Mechanistic Insights into the Crystallization of Amorphous Calcium Carbonate (ACC)
Abstract
Many organisms use amorphous calcium carbonate (ACC) during crystalline calcium carbonate biomineralization, as a means to control particle shape/size and phase stability. Here, we present an in situ small- and wide-angle X-ray scattering (SAXS/WAXS) study of the mechanisms and kinetics of ACC crystallization at rapid time scales (seconds). Combined with offline solid and solution characterization, we show that ACC crystallizes to vaterite via a three-stage process. First, hydrated and disordered ACC forms, then rapidly transforms to more ordered and dehydrated ACC; in conjunction with this, vaterite forms via a spherulitic growth mechanism. Second, when the supersaturation of the solution with respect to vaterite decreases sufficiently, the mechanism changes to ACC dissolution and vaterite crystal growth. The third stage is controlled by Ostwald ripening of the vaterite particles. Combining this information with previous studies, allowed us to develop a mechanistic understanding of the abiotic crystallization process from ACC to vaterite and all the way to calcite. We propose this is the underlying abiotic mechanism for calcium carbonate biomineralization from ACC. This process is then augmented or altered by organisms (e.g., using organic compounds) to form intricate biominerals. This study also highlights the applicability of in situ time-resolved SAXS/WAXS to study rapid crystallization reactions.
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Magnesium-free ACC crystallizes rapidly to vaterite via spherulitic growth, followed by slower transformation of vaterite to calcite via dissolution and re-precipitation.
“Magnesium-free ACC crystallizes rapidly to vaterite via spherulitic growth (Bots et al. 2012), followed by the slower transformation of vaterite to calcite via dissolution and re-precipitation (Rodriguez-Blanco et al. 2011).”
From A route for the direct crystallization of dolomite (2015) · cites this paper as Bots et al. 2012
In the carbonate system, amorphous ACC precursor transforms to vaterite via spherulitic growth at high supersaturations and leads to spheroidal vaterite aggregates.
“For the carbonate system it has been demonstrated that the amorphous ACC precursor transforms to vaterite via spherulitic growth (Beck and Andreassen 2010; Andreassen et al. 2010; Bots et al. 2012), and that this reaction occurs at high superaturations and leads to spheroidal vaterite aggregates.”
From A route for the direct crystallization of dolomite (2015) · cites this paper as Bots et al. 2012
The morphology (spherical) and size (44 ± 13 nm) of the starting Mg-ACC were similar to that reported for ACC.
“The morphology (spherical) and size (44 ± 13 nm) of our starting Mg-ACC were also similar to that reported for ACC (e.g., Radha et al. 2010, sample ACC-5, Ø 50-100 nm; Bots et al. 2012, ACC, Ø ~ 40 nm).”
From A route for the direct crystallization of dolomite (2015) · cites this paper as Bots et al. 2012
This is akin to behavior observed for pure ACC where prior to crystallization an increase in ordering of the amorphous phase was likely accompanied by a lowering in water content and a final transformation to a fully anhydrous amorphous phase.
“This is akin to the behavior observed for pure ACC (Radha et al. 2010; Bots et al. 2012) where prior to crystallization an increase in ordering of the amorphous phase was also likely accompanied by a lowering in water content and a final transformation to a fully anhydrous amorphous phase.”
From A route for the direct crystallization of dolomite (2015) · cites this paper as Bots et al. 2012
The ordering and partial dehydration of Mg-ACC prior to crystallization likely occurs via a mechanism similar to that observed for pure ACC.
“We have shown that the initially hydrated and highly disordered Mg-ACC forms from solution and we suggest that this Mg-ACC gradually orders and may partially dehydrate prior to its crystallization, and that this likely occurs via a similar mechanism to that observed for pure ACC (Bots et al. 2012).”
From A route for the direct crystallization of dolomite (2015) · cites this paper as Bots et al. 2012
Studies of both inorganic and biogenic ACC have shown that an initial hydrated and highly disordered ACC forms from solution and transforms to a less disordered and anhydrous ACC prior to crystallization.
“Studies of both inorganic and biogenic ACC have shown that an initial hydrated and highly disordered ACC (i.e., ACC with low-structural order) forms from solution and that this transforms to a less disordered and anhydrous ACC prior to crystallization (Gower 2008; Bots et al. 2012).”
From A route for the direct crystallization of dolomite (2015) · cites this paper as Bots et al. 2012
In the absence of magnesium, ACC transforms to vaterite via spherulitic growth and subsequently ripens and re-crystallizes to calcite.
“In the absence of magnesium, ACC transforms to vaterite via spherulitic growth and this subsequently ripens and re-crystallizes to calcite (Bots et al. 2012; Rodriguez-Blanco et al. 2011).”
From A route for the direct crystallization of dolomite (2015) · cites this paper as Bots et al. 2012
Pure ACC to vaterite transformation occurs via spherulitic growth, and the SI for vaterite was usually equal to or larger than 3.
“For example, in the case of the pure ACC to vaterite transformation that occurs also via spherulitic growth (Beck and Andreassen 2010; Andreassen et al. 2010; Bots et al. 2012) the SI for vaterite was usually equal or larger than 3.”
From A route for the direct crystallization of dolomite (2015) · cites this paper as Bots et al. 2012
This spherulitic growth pathway has so far been documented for crystallization of pure ACC, for a 30% Mg-ACC precursor to monohydrocalcite, and in this study where initial solutions contained 50% Mg.
“This spherulitic growth pathway has so far been documented for the crystallization of pure ACC (Andreassen 2005; Bots et al. 2012; Rodriguez-Blanco et al. 2011; Sand et al. 2012), for a 30% Mg-ACC precursor to monohydrocalcite (Rodriguez-Blanco et al. 2014) as well as in this study where the initial solutions contained 50% Mg.”
From A route for the direct crystallization of dolomite (2015) · cites this paper as Bots et al. 2012
These particle sizes are comparable with the crystallite size for vaterite also formed via spherulitic growth (~10 nm).
“These particle sizes are comparable with the crystallite size for vaterite also formed via spherulitic growth ( ~ 10 nm, Bots et al. 2012).”
From A route for the direct crystallization of dolomite (2015) · cites this paper as Bots et al. 2012
In bacterially mediated reactions, SI values of 3.36 were reported, comparable to those reported here and by others for spherulitic growth carbonate systems.
“Similarly, in bacterially mediated reactions, SI values of 3.36 were reported (Kenward et al. 2009) which are comparable to those reported here and by others for spherulitic growth carbonate systems (Andreassen 2005; Bots et al. 2012).”
From A route for the direct crystallization of dolomite (2015) · cites this paper as Bots et al. 2012
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- Authors
- Bots, P., Benning, L. G., Rodriguez-Blanco, J.-D., Roncal-Herrero, T., & Shaw, S.
- Affiliations
- University of Leeds (GB)
- Earth Surface Science Institute, School of Earth and Environment, University of Leeds, Leeds LS2 9JT, U.K.
- Corresponding author
- Shaw, Samuel
- Venue
- Crystal Growth & Design
- Publisher
- American Chemical Society (ACS)
- Published
- 2012-05-31
- Volume
- 12
- Issue
- 7
- Pages
- 3806-3814
- ISSN
- 1528-7483 (ISSN-L)
- 1528-7505
- OpenAlex
- W2094082807
- Cited by
- 474
- References
- 55
- Citations by year
- 2026: 47 · 2025: 55 · 2024: 40 · 2023: 44 · 2022: 49 · 2021: 40 · 2020: 34 · 2019: 24 · 2018: 34 · 2017: 30 · 2016: 17 · 2015: 22 · 2014: 23 · 2013: 14 · 2012: 1
- FWCI
- 7.78
- Type
- journal article
- Language
- en
- Open access
- closed
- Locations
- Crystal Growth & Design (publishedVersion)
- Publication Database GFZ (GFZ German Research Centre for Geosciences) (submittedVersion)
- Research Explorer (The University of Manchester) (submittedVersion)
- Topics
- Physical Sciences › Materials Science › Biomaterials › Calcium Carbonate Crystallization and Inhibition
- Physical Sciences › Materials Science › Materials Chemistry › Crystallization and Solubility Studies
- Physical Sciences › Environmental Science › Environmental Engineering › Microbial Applications in Construction Materials
- Keywords
- amorphous calcium carbonate, calcium carbonate crystallization, vaterite, calcite, biomineralization, spherulite growth, Ostwald ripening, crystallization kinetics, phase transformation
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