Synchrotron-Based Method for the Study of Crystallization: Templated Formation of CoALPO-5 Catalyst

Rey, Fernando; Sankar, Gopinathan; Thomas, John Meurig; Barrett, Phillip A; Lewis, Dewi W.; Catlow, C. Richard A.; Clark, S. M.; Greaves, G. Neville

doi:10.1021/cm00056a004

Cited by 62 publications

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“…It is very difficult to establish how crystals actually evolve during growth by applying experimental techniques for a wide range of reasons; e.g., due to limitations arising from the crystallization apparatus, the specific experimental conditions required or the time scales involved. [9][10][11][12][13][14][15][16][17] Solution-based synthesis approaches are the most widely adopted ''bottom-up'' strategies, which enable the precise control of the nanocrystals size, shape and composition of nanocrystals during the growth process and hence the ability to tailor their properties at the nanoscale size. [18][19][20][21][22] Considerable knowledge has evolved regarding a general understanding of the nucleation and growth processes in solution; however, the crystal structure prediction resulting from a specific reaction is still elusive.…”

Section: Introductionmentioning

confidence: 99%

On the reversed crystal growth of BaZrO3 decaoctahedron: shape evolution and mechanism

Moreira

Andrés

Mastelaro³

et al. 2011

CrystEngComm

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BaZrO 3 (BZO) nanoparticles were nucleated, grown and subsequently self-assembled into a 3D decaoctahedronal architecture via a microwave-assisted hydrothermal (MAH) method. X-Ray diffraction (XRD), field emission scanning microscopy (FE-SEM), X-ray absorption spectroscopy (XAFS) as well as both photoluminescence (PL) and radioluminescence (RL) emission studies have provided fundamental insight into the nature of the anisotropic crystal growth mechanism of BZO nanocrystals into their final decaoctahedral shape. The growth mechanism of the assembled nanoparticles via mesoscale transformations to form BZO decaoctahedrons occurs from the surface to the core along a reversed crystallization route. This pathway is accompanied by a large enhancement of RL emissions while the intensity of PL emissions is enhanced and worsened along the process. The analysis of the results reveals a relationship between the decaoctahedrons obtained and their optical properties.

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Section: Introductionmentioning

confidence: 99%

On the reversed crystal growth of BaZrO3 decaoctahedron: shape evolution and mechanism

Moreira

Andrés

Mastelaro³

et al. 2011

CrystEngComm

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“…[6,10] In situ characterization of silicalite has been attempted by NMR spectroscopy, [11] SAXS, [12] and X-ray diffraction (XRD). [13] Relatively few in situ studies have been reported in which attempts were made to follow the crystallization of practically used aluminophosphate molecular sieves. [4,6,10,11,14,15] Raman spectroscopy is a suitable technique to investigate aqueous solutions as well as solid phases of zeolite synthesis mixtures because of the low Raman scattering cross section of water.…”

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confidence: 99%

In Situ UV Raman Spectroscopic Study on the Synthesis Mechanism of AlPO‐5

et al. 2009

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“…It is important to note that both these studies referred to above used triethylamine as the organic template, which is well-known to produce a CHA phase as a competing material, under certain conditions. 35 Although the CHA phase was not observed during the crystallisation process (with the given XRD detection limit), the use of this template may have a different effect on the Co(II) ions. For example, an ex situ XRD/Diffuse Reectance Spectroscopy (DRS) study 36 on the formation of MeAlPOs observed a pseudo-octahedral Co(II) species during the formation of CoAlPO-5 (AFI).…”

Section: Resultsmentioning

confidence: 99%

Time resolved in situ X-ray diffraction study of crystallisation processes of large pore nanoporous aluminophosphate materials

2015

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Time resolved high-resolution X-ray powder diffraction was utilized to obtain detailed changes in the crystal structure parameters during the hydrothermal crystallization process of the nanoporous aluminophosphate AlPO-5 (AFI) structure. This in situ study offered not only the influence of metal ions on the onset of crystallization and estimation of the activation energy of the process, but also allowed us to determine in detail the changes in lattice parameters during this process. More importantly the time-resolved study clearly showed the lattice expansion in the divalent metal ions substituted system right from the on-set of crystallization process, compared to the one without any dopant ions, which suggest that an amorphous or poorly crystalline network is formed prior to crystallization that contains the large divalent ions (compared to Al(iii), the substituting element), which is in agreement with the combined XAS/XRD study reported earlier. A mechanism based on this and the earlier study is suggested.

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Synchrotron-Based Method for the Study of Crystallization: Templated Formation of CoALPO-5 Catalyst

Cited by 62 publications

References 0 publications

On the reversed crystal growth of BaZrO3 decaoctahedron: shape evolution and mechanism

On the reversed crystal growth of BaZrO3 decaoctahedron: shape evolution and mechanism

In Situ UV Raman Spectroscopic Study on the Synthesis Mechanism of AlPO‐5

Time resolved in situ X-ray diffraction study of crystallisation processes of large pore nanoporous aluminophosphate materials

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