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1.
Dalton Trans ; 50(17): 5883-5889, 2021 May 04.
Artículo en Inglés | MEDLINE | ID: mdl-33949545

RESUMEN

Barium oxynitridosilicates, Ba3Si6O12N2 and Ba3Si6O9N4, were obtained from a mixture of BaCN2 and SiO2 at 800 °C, which is several hundred degrees lower than the temperature required in solid state reactions using BaCO3, SiO2 and Si3N4. The low-temperature formation mechanism was investigated by thermogravimetry analysis in conjunction with gas chromatography and mass spectroscopy. The phase ratio between the oxynitridosilicates was controlled by tuning the reaction temperature, duration, and atmosphere. Almost single-phase Ba3Si6O12N2 was obtained by reaction at 800 °C for 15 h under a N2 atmosphere, but the product changed to Ba3Si6O9N4 after 50 h at 800 °C or by heating at 950 °C for 15 h. The photoluminescence properties of Eu-doped products obtained at 800 °C using a mixture of BaCN2 : Eu and SiO2 were investigated.

2.
Langmuir ; 36(22): 6277-6285, 2020 Jun 09.
Artículo en Inglés | MEDLINE | ID: mdl-32423218

RESUMEN

Amorphous high-surface-area aluminum hydroxide-bicarbonates were synthesized starting from AlCl3, base, and bicarbonate in water. Composites with a chemical formulas of [Al13O4(µ-OH)24(H2O)6.5(OH)5.5](HCO3)1.5 (I-NaOH) and [Al13O4(µ-OH)24(H2O)6(OH)6](HCO3) (I-NH3) were obtained by the use of NaOH/NaHCO3 and NH3/NH4HCO3 as base/bicarbonate, respectively. The surface area of the composites was highly dependent on the pH level of the synthetic solution, and composites with high surface areas (ca. 200 m2 g-1) were obtained around pH 7-8. Pore-size distributions determined from the N2 adsorption isotherms showed that I-NH3 and I-NaOH possess mainly large (pore radius rp > 3 nm) and small (rp < 3 nm) pores, respectively, despite similar surface areas. While SEM images showed that both I-NH3 and I-NaOH were aggregates of nanoparticles, the particles were more fused in I-NaOH, which is in line with the existence of small pores and the use of a stronger base (NaOH), which would facilitate the dehydration condensation reaction. The composites were applied as adsorbents to remove methyl orange (MO) from water. The time course of MO adsorption was readily fitted with a pseudo-second-order model, and over 90% MO removal was attained within 10 min with I-NH3, while I-NaOH showed much less MO removal (26%). The MO adsorption isotherm of I-NH3 was reproduced with a Langmuir model with an adsorption capacity of 154 mg g-1. Notably, the aluminum hydroxide-bicarbonates could not absorb methylene blue, which is a cationic dye, while anions (MO and PO43-) were readily absorbed. Solid-state 27Al MAS NMR spectra showed that the concentration of 5-coordinated aluminum species, which may serve as guest binding sites, was higher for I-NH3. These results show that electrostatic interaction between anionic MO and coordinatively unsaturated 5-coordinated cationic aluminum species and the large external surface area of I-NH3 contribute to the highly efficient MO adsorption.

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