Volume 33
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Singh, J. P., Ji, M.-J., Shim, C.-H., Kim, S. O., & Chae, K. H. (2017). Effect of precursor thermal history on the formation of amorphous and crystalline calcium carbonate. Particuology, 33, 29-34. https://doi.org/10.1016/j.partic.2016.10.003
Effect of precursor thermal history on the formation of amorphous and crystalline calcium carbonate
Jitendra Pal Singh a *, Mi-Jung Ji a, Cheol-Hwee Shim a, Sang Ok Kim b, Keun Hwa Chae a *
a Advanced Analysis Center, Korea Institute of Science and Technology, Seoul 02792, Republic of Korea
b Department of Biomedical Engineering, Seonam University, Namwon 55724, Republic of Korea
10.1016/j.partic.2016.10.003
Volume 33, August 2017, Pages 29-34
Received 29 July 2016, Revised 27 September 2016, Accepted 10 October 2016, Available online 28 February 2017, Version of Record 13 June 2017.
E-mail: jitendra_singh2029@rediffmail.com; email_jps@yahoo.co.in; khchae@kist.re.kr

Highlights

• Amorphous and crystalline phases of calcium carbonate were synthesized from calcium nitrate.

• The amorphous or crystalline phases were unaffected by the thermal history of the precursor.

• Electronic structure was sensitive to precursor thermal history and annealing.


Abstract

The role of the thermal history of the precursor was studied for amorphous and crystalline calcium carbonate phases synthesized from calcium nitrate. The X-ray diffraction patterns of these phases are influenced by their annealing temperature of 0, 300, 400, and 500 °C. However, the effect of the precursor thermal history on the X-ray diffraction pattern of the resulting calcium carbonate phase is negligible. Transmission electron microscopy indicates that materials annealed at 400 °C consist of amorphous aggregates, irrespective of the precursor thermal history. The crystallite size of crystalline calcium carbonate is influenced by the precursor thermal history, and ranges from 23 to 26 nm. Near-edge X-ray absorption fine structure measurements indicate that the annealing temperature plays an important role in determining the local electronic structure. The role of the thermal history of the precursor is also important for the resulting electronic structure.

Graphical abstract
Keywords
Amorphous material; Particles; Electron microscopy; X-ray techniques; NEXAFS; Calcium carbonate