Mechanochemical synthesis of low-fluorine doped aluminum hydroxide fluorides
Different aluminum hydroxide fluorides with varying Al/F molar ratios from 1:1.5 up to 1:0.05 were successfully synthesized by mechanochemical reactions. The characterization of the products by XRD, {sup 27}Al and {sup 19}F MAS NMR, thermal analysis, nitrogen adsorption and zeta potential techniques allows a detailed understanding of the structure and surface properties of the products. Using γ-Al(OH){sub 3} and β-AlF{sub 3}·3H{sub 2}O as OH- and F-sources, respectively, strongly disordered products were obtained with an Al: F molar ratio higher than 1:0.25. The fluorination degree has affected the amount of 4- and 5-fold coordinated Al sites, not present in the reactants. An evolution of the sub-coordinated Al-species has been detected also as a consequence of annealing processes. Obviously, these species affect the phase transition to alumina, by decreasing the transition temperature of the formation of α-Al{sub 2}O{sub 3}. Synthesis conditions (milling time, fluorination degree) play a crucial role for the product composition. - Graphical abstract: The impact of the combined action of the milling and the different fluorine doping on the structure of new aluminum hydroxide fluorides was followed by {sup 27}Al and {sup 19}F NMR and by other complementary techniques. - Highlights: • Low F-doped Al-hydroxide fluorides can be successfully prepared by mechanosynthesis. • Both F-doping and mechanochemical synthesis introduce a high number of defects in the structure. • The fluorination degree affects the amount of 4- and 5-fold coordinated Al sites as well as the transition temperature to corundum.
- OSTI ID:
- 22658095
- Journal Information:
- Journal of Solid State Chemistry, Journal Name: Journal of Solid State Chemistry Vol. 243; ISSN 0022-4596; ISSN JSSCBI
- Country of Publication:
- United States
- Language:
- English
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