Tetrahydroborate sodalite nanocrystals: Low temperature synthesis and thermally controlled intra-cage reactions for hydrogen release of nano- and micro crystals

• Published in: Microporous and mesoporous materials 2010-07, Vol.132 (1), p.210-218
• Main Authors: Buhl, Josef-Christian, Schomborg, Lars, Rüscher, Claus Henning
• Format: Article
• Language: English
• Subjects: Agglomeration; Chemistry; Colloidal state and disperse state; Crystals; Exact sciences and technology; General and physical chemistry; Mathematical analysis; Model for hydride enclathration; Nanocrystalline solids; Nanocrystals; Nanostructure; Physical and chemical studies. Granulometry. Electrokinetic phenomena; Porous materials; Reduction; Sodalite; Synthesis; Tetrahydroborate sodalite; Thermal behaviour; X-rays
• ISSN: 1387-1811; 1873-3093
• DOI: 10.1016/j.micromeso.2010.02.022

Tetrahydroborate sodalite nanoparticles were successfully synthesized under low temperature hydrothermal conditions (333 K) from high alkaline aluminosilicate gels and NaBH 4 salt. The products were characterized by X-ray powder diffraction, scanning electron microscopy, FTIR spectroscopy and thermogravimetry in comparison with the microcrystalline sample Na 8[AlSiO 4] 6(BH 4) 2· NaBH 4-sodalite of 25 nm average crystal size agglomerated by X-ray amorphous hydrosodalite type phase to bigger particles up to ∼100 nm was observed after a reaction period of 12 h. The sodalite host framework protects the BH 4 - ions from hydrolysis under open conditions at room temperature. Hydrogen release is detected via nitrate tracer reduction in temperature dependent IR (TIR) experiments. A total conversion of the BH 4 groups for the nanocrystalline sodalite sample is reached at 773 K whereas a larger amount of the BH 4 - -units remained stable within the microcrystalline sample under the same conditions. This can be explained by the smaller crystal size and the high amount of inter grown hydrosodalite type phase in the BH 4 - -sodalite nanocrystals compared to the microcrystals. The minor hydrosodalite type phase also present in the microcrystalline sample can be reloaded with water and the main hydrogen release reaction BH 4 - + 2H 2O => 4H 2 + BO 2 − can be continued.