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Title: Synthesis and structure of synthetically pure and deuterated amorphous (basic) calcium carbonates

Abstract

It is generally believed that H2O and OH- are the key species stabilizing and controlling amorphous calcium carbonate “polyamorph” forms, and may in turn control the ultimate crystallization products during synthesis and in natural systems. Yet, the locations and hydrogen-bonding network of these species in ACC have never been measured directly using neutron diffraction. In this paper, we report a synthesis route that overcomes the existing challenges with respect to yield quantities and deuteration, both of which are critically necessary for high quality neutron studies.

Authors:
 [1];  [2];  [3];  [3];  [3];  [4];  [2];  [2];  [2];  [2]
  1. Univ. of Tennessee, Knoxville, TN (United States)
  2. Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States). Spallation Neutron Source
  3. Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States). Chemical Sciences Division
  4. Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States). Materials Science and Technology Division
Publication Date:
Research Org.:
Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States)
Sponsoring Org.:
USDOE Office of Science (SC), Basic Energy Sciences (BES)
OSTI Identifier:
1347339
Grant/Contract Number:  
AC05-00OR22725; AC02-06CH11357
Resource Type:
Accepted Manuscript
Journal Name:
ChemComm
Additional Journal Information:
Journal Volume: 53; Journal Issue: 20; Journal ID: ISSN 1359-7345
Publisher:
Royal Society of Chemistry
Country of Publication:
United States
Language:
English
Subject:
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY

Citation Formats

Wang, Hsiu-Wen, Daemen, Luke L., Cheshire, Michael C., Kidder, Michelle K., Stack, Andrew G., Allard, Lawrence F., Neuefeind, Jörg, Olds, Daniel, Liu, Jue, and Page, Katharine. Synthesis and structure of synthetically pure and deuterated amorphous (basic) calcium carbonates. United States: N. p., 2017. Web. doi:10.1039/C6CC08848A.
Wang, Hsiu-Wen, Daemen, Luke L., Cheshire, Michael C., Kidder, Michelle K., Stack, Andrew G., Allard, Lawrence F., Neuefeind, Jörg, Olds, Daniel, Liu, Jue, & Page, Katharine. Synthesis and structure of synthetically pure and deuterated amorphous (basic) calcium carbonates. United States. https://doi.org/10.1039/C6CC08848A
Wang, Hsiu-Wen, Daemen, Luke L., Cheshire, Michael C., Kidder, Michelle K., Stack, Andrew G., Allard, Lawrence F., Neuefeind, Jörg, Olds, Daniel, Liu, Jue, and Page, Katharine. Fri . "Synthesis and structure of synthetically pure and deuterated amorphous (basic) calcium carbonates". United States. https://doi.org/10.1039/C6CC08848A. https://www.osti.gov/servlets/purl/1347339.
@article{osti_1347339,
title = {Synthesis and structure of synthetically pure and deuterated amorphous (basic) calcium carbonates},
author = {Wang, Hsiu-Wen and Daemen, Luke L. and Cheshire, Michael C. and Kidder, Michelle K. and Stack, Andrew G. and Allard, Lawrence F. and Neuefeind, Jörg and Olds, Daniel and Liu, Jue and Page, Katharine},
abstractNote = {It is generally believed that H2O and OH- are the key species stabilizing and controlling amorphous calcium carbonate “polyamorph” forms, and may in turn control the ultimate crystallization products during synthesis and in natural systems. Yet, the locations and hydrogen-bonding network of these species in ACC have never been measured directly using neutron diffraction. In this paper, we report a synthesis route that overcomes the existing challenges with respect to yield quantities and deuteration, both of which are critically necessary for high quality neutron studies.},
doi = {10.1039/C6CC08848A},
journal = {ChemComm},
number = 20,
volume = 53,
place = {United States},
year = {Fri Feb 17 00:00:00 EST 2017},
month = {Fri Feb 17 00:00:00 EST 2017}
}

