Role of Water During Crystallization of Amorphous Cobalt Phosphate Nanoparticles

Bach, Sven; Panthöfer, Martin; Bienert, Ralf; Buzanich, Ana de Oliveira Guilherme; Emmerling, Franziska; Tremel, Wolfgang

doi:10.1021/acs.cgd.6b00208

Title: Role of Water During Crystallization of Amorphous Cobalt Phosphate Nanoparticles

Journal Article · Mon Jun 27 00:00:00 EDT 2016 · Crystal Growth and Design

DOI:https://doi.org/10.1021/acs.cgd.6b00208· OSTI ID:1324797

Bach, Sven ^[1]; Panthöfer, Martin ^[2]; Bienert, Ralf ^[3]; Buzanich, Ana de Oliveira Guilherme ^[3]; Emmerling, Franziska ^[3]; Tremel, Wolfgang ^[2]

Johannes Gutenberg Univ. Mainz (Germany); Graduate School Materials Science in Mainz (Germany)
Johannes Gutenberg Univ. Mainz (Germany)
Federal Inst. for Materials Research and Testing, Berlin (Germany)

The transformation of amorphous precursors into crystalline solids and the associated mechanisms are still poorly understood. We illuminate the formation and reactivity of an amorphous cobalt phosphate hydrate precursor and the role of water for its crystallization process. Amorphous cobalt phosphate hydrate nanoparticles (ACP) with diameters of ~20 nm were prepared in the absence of additives from aqueous solutions at low concentrations and with short reaction times. To avoid the kinetically controlled transformation of metastable ACP into crystalline Co₃(PO₄)₂ × 8 H₂O (CPO) its separation must be fast. The crystallinity of ACP could be controlled through the temperature during precipitation. A second amorphous phase (HT-ACP) containing less water and anhydrous Co₃(PO₄)₂ was formed at higher temperature by the release of coordinating water. ACP contains approximately five molecules of structural water per formula unit as determined by thermal analysis (TGA) and quantitative IR spectroscopy. The Co²⁺ coordination in ACP is tetrahedral, as shown by XANES/EXAFS spectroscopy, but octahedral in crystalline CPO. ACP is stable in the absence of water even at 500 °C. In the wet state, the transformation of ACP to CPO is triggered by the diffusion and incorporation of water into the structure. Lastly, quantitative in situ IR analysis allowed monitoring the crystallization kinetics of ACP in the presence of water.

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Research Organization:: Argonne National Laboratory (ANL), Argonne, IL (United States)

Sponsoring Organization:: USDOE Office of Science (SC), Basic Energy Sciences (BES)

Grant/Contract Number:: AC02-06CH11357

OSTI ID:: 1324797

Journal Information:: Crystal Growth and Design, Vol. 16, Issue 8; ISSN 1528-7483

Publisher:: American Chemical SocietyCopyright Statement

Country of Publication:: United States

Language:: ENGLISH

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Cited by: 15 works

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37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY
crystallization
nanoparticles
phosphates
cobalt
water
cobalt phosphate
amorphous

Title: Role of Water During Crystallization of Amorphous Cobalt Phosphate Nanoparticles

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