Issue 16, 2003
From the journal:

Dalton Transactions

In-situX-ray powder diffraction studies of hydrothermal and thermal decomposition reactions of basic bismuth(iii) nitrates in the temperature range 20–650 °C†

Axel Nørlund Christensen,a   Torben René Jensen,b   Nicola V. Y. Scarlett,c   Ian C. Madsen,c   Jonathan C. Hansond  and  Angela Altomaree  

a Højkolvej 7, DK-8210 Aarhus V, Denmark

b Department of Inorganic Chemistry, University of Aarhus, DK-8000 Aarhus C, Denmark

c CSIRO Minerals, Clayton South, Victoria 3169, Australia

d Chemistry Department, Brookhaven National Laboratory, Upton, NY 11973, USA

e CNR ISMEC c/o Dipartimento Geomineralogico, Via Orabona 4, I-70125 Bari, Italy

Abstract

The syntheses of basic bismuth(III) nitrates under hydrothermal conditions and their dry decomposition to α-Bi2O3 in solid-state reactions was investigated by in-situ synchrotron X-ray radiation powder diffraction. Three basic bismuth(III) nitrates with known structures are: [Bi6O4(OH)4](NO3)6·4H2O, C, [Bi6O4(OH)4](NO3)6·H2O, D, and [Bi6O5(OH)3](NO3)5·3H2O, A. They contain the complex ions [Bi6O4(OH)4]6+ and{[Bi6O5(OH)3]5+}2, respectively. A fourth basic bismuth(III) nitrate, X, apparently has the composition [Bi6O4.5(OH)3.5](NO3)5.5·H2O according to chemical analysis. The transformation of C via D to X, or of C directly to X was established in the in-situ hydrothermal synthesis. Similarities in the decomposition paths of C, D and X in the solid-state in-situ investigations support the above composition indicated for X. The compound A has a decomposition path different from those of C, D and X. This is consistent with the complex ion {[Bi6O5(OH)3]5+}2 in A, being different from the complex ion [Bi6O4(OH)4]6+ in the other two basic bismuth(III) nitrates. All four compounds have α-Bi2O3 as the final decomposition product.

Graphical abstract: In-situ X-ray powder diffraction studies of hydrothermal and thermal decomposition reactions of basic bismuth(iii) nitrates in the temperature range 20–650 °C

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Article information

DOI
https://doi.org/10.1039/B303926A
Article type
Paper
Submitted
08 Apr 2003
Accepted
18 Jun 2003
First published
07 Jul 2003

Dalton Trans., 2003, 3278-3282

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In-situ X-ray powder diffraction studies of hydrothermal and thermal decomposition reactions of basic bismuth(III) nitrates in the temperature range 20–650 °C

A. N. Christensen, T. R. Jensen, N. V. Y. Scarlett, I. C. Madsen, J. C. Hanson and A. Altomare, Dalton Trans., 2003, 3278 DOI: 10.1039/B303926A

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