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Works referenced in this record:

Transformation and crystallization energetics of synthetic and biogenic amorphous calcium carbonate
journal, September 2010

  • Radha, A. V.; Forbes, T. Z.; Killian, C. E.
  • Proceedings of the National Academy of Sciences, Vol. 107, Issue 38
  • DOI: 10.1073/pnas.1009959107

Characterization of Structure in Biogenic Amorphous Calcium Carbonate: Pair Distribution Function and Nuclear Magnetic Resonance Studies of Lobster Gastrolith
journal, April 2013

  • Reeder, Richard J.; Tang, Yuanzhi; Schmidt, Millicent P.
  • Crystal Growth & Design, Vol. 13, Issue 5
  • DOI: 10.1021/cg301653s

Amorphous Calcium Carbonate: Synthesis and Potential Intermediate in Biomineralization
journal, June 2004


Stability and Structure of Hydrated Amorphous Calcium Carbonate
journal, October 2015

  • Bushuev, Yuriy G.; Finney, Aaron R.; Rodger, P. Mark
  • Crystal Growth & Design, Vol. 15, Issue 11
  • DOI: 10.1021/acs.cgd.5b00771

Taking Advantage of Disorder: Amorphous Calcium Carbonate and Its Roles in Biomineralization
journal, June 2003


Anisotropic thermal expansion and hydrogen bonding behavior of portlandite: A high-temperature neutron diffraction study
journal, April 2007


Binding of Ethanol on Calcite: The Role of the OH Bond and Its Relevance to Biomineralization
journal, October 2010

  • Sand, K. K.; Yang, M.; Makovicky, E.
  • Langmuir, Vol. 26, Issue 19
  • DOI: 10.1021/la101136j

Ethanol assisted synthesis of pure and stable amorphous calcium carbonate nanoparticles
journal, January 2013

  • Chen, Shao-Feng; Cölfen, Helmut; Antonietti, Markus
  • Chemical Communications, Vol. 49, Issue 83
  • DOI: 10.1039/c3cc45427d

Energetic and structural studies of amorphous Ca1−xMgxCO3·nH2O (0⩽x⩽1)
journal, August 2012

  • Radha, A. V.; Fernandez-Martinez, Alejandro; Hu, Yandi
  • Geochimica et Cosmochimica Acta, Vol. 90
  • DOI: 10.1016/j.gca.2012.04.056

Freeze-drying yields stable and pure amorphous calcium carbonate (ACC)
journal, January 2013

  • Ihli, Johannes; Kulak, Alexander N.; Meldrum, Fiona C.
  • Chemical Communications, Vol. 49, Issue 30
  • DOI: 10.1039/c3cc40807h

The Multiple Structures of Vaterite
journal, April 2013

  • Demichelis, Raffaella; Raiteri, Paolo; Gale, Julian D.
  • Crystal Growth & Design, Vol. 13, Issue 6
  • DOI: 10.1021/cg4002972

Pressure-Induced Polyamorphism and Formation of ‘Aragonitic’ Amorphous Calcium Carbonate
journal, July 2013

  • Fernandez-Martinez, Alejandro; Kalkan, Bora; Clark, Simon M.
  • Angewandte Chemie International Edition, Vol. 52, Issue 32
  • DOI: 10.1002/anie.201302974

Stable Prenucleation Calcium Carbonate Clusters
journal, December 2008


Microscopic Evidence for Liquid-Liquid Separation in Supersaturated CaCO3 Solutions
journal, August 2013


Viscosity of deuterium oxide and water in the range 5 to 125 C
journal, June 1949

  • Hardy, Robert C.; Cottington, Robert L.
  • Journal of Research of the National Bureau of Standards, Vol. 42, Issue 6
  • DOI: 10.6028/jres.042.049

In vitro Synthesis and Structural Characterization of Amorphous Calcium Carbonate
journal, October 2005

