A multiple-quantum 23Na MAS NMR study of amorphous sodium gallium silicate zeolite precursors

Antonijevic, Sasa; Ashbrook, Sharon E.; Walton, Richard I.; Wimperis, Stephen

doi:10.1039/b201581c

Cited by 20 publications

(21 citation statements)

References 46 publications

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“…The incorporation of aluminum into the silicate framework is also accompanied by association with charge-compensating Na + cations, as indicated by an increase in the Na-O peak in radial distribution functions from neutron scattering data. These results are similar to those reported by Antonijevic et al [65] for the formation of gallosilicate zeolites [66], for which similar ordering processes were observed by 71 Ga MAS NMR. The conversion of six-coordinated gallium species of the starting material into four-coordinated gallium atoms was monitored prior to crystallization.…”

Section: Zeolite Crystallization From Alkaline Solutions and Amorphousupporting

confidence: 93%

“…While no great differences have been encountered by the substitution of aluminum by gallium [65,66], Zones and Hwang studied the formation of borosilicate SSZ-42 and aluminosilicate zeolite BEA, which have different structures, from intermediate gels that were identical except for containing B 2 O 3 or Al 2 O 3 , respectively [83]. By using 1 H, 11 B, and 27 Al MAS NMR in conjunction with X-ray scattering and elemental analysis, they found that the borosilicate system crystallized more rapidly then the aluminosilicate system, when both reactions were carried out in the presence of N-benzyldiaza-bicyclo[2.2.2.…”

Section: Zeolite Crystallization From Alkaline Solutions and Amorphoumentioning

confidence: 98%

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Nucleation and growth of zeolites and inorganic mesoporous solids: Molecular insights from magnetic resonance spectroscopy

Epping

Chmelka

2006

Current Opinion in Colloid & Interface Science

139

117

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Section: Zeolite Crystallization From Alkaline Solutions and Amorphousupporting

confidence: 93%

Section: Zeolite Crystallization From Alkaline Solutions and Amorphoumentioning

confidence: 98%

Nucleation and growth of zeolites and inorganic mesoporous solids: Molecular insights from magnetic resonance spectroscopy

Epping

Chmelka

2006

Current Opinion in Colloid & Interface Science

139

117

View full text Add to dashboard Cite

“…Despite the fairly small chemical shift range of 23 Na, some general trends with structure have been observed, particularly within groups of similar materials. For example, a number of correlations between isotropic chemical shift (d CS ) and Na-O distances and coordination number, [3][4][5][6][7][8][9] have been observed, particularly for silicates [4][5][6] and fluorides, 8,9 and whilst they are not identical, it is clear that sodium atoms with a larger number of oxygen or fluorine near neighbours (usually, therefore, with a higher average bond distance) exhibit a lower chemical shift. The significant progress in the development of ab initio calculations of NMR parameters over the past few years has also facilitated the study of the variation of NMR parameters with structural changes.…”

Section: Introductionmentioning

confidence: 99%

²³Na multiple-quantum MAS NMR of the perovskites NaNbO₃and NaTaO₃

Ashbrook

Pollès

Gautier

et al. 2006

Phys. Chem. Chem. Phys.

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The distorted perovskites NaTaO(3) and NaNbO(3) have been studied using (23)Na multiple-quantum (MQ) MAS NMR. NaTaO(3) was prepared by high temperature solid state synthesis and the NMR spectra are consistent with the expected room temperature structure of the material (space group Pbnm), with a single crystallographic sodium site. Two samples of NaNbO(3) were studied. The first, a commercially available sample which was annealed at 900 degrees C, showed two crystallographic sodium sites, as expected for the room temperature structure of the material (space group Pbcm). The second sample, prepared by a low temperature hydrothermal method, showed the presence of four sodium sites, two of which match the expected room temperature structure and the second pair, another polymorph of the material (space group P21ma). This is consistent with powder X-ray diffraction data which showed weak extra peaks which can be accounted for by the presence of this second polymorph. Density functional theory (DFT) calculations support our conclusions, and aid assignment of the NMR spectra. Finally, we discuss the measured NMR parameters in relation to other studies of sodium in high coordination sites in the solid state.

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“…The external surface area of the amorphous precursor nanoparticles, To get further information, 23 Na MAS and multiple-quantum MAS (MQMAS) NMR was used, as it was previously shown that this technique has the potential to shed more light on the nature of the structural units present in the amorphous precursor nanoparticles. [17] 23 Na MAS NMR spectra of dehydrated amorphous precursor nanoparticles, FAU and SOD nanocrystals are recorded at two magnetic fields of 11.7 and 20.0 T ( Figure S2, Table S3). These results enable us to distinguish between the effects of second order quadrupolar interaction and chemical shift distribution.…”

Section: Resultsmentioning

confidence: 99%

Transformation of Discrete Amorphous Aluminosilicate Nanoparticles into Nanosized Zeolites

Guo

Zhao

Martineau‐Corcos

et al. 2020

Adv Materials Inter

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The effect of amorphous aluminosilicate precursor nanoparticles on the formation of nanosized zeolites with faujasite (FAU) and sodalite (SOD) type frameworks is illustrated using a new synthetic strategy to prepare nanosized zeolites with tailored particle size distribution, morphology, and structure. This two‐step synthesis procedure includes the formation of colloidal suspensions followed by separation of the amorphous precursor nanoparticles, and their subsequent transformation into nanosized crystals by treatment with alkali suspensions (NaOH) solutions only. The selective transformation of the amorphous nanoparticles into FAU and SOD nanosized crystals is studied at atomistic and microscopic levels using 29Si and 23Na nuclear magnetic resonanse (NMR) spectroscopy, X‐ray powder diffraction, and N2 physisorption, respectively. The presence of sodalite cages occluding highly mobile sodium in the amorphous nanoparticles is confirmed by 23Na‐1H D‐HMQC NMR spectroscopy. The subsequent treatment of these amorphous precursor particles with aqueous sodium hydroxide illustrates that the cations are not only charge compensators but also inorganic templates stabilizing sodalite cages during the long‐range ordering in the amorphous particles.

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A multiple-quantum 23Na MAS NMR study of amorphous sodium gallium silicate zeolite precursors

Cited by 20 publications

References 46 publications

Nucleation and growth of zeolites and inorganic mesoporous solids: Molecular insights from magnetic resonance spectroscopy

Nucleation and growth of zeolites and inorganic mesoporous solids: Molecular insights from magnetic resonance spectroscopy

²³Na multiple-quantum MAS NMR of the perovskites NaNbO₃and NaTaO₃

Transformation of Discrete Amorphous Aluminosilicate Nanoparticles into Nanosized Zeolites

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A multiple-quantum 23Na MAS NMR study of amorphous sodium gallium silicate zeolite precursors

Cited by 20 publications

References 46 publications

Nucleation and growth of zeolites and inorganic mesoporous solids: Molecular insights from magnetic resonance spectroscopy

Nucleation and growth of zeolites and inorganic mesoporous solids: Molecular insights from magnetic resonance spectroscopy

23Na multiple-quantum MAS NMR of the perovskites NaNbO3and NaTaO3

Transformation of Discrete Amorphous Aluminosilicate Nanoparticles into Nanosized Zeolites

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²³Na multiple-quantum MAS NMR of the perovskites NaNbO₃and NaTaO₃