Abstract:Abstraer. There have been great improvements in the quality of 27A1 NMR spectra from solids over the last decade. The impact of this technique on structure determination fora wide range of solids is briefly reviewed. Emphasis is placed on the effects arising from the presence of the quadrupolar interaction and strategies that allow unambiguous spectral interpretation. It is demonstrated that in addition to the chemical shift, the quadrupolar interaction itself can be a rich source of local information about so… Show more
“…On the other hand, the tetrahedral peak at 54 ppm is more intense and sharper in the spectrum of the nanoparticles. A resonance corresponding to penta-coordinated Al, at 32 ppm, is clearly observable; this peak has been reported to be commonly observed in oxides formed by sol-gel processes [23]. These results confirm that elemental aluminum was incorporated into the silica framework affecting its tetrahedral configuration.…”
Section: Characterization Of the Si-al Nanoparticlessupporting
Blast-furnace slag (BFS) has been used as a feedstock for CO 2 sequestration by indirect mineral carbonation to produce calcium carbonate precipitates and solid residues. The most-abundant elements in these residues, Si and Al, are usually considered to be impurities that need to be removed in acid-dissolution processes involving BFS. The co-production of value-added materials from these residues is an attractive option for strengthening the economic competitiveness of mineral carbonation methods. In view of this, we separated the Si and Al, as their hydrated forms, during the dissolution of BFS in acetic acid prior to carbonation. During the sol-gel processing of Si-Al nanoparticles, a catalyst is usually required during the hydrolysis and subsequent condensation processes. In this study, only condensation occurs because the low-concentrations of acetic acid used facilitate in-situ hydrolysis during the dissolution process. Aging was carried out not only to structurally arrange the Si and Al but also to oxidize the marginal Fe(II) to reddish Fe(III). Silica-alumina nanoparticles (78% Si and 22% Al) were prepared by a simple sol-gel route at ambient pressure. These nanoparticles were amorphous and below 20 nm in size. Fourier-transform infrared (FT-IR) studies reveal that the nanoparticles consist of Si-O-Si and Si-O-Al bonds. 27 Al nuclear magnetic resonance (NMR) spectroscopy reveals a significant resonance corresponding to tetra-coordinated Al inside the particle framework.
“…On the other hand, the tetrahedral peak at 54 ppm is more intense and sharper in the spectrum of the nanoparticles. A resonance corresponding to penta-coordinated Al, at 32 ppm, is clearly observable; this peak has been reported to be commonly observed in oxides formed by sol-gel processes [23]. These results confirm that elemental aluminum was incorporated into the silica framework affecting its tetrahedral configuration.…”
Section: Characterization Of the Si-al Nanoparticlessupporting
Blast-furnace slag (BFS) has been used as a feedstock for CO 2 sequestration by indirect mineral carbonation to produce calcium carbonate precipitates and solid residues. The most-abundant elements in these residues, Si and Al, are usually considered to be impurities that need to be removed in acid-dissolution processes involving BFS. The co-production of value-added materials from these residues is an attractive option for strengthening the economic competitiveness of mineral carbonation methods. In view of this, we separated the Si and Al, as their hydrated forms, during the dissolution of BFS in acetic acid prior to carbonation. During the sol-gel processing of Si-Al nanoparticles, a catalyst is usually required during the hydrolysis and subsequent condensation processes. In this study, only condensation occurs because the low-concentrations of acetic acid used facilitate in-situ hydrolysis during the dissolution process. Aging was carried out not only to structurally arrange the Si and Al but also to oxidize the marginal Fe(II) to reddish Fe(III). Silica-alumina nanoparticles (78% Si and 22% Al) were prepared by a simple sol-gel route at ambient pressure. These nanoparticles were amorphous and below 20 nm in size. Fourier-transform infrared (FT-IR) studies reveal that the nanoparticles consist of Si-O-Si and Si-O-Al bonds. 27 Al nuclear magnetic resonance (NMR) spectroscopy reveals a significant resonance corresponding to tetra-coordinated Al inside the particle framework.
“…Another technique that shows considerable promise for examining SGAs is Solid State Magic Angle Spinning NMR (SS MAS NMR) [15]. SS MAS NMR studies gives insight into the structural co-ordination of all the aluminium ions in the structure, irrespective of long range ordering [16], which is key to understanding the forms of alumina. Chemical shift ranges for aluminium in different coordinations with oxygen (or hydroxyls) are typically −10 to 20 ppm for octahedrally coordinated aluminium (AlO 6 ), 30 to 40 ppm for pentahedrally coordinated aluminium (AlO 5 ) and 50 to 80 ppm for tetrahedrally coordinated aluminium (AlO 4 ) [16,17].…”
Section: A More Complex Problem?mentioning
confidence: 99%
“…SS MAS NMR studies gives insight into the structural co-ordination of all the aluminium ions in the structure, irrespective of long range ordering [16], which is key to understanding the forms of alumina. Chemical shift ranges for aluminium in different coordinations with oxygen (or hydroxyls) are typically −10 to 20 ppm for octahedrally coordinated aluminium (AlO 6 ), 30 to 40 ppm for pentahedrally coordinated aluminium (AlO 5 ) and 50 to 80 ppm for tetrahedrally coordinated aluminium (AlO 4 ) [16,17]. Several NMR studies explore the transition aluminas [17][18][19][20][21] but the technique has not yet been widely applied to SGAs.…”
Fines in smelter grade aluminas are recognised as a significant process problem in aluminium smelting. However the understanding of the nature of this fine material and how it impacts on the reduction process are less clearly understood. The combination of new analytical methods such as Variable Pressure Scanning Electron Microscopy and very high field Solid State NMR provide new insights into the spatial distribution of phases within aluminas, and suggest how such fine materials are generated, particularly during calcination in the alumina refinery.
“…Typically Al 3 is found in a pure octahedral co-ordination (like in a-Al 2 O 3 ) or in both, octahedral and tetrahedral co-ordination (like in g-Al 2 O 3 or q-Al 2 O 3 ). CN 5 is also found for oxygen polyhedra around Al 3 [15].…”
Section: Structural Aspects Leading To Doubts About a Simple Model Ofmentioning
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