  • Günther, C.; Becker, A.; Wolf, G.
  • Zeitschrift für anorganische und allgemeine Chemie, Vol. 631, Issue 13-14
  • DOI: 10.1002/zaac.200500164

Synthesis of Amorphous Calcium Carbonate and Its Crystallization
journal, January 1993

  • Kojima, Yoshiyuki; Kawanobe, Akio; Yasue, Tamotsu
  • Journal of the Ceramic Society of Japan, Vol. 101, Issue 1178
  • DOI: 10.2109/jcersj.101.1145

How to make ‘stable’ ACC: protocol and preliminary structural characterization
journal, February 2008


Monohydrocalcite in Comparison with Hydrated Amorphous Calcium Carbonate: Precipitation Condition and Thermal Behavior
journal, September 2011

  • Kimura, Tomoyasu; Koga, Nobuyoshi
  • Crystal Growth & Design, Vol. 11, Issue 9
  • DOI: 10.1021/cg200412h

On the Structure of Amorphous Calcium CarbonateA Detailed Study by Solid-State NMR Spectroscopy
journal, September 2008

  • Nebel, Holger; Neumann, Markus; Mayer, Christian
  • Inorganic Chemistry, Vol. 47, Issue 17
  • DOI: 10.1021/ic8007409

Structural Changes upon Dehydration of Amorphous Calcium Carbonate
journal, January 2014

  • Schmidt, Millicent P.; Ilott, Andrew J.; Phillips, Brian L.
  • Crystal Growth & Design, Vol. 14, Issue 3
  • DOI: 10.1021/cg401073n

Nanoporous Structure and Medium-Range Order in Synthetic Amorphous Calcium Carbonate
journal, May 2010

  • Goodwin, Andrew L.; Michel, F. Marc; Phillips, Brian L.
  • Chemistry of Materials, Vol. 22, Issue 10
  • DOI: 10.1021/cm100294d

The roles of water and polyelectrolytes in the phase transformation of amorphous calcium carbonate
journal, August 2008


Proto-Calcite and Proto-Vaterite in Amorphous Calcium Carbonates
journal, October 2010

  • Gebauer, Denis; Gunawidjaja, Philips N.; Ko, J. Y. Peter
  • Angewandte Chemie International Edition, Vol. 49, Issue 47
  • DOI: 10.1002/anie.201003220

Dehydration-Induced Amorphous Phases of Calcium Carbonate
journal, March 2013

  • Saharay, Moumita; Yazaydin, A. Ozgur; Kirkpatrick, R. James
  • The Journal of Physical Chemistry B, Vol. 117, Issue 12
  • DOI: 10.1021/jp308353t

Synthesis of Vaterite by Carbonation Process in Aqueous System
journal, January 1996

  • Matsushita, Isao; Hamada, Yukitoshi; Moriga, Toshihiro
  • Journal of the Ceramic Society of Japan, Vol. 104, Issue 1215
  • DOI: 10.2109/jcersj.104.1081

Effect of pH on Amorphous Calcium Carbonate Structure and Transformation
journal, July 2016

  • Tobler, Dominique J.; Rodriguez Blanco, Juan Diego; Sørensen, Henning O.
  • Crystal Growth & Design, Vol. 16, Issue 8
  • DOI: 10.1021/acs.cgd.6b00630

THE ORTHORHOMBIC STRUCTURE OF CaCO3, SrCO3, PbCO3 AND BaCO3: LINEAR STRUCTURAL TRENDS
journal, October 2009


Stable prenucleation mineral clusters are liquid-like ionic polymers
journal, September 2011

  • Demichelis, Raffaella; Raiteri, Paolo; Gale, Julian D.
  • Nature Communications, Vol. 2, Issue 1
  • DOI: 10.1038/ncomms1604

Neutron and X-ray diffraction and empirical potential structure refinement modelling of magnesium stabilised amorphous calcium carbonate
journal, October 2014


