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Stacking sequence variations in vaterite resolved by precession electron diffraction tomography using a unified

Gwladys Steciuk1, Lukáš Palatinus2, Jan Rohlíček2

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Vaterite, a key phase in biomineralization, has its structure fully determined using precession electron diffraction tomography. This reveals temperature-dependent stacking sequences crucial for understanding carbonate formation.

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Area of Science:

  • Crystallography and Materials Science
  • Geochemistry and Mineralogy
  • Biomineralization and Biogeochemistry

Background:

  • Vaterite is a metastable calcium carbonate polymorph, crucial in initial crystallization steps for calcite and aragonite.
  • Understanding vaterite's complete structure is vital for unraveling scaling formation and biomineralization processes.
  • Previous studies identified vaterite's hexagonal substructure but lacked clarity on its stacking sequence.

Purpose of the Study:

  • To resolve ambiguities in vaterite's crystal structure, particularly its stacking sequence.
  • To provide a complete structural determination of vaterite across a temperature range.
  • To elucidate the role of temperature in vaterite's structural modulation and stacking.

Main Methods:

  • Precession electron diffraction tomography (PEDT) was employed to gather single-crystal data from 100 K to ambient temperature.
  • Ab initio structure solution was performed, utilizing a unified modulated structure model in superspace group C12/c1(α0γ)00.
  • The model was refined against PEDT data (including modulation and twinning) and X-ray powder diffraction data (Rietveld refinement).

Main Results:

  • A complete, temperature-dependent structural model for vaterite was established.
  • At 100 K, vaterite exhibits a pure 4-layer stacking sequence (γ = 1/2).
  • At ambient temperature, ordered stacking faults emerge, altering the sequence (γ < 1/2).

Conclusions:

  • The study provides the first complete structural determination of vaterite, resolving previous ambiguities.
  • Temperature-induced changes in stacking sequences are identified, impacting vaterite's stability and transformation.
  • The findings offer critical insights into the structural mechanisms governing carbonate formation, biomineralization, and scaling.