Journal
JOURNAL OF APPLIED CRYSTALLOGRAPHY
Volume 55, Issue -, Pages 484-502Publisher
INT UNION CRYSTALLOGRAPHY
DOI: 10.1107/S1600576722003594
Keywords
chrysotile; Rietveld refinement; nanocrystallites; transmission electron microscopy (TEM); X-ray diffraction (XRD)
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Funding
- Russian Science Foundation [19-13-00151]
- Lomonosov Moscow State University Program of Development
- Russian Science Foundation [19-13-00151] Funding Source: Russian Science Foundation
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The morphology and structure of (NixMg1-x)(3)Si2O5(OH)(4) synthetic phyllosilicate nanoscrolls were investigated, revealing the mechanism and direction of scrolling, and concluding that scrolling is an effective means of stress relaxation.
The morphology and structure of (NixMg1-x)(3)Si2O5(OH)(4) synthetic phyllosilicate nanoscrolls have been studied by means of electron microscopy and X-ray powder diffraction. Scrolling of phyllosilicate layers originates from size differences between octahedral and tetrahedral sheets. This strain-energy-driven process raises a number of questions, including the preferred direction of scrolling (along the a or b axis) and the presence of residual microstrain. In order to clarify these points, the structure of (NixMg1-x)(3)Si2O5(OH)(4) phyllosilicates (x = 0, 0.33, 0.5, 0.67, 1) was first described by a monoclinic Cc (9) unit cell, whose parameters decrease with increasing Ni concentration. The Williamson-Hall plots constructed for x = 0 and 0.67 reveal the absence of microstrain, which suggests that scrolling is an effective means of stress relaxation. The sizes of the crystallites were determined by using Rietveld refinement with predefined needle-like models and fundamental parameter fitting with crystallites of arbitrary form. Both approaches show qualitative and quantitative correlation, in terms of aspect ratio, with electron microscopy data. At the same time, the phyllosilicates studied do not demonstrate one preferred direction of scrolling: instead, there might be a mixture of chirality vectors codirected with the a or b axis, with the proportion altering with Ni concentration.
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