Structure and Transformation of Amorphous Calcium Carbonate: A Solid-State 43 Ca NMR and Computational Molecular Dynamics Investigation
journal, May 2012

  • Singer, Jared Wesley; Yazaydin, A. Özgür; Kirkpatrick, R. James
  • Chemistry of Materials, Vol. 24, Issue 10
  • DOI: 10.1021/cm300389q

Microtwinning hypothesis for a more ordered vaterite model
journal, March 2011

  • Le Bail, A.; Ouhenia, S.; Chateigner, D.
  • Powder Diffraction, Vol. 26, Issue 1
  • DOI: 10.1154/1.3552994

Biomimetic Model Systems for Investigating the Amorphous Precursor Pathway and Its Role in Biomineralization
journal, November 2008


Disordered amorphous calcium carbonate from direct precipitation
journal, January 2015

  • Farhadi Khouzani, Masoud; Chevrier, Daniel M.; Güttlein, Patricia
  • CrystEngComm, Vol. 17, Issue 26
  • DOI: 10.1039/C5CE00720H

The role of pH and Mg on the stability and crystallization of amorphous calcium carbonate
journal, September 2012


Water Is the Key to Nonclassical Nucleation of Amorphous Calcium Carbonate
journal, December 2010

  • Raiteri, Paolo; Gale, Julian D.
  • Journal of the American Chemical Society, Vol. 132, Issue 49
  • DOI: 10.1021/ja108508k

Crystallization of amorphous calcium carbonate
journal, September 1998


Mechanistic Insights into the Crystallization of Amorphous Calcium Carbonate (ACC)
journal, May 2012

  • Bots, Pieter; Benning, Liane G.; Rodriguez-Blanco, Juan-Diego
  • Crystal Growth & Design, Vol. 12, Issue 7
  • DOI: 10.1021/cg300676b

Structural Characteristics of Synthetic Amorphous Calcium Carbonate
journal, July 2008

  • Michel, F. Marc; MacDonald, Jason; Feng, Jian
  • Chemistry of Materials, Vol. 20, Issue 14
  • DOI: 10.1021/cm800324v

Calcium Carbonate Polyamorphism and Its Role in Biomineralization: How Many Amorphous Calcium Carbonates Are There?
journal, November 2012

  • Cartwright, Julyan H. E.; Checa, Antonio G.; Gale, Julian D.
  • Angewandte Chemie International Edition, Vol. 51, Issue 48
  • DOI: 10.1002/anie.201203125

Synthesis-dependant structural variations in amorphous calcium carbonate
journal, January 2007

  • Lam, Raymond S. K.; Charnock, John M.; Lennie, Alistair
  • CrystEngComm, Vol. 9, Issue 12
  • DOI: 10.1039/b710895h

Works referencing / citing this record:

A high temperature gas flow environment for neutron total scattering studies of complex materials
journal, September 2018

  • Olds, Daniel; Mills, Rebecca A.; McDonnell, Marshall T.
  • Review of Scientific Instruments, Vol. 89, Issue 9
  • DOI: 10.1063/1.5033464

A suite-level review of the neutron powder diffraction instruments at Oak Ridge National Laboratory
journal, September 2018

  • Calder, S.; An, K.; Boehler, R.
  • Review of Scientific Instruments, Vol. 89, Issue 9
  • DOI: 10.1063/1.5033906

Advances in utilizing event based data structures for neutron scattering experiments
journal, September 2018

  • Peterson, Peter F.; Olds, Daniel; Savici, Andrei T.
  • Review of Scientific Instruments, Vol. 89, Issue 9
  • DOI: 10.1063/1.5034782

Selective Separation of MA(III) from Ln(III) by Highly Stable Silica-Polymer-based N-Donor Iso Bu-BTP/SiO 2 - P Adsorbent
journal, February 2019