Tracking 2D-to-3D crystal growth of a layered material in situ with X-ray scattering

Abstract

The dimensionality of a layered material, i.e. the number of 2D layers bound together, is a structural property underpinning the functional properties of the material. Uncovering synthetic methodologies for controlling dimensionality is therefore crucial for enabling the targeted design of high-functioning materials. This in situ X-ray total scattering study demonstrates the crystal growth of anisotropic Bi24O31Br10, a layered material increasingly utilised for its promising photocatalytic properties. Interlayer and intralayer crystal growth were facilitated by calcining Bi24O31Br10 over the temperature range of 30–600 °C. Analyses of the scattering data were conducted in reciprocal space and real space, combining model-free, model-based, and simulation-based analyses, with all conferring that the Bi24O31Br10 sample exhibits low dimensionality at lower temperatures, which gradually transitions to higher dimensionality as the calcination temperature increases. The inevitable thermal effects brought on by conducting measurements at elevated temperatures were analysed using the Python package, diffpy.morph, facilitating insight into the extent of thermal expansion and vibration throughout the data series, which in turn facilitated a focused analysis of crystal growth in an anisotropic nanomaterial. This study provides novel insight into structural analyses of 2D-to-3D transitions in anisotropic nanomaterials via X-ray scattering, and contributes significantly to the structural understanding of an emerging functional layered material.

Graphical abstract: Tracking 2D-to-3D crystal growth of a layered material in situ with X-ray scattering

Supplementary files

Article information

Article type
Paper
Submitted
10 Feb 2025
Accepted
17 Jun 2025
First published
19 Jun 2025

Nanoscale, 2025, Advance Article

Tracking 2D-to-3D crystal growth of a layered material in situ with X-ray scattering

M. J. Marks, S. Frank, M. L. Henriksen, H. S. Jeppesen and N. Lock, Nanoscale, 2025, Advance Article , DOI: 10.1039/D5NR00594A

To request permission to reproduce material from this article, please go to the Copyright Clearance Center request page.

If you are an author contributing to an RSC publication, you do not need to request permission provided correct acknowledgement is given.

If you are the author of this article, you do not need to request permission to reproduce figures and diagrams provided correct acknowledgement is given. If you want to reproduce the whole article in a third-party publication (excluding your thesis/dissertation for which permission is not required) please go to the Copyright Clearance Center request page.

Read more about how to correctly acknowledge RSC content.

Social activity

Spotlight

Advertisements