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Title: Nano size crystals of goethite, {alpha}-FeOOH: Synthesis and thermal transformation

Abstract

An aqueous suspension of amorphous iron(III) hydroxide was kept at room temperature (298 K) for 23 years. During this period of time the pH of the liquid phase changed from 4.3 to 2.85, and nano size crystals of goethite, {alpha}-FeOOH crystallised from the amorphous iron(III) hydroxide. Transmission electron microscopy (TEM) investigations, Moessbauer spectra, and powder X-ray diffraction using Co K{alpha} radiation showed that the only iron containing crystalline phase present in the recovered product was {alpha}-FeOOH. The size of these nano particles range from 10 to 100 nm measured by TEM. The thermal decomposition of {alpha}-FeOOH was investigated by time-resolved in situ synchrotron radiation powder X-ray diffraction and the data showed that the sample of {alpha}-FeOOH transformed to {alpha}-Fe{sub 2}O{sub 3} in the temperature range 444-584 K. A quantitative phase analysis shows the increase in scattered X-ray intensity from {alpha}-Fe{sub 2}O{sub 3} to follow the decrease of intensity from {alpha}-FeOOH in agreement with the topotactic phase transition. - Graphical abstract: Nano size crystals of goethite, {alpha}-FeOOH formed from amorphous iron(III) hydroxide after 23 years, and transforms faster to {alpha}-Fe{sub 2}O{sub 3} upon heating.

Authors:
 [1];  [2];  [3];  [4]
  1. Crystal Chemistry, Hojkolvej 7, DK-8210 Arhus V (Denmark)
  2. Interdisciplinary Nanoscience Centre (iNANO), Department of Chemistry, University of Aarhus, DK-8000 Arhus C (Denmark), E-mail: trj@chem.au.dk
  3. Materials Research Department, Riso National Laboratory, P.O. Box 49, DK-4000 Roskilde (Denmark)
  4. National Synchrotron Light Source Department, Brookhaven National Laboratory, Upton, NY 11973 (United States)
Publication Date:
OSTI Identifier:
21015793
Resource Type:
Journal Article
Resource Relation:
Journal Name: Journal of Solid State Chemistry; Journal Volume: 180; Journal Issue: 4; Other Information: DOI: 10.1016/j.jssc.2007.01.032; PII: S0022-4596(07)00064-3; Copyright (c) 2007 Elsevier Science B.V., Amsterdam, The Netherlands, All rights reserved; Country of input: International Atomic Energy Agency (IAEA)
Country of Publication:
United States
Language:
English
Subject:
37 INORGANIC, ORGANIC, PHYSICAL AND ANALYTICAL CHEMISTRY; GOETHITE; IRON HYDROXIDES; IRON OXIDES; MOESSBAUER EFFECT; PHASE STUDIES; PHASE TRANSFORMATIONS; SYNCHROTRON RADIATION; SYNTHESIS; TEMPERATURE RANGE 0273-0400 K; TRANSMISSION ELECTRON MICROSCOPY; X-RAY DIFFRACTION

Citation Formats

Christensen, Axel Norlund, Jensen, Torben R., Bahl, Christian R.H., and DiMasi, Elaine. Nano size crystals of goethite, {alpha}-FeOOH: Synthesis and thermal transformation. United States: N. p., 2007. Web. doi:10.1016/j.jssc.2007.01.032.
Christensen, Axel Norlund, Jensen, Torben R., Bahl, Christian R.H., & DiMasi, Elaine. Nano size crystals of goethite, {alpha}-FeOOH: Synthesis and thermal transformation. United States. doi:10.1016/j.jssc.2007.01.032.
Christensen, Axel Norlund, Jensen, Torben R., Bahl, Christian R.H., and DiMasi, Elaine. Sun . "Nano size crystals of goethite, {alpha}-FeOOH: Synthesis and thermal transformation". United States. doi:10.1016/j.jssc.2007.01.032.
@article{osti_21015793,
title = {Nano size crystals of goethite, {alpha}-FeOOH: Synthesis and thermal transformation},
author = {Christensen, Axel Norlund and Jensen, Torben R. and Bahl, Christian R.H. and DiMasi, Elaine},
abstractNote = {An aqueous suspension of amorphous iron(III) hydroxide was kept at room temperature (298 K) for 23 years. During this period of time the pH of the liquid phase changed from 4.3 to 2.85, and nano size crystals of goethite, {alpha}-FeOOH crystallised from the amorphous iron(III) hydroxide. Transmission electron microscopy (TEM) investigations, Moessbauer spectra, and powder X-ray diffraction using Co K{alpha} radiation showed that the only iron containing crystalline phase present in the recovered product was {alpha}-FeOOH. The size of these nano particles range from 10 to 100 nm measured by TEM. The thermal decomposition of {alpha}-FeOOH was investigated by time-resolved in situ synchrotron radiation powder X-ray diffraction and the data showed that the sample of {alpha}-FeOOH transformed to {alpha}-Fe{sub 2}O{sub 3} in the temperature range 444-584 K. A quantitative phase analysis shows the increase in scattered X-ray intensity from {alpha}-Fe{sub 2}O{sub 3} to follow the decrease of intensity from {alpha}-FeOOH in agreement with the topotactic phase transition. - Graphical abstract: Nano size crystals of goethite, {alpha}-FeOOH formed from amorphous iron(III) hydroxide after 23 years, and transforms faster to {alpha}-Fe{sub 2}O{sub 3} upon heating.},
doi = {10.1016/j.jssc.2007.01.032},
journal = {Journal of Solid State Chemistry},
number = 4,
volume = 180,
place = {United States},
year = {Sun Apr 15 00:00:00 EDT 2007},
month = {Sun Apr 15 00:00:00 EDT 2007}
}