Synthesis of CaNb2O6 with a Rynersonite-like Structure: Morphology, Rietveld Refinement, Optical, and Vibrational Properties.

In this study, we report the easy and low-cost synthesis of calcium niobate (CaNb2O6) with the isomorphic structure of the Rynersonite mineral for CaTa2O6. The samples were prepared by the ball milling method at room temperature at a synthesis time of 0.5, 1, 2, 3, and 4 h. The structural analysis by XRD, Rietveld refinement, and vibrational Raman spectroscopy confirms all diffraction peaks and active mode characteristics of the pure phase of CaNb2O6 for the 3-h and 4-h samples, with a crystallite size of 22.5 and 23.2 nm, respectively. The optical band gap obtained was 3.18(2) eV (3-h sample), lower than the optical band gap for niobium oxide, characteristic of materials with strong photon absorption in the UVA region of the spectrum. The surface analysis by scanning electron microscopy reveals the obtention of several agglomerates of irregular particles ranging in the submicro and micro scales. Therefore, the present approach successfully obtained calcium niobate with the formula CaNb2O6 at a short synthesis time and room temperature.

Rietveld Refinement, Morphology, and Optical and Photoluminescence Properties of a ß-Ag1.94Cu0.06MoO4 Solid Solution.

Corner-truncated cubic ß-Ag1.94Cu0.06MoO4 microcrystals were synthesized using the hydrothermal method. These were investigated by X-ray diffraction, confirming obtention of the spinel structure Fd3̅m. Through Raman spectroscopy are confirmed all modes for the point group of Oh7. The Egap shows a decrease of the band gap from 3.20 to 3.07 eV, with reduction of the conduction band occurring from -0.20 eV (ß-Ag2MoO4) to -0.13 eV (ß-Ag1.94Cu0.06MoO4), suggesting a p-type behavior for the Cu2+ ion. The field-emission scanning electron microscopy images confirm the morphological changes for ß-Ag2MoO4, where potato-like microcrystals were found. Meanwhile, corner-truncated cubic microcrystals for ß-Ag1.94Cu0.06MoO4. The photoluminescence (PL) spectrum confirms the increase in the PL emission for ß-Ag1.94Cu0.06MoO4, with suppression of the deep defects occurring in the structure caused by oxygen and silver atoms. In contrast, the green region is intensified because of distortions of the Ag-O and Mo-O bonds. Therefore, the ß-Ag1.94Cu0.06MoO4 solid solution has PL emission with CCT (4510 K) and CIE coordinates (x = 0.372 and y = 0.433), which could be interesting properties for applications as light-emitting diodes.

Structural and Optical Properties of Ca0.9Cu0.01WO4 Solid Solution Synthesized by Sonochemistry Method at Room Temperature.

In this work, we report the room-temperature synthesis of pure calcium tungstate (CaWO4) and copper-doped calcium tungstate solid solution (Ca0.99Cu0.01WO4) by using a sonochemistry method. These materials were structurally characterized by X-ray diffraction (XRD) and Raman spectroscopy. The obtained XRD patterns were submitted to a Rietveld refinement showing, in both materials, a tetragonal phase with space group and point group of I41/a and C4h6, respectively. Microscopy images of both materials, obtained by field emission scanning electron microscopy, showed spherical agglomerated structures composed by spherical nanoparticles, while calcium and tungstate elements were identified by energy-dispersive X-ray spectroscopy for pure calcium tungstate and copper, calcium, and tungstate for Ca0.99Cu0.01WO4 solid solution. The decrease of optical band gap (Egap) from 4.0 eV (CaWO4) to 3.45 eV (Ca0.99Cu0.01WO4) confirmed the substitution of calcium atoms for copper atoms in the clusters [CaO8]. Maximum photoluminescence (PL) emission was shifted from 522 nm in the pure CaWO4 to 475 nm in the Ca0.99Cu0.01WO4 solid solution. Consequently, there was an increase of PL emissions intensity in the blue and green regions of the visible spectrum, due to electronic transitions between the orbitals O 2p, Cu 3d, and W 5d.