Influence of aging in an alkaline medium on the microstructural properties of α-FeOOH

The influence of the aging in a highly alkaline medium at 160 °C on the microstructural properties of α-FeOOH was monitored by XRD, 57Fe Mössbauer and FT-IR spectroscopies and FE-SEM. In the synthesis of acicular and monodisperse α-FeOOH particles, tetramethylammonium hydroxide was used as a precipi...

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Published in	Journal of crystal growth Vol. 310; no. 2; pp. 513 - 520
Main Authors	Krehula, S., Musić, S.
Format	Journal Article
Language	English
Published	Amsterdam Elsevier B.V 15.01.2008 Elsevier
Subjects	A1. Crystal morphology A2. Hydrothermal crystal growth B1. Goethite Cross-disciplinary physics: materials science; rheology Exact sciences and technology Growth from solutions Materials science Methods of crystal growth; physics of crystal growth Physics Theory and models of crystal growth; physics of crystal growth, crystal morphology and orientation 81.05.Je 82.80.Ej 82.80.Gk B1. Goethite A1. Crystal morphology 81.10.Dn A2. Hydrothermal crystal growth Crystal growth 81.05.Je; 81.10.Dn; 82.80.Ej; 82.80.Gk Scanning electron microscopy A1. Crystal morphology; A2. Hydrothermal crystal growth; B1. Goethite Fourier transform spectroscopy Thermal ageing XRD Hydrothermal growth Crystallites Iron hydroxide Iron compounds Growth mechanism Microstructure Crystal morphology Goethite
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Abstract	The influence of the aging in a highly alkaline medium at 160 °C on the microstructural properties of α-FeOOH was monitored by XRD, 57Fe Mössbauer and FT-IR spectroscopies and FE-SEM. In the synthesis of acicular and monodisperse α-FeOOH particles, tetramethylammonium hydroxide was used as a precipitating agent. The crystal growth of α-FeOOH by the mechanism of lateral arraying was observed with prolonged aging time. Smaller α-FeOOH particles were dissolving with time, thus providing Fe ( OH ) 4 - ions for the additional growth of α-FeOOH particles and improvement of their crystal shape. The XRD analysis confirmed that the growth of α-FeOOH crystallites perpendicularly to the crystallographic c-axis was favoured. The Mössbauer spectrum of α-FeOOH showed a distribution of the hyperfine magnetic field (HMF) which gradually narrowed with a longer aging time. The average value of the HMF distribution was shifted from 35.3 to 37.1 T between 2 and 168 h of aging. Characteristic IR bands of α-FeOOH were sensitive to the microstructural changes of α-FeOOH particles during their aging in the suspension in a highly alkaline medium at 160 °C.
AbstractList	The influence of the aging in a highly alkaline medium at 160 °C on the microstructural properties of α-FeOOH was monitored by XRD, 57Fe Mössbauer and FT-IR spectroscopies and FE-SEM. In the synthesis of acicular and monodisperse α-FeOOH particles, tetramethylammonium hydroxide was used as a precipitating agent. The crystal growth of α-FeOOH by the mechanism of lateral arraying was observed with prolonged aging time. Smaller α-FeOOH particles were dissolving with time, thus providing Fe ( OH ) 4 - ions for the additional growth of α-FeOOH particles and improvement of their crystal shape. The XRD analysis confirmed that the growth of α-FeOOH crystallites perpendicularly to the crystallographic c-axis was favoured. The Mössbauer spectrum of α-FeOOH showed a distribution of the hyperfine magnetic field (HMF) which gradually narrowed with a longer aging time. The average value of the HMF distribution was shifted from 35.3 to 37.1 T between 2 and 168 h of aging. Characteristic IR bands of α-FeOOH were sensitive to the microstructural changes of α-FeOOH particles during their aging in the suspension in a highly alkaline medium at 160 °C. The influence of the aging in a highly alkaline medium at 160 deg C on the microstructural properties of alpha-FeOOH was monitored by XRD, 57Fe Mossbauer and FT-IR spectroscopies and FE-SEM. In the synthesis of acicular and monodisperse alpha-FeOOH particles, tetramethylammonium hydroxide was used as a precipitating agent. The crystal growth of alpha-FeOOH by the mechanism of lateral arraying was observed with prolonged aging time. Smaller alpha-FeOOH particles were dissolving with time, thus providing ions for the additional growth of alpha-FeOOH particles and improvement of their crystal shape. The XRD analysis confirmed that the growth of alpha-FeOOH crystallites perpendicularly to the crystallographic c-axis was favoured. The Mossbauer spectrum of alpha-FeOOH showed a distribution of the hyperfine magnetic field (HMF) which gradually narrowed with a longer aging time. The average value of the HMF distribution was shifted from 35.3 to 37.1T between 2 and 168h of aging. Characteristic IR bands of alpha-FeOOH were sensitive to the microstructural changes of alpha-FeOOH particles during their aging in the suspension in a highly alkaline medium at 160 deg C.
Author	Krehula, S. Musić, S.
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Keywords	81.05.Je 82.80.Ej 82.80.Gk B1. Goethite A1. Crystal morphology 81.10.Dn A2. Hydrothermal crystal growth Crystal growth 81.05.Je; 81.10.Dn; 82.80.Ej; 82.80.Gk Scanning electron microscopy A1. Crystal morphology; A2. Hydrothermal crystal growth; B1. Goethite Fourier transform spectroscopy