstrate method for clusters with a [Bi 38 O 45 ] core. Upon dissolution crystalline 6 5 (OH) 3 (NO ) ]⋅3 H 2 DMSO, an intermediate rapidly forms, which slowly grows to stable clusters. To identify intermediate, developed automated modeling method, where...

Amphoteric oxides can be challenging to produce in phase pure form due their sensitivity the pH of reaction mixture. The high-pressure, high-temperature conditions hydrothermal processes make difficult control. Here we report a simple approach obtaining nanoparticles amphoteric oxides, where cheap metal nitrate precursors are reacted alcohol (2-propanol) water mixtures (25 vol.%:75 vol.%) maintain neutral under solvothermal conditions. Phase SnO2 were synthesized continuous flow reactor at...

Understanding material nucleation processes is crucial for the development of synthesis pathways tailormade materials. However, we currently have little knowledge influence precursor solution structure on formation pathway We here use in situ total scattering to show how influences which crystal formed during hydrothermal tungsten oxides. investigate oxide from two polyoxometalate salts, ammonium metatungstate and paratungstate. In both cases, a hexagonal bronze (NH4)0.25WO3, as final...

The properties of functional materials are intrinsically linked to their atomic structure. When going the nanoscale, size-induced structural changes in structure often occur, however these rarely well-understood. Here, we systematically investigate tungsten oxide nanoparticles as a function nanoparticle size and observe drastic when particles smaller than 5 nm, where amorphous. synthesized by thermal decomposition ammonium metatungstate hydrate oleylamine varying concentration, size, shape...

Understanding material nucleation processes is crucial for the development of synthesis pathways tailormade materials. However, we currently have little knowledge influence precursor solution structure on formation pathway We here use in situ total scattering to show how influences which crystal formed during hydrothermal tungsten oxides. investigate oxide from two polyoxometalate salts, ammonium metatungstate and paratungstate. In both cases, a hexagonal bronze (NH4)0.25WO3, as final...

The realization of autonomous IOT sensors and devices will require the development high performance microbatteries. Though numerous microfabrication methods lead to successful creation sub-millimeter scale electrodes, practical approaches that provide cost-effective nanoscale resolution for energy storage remain elusive. We have developed an approach direct imprint patterning crystalline metal oxides using a soft polymer master inks containing concentrations nanoparticles dispersed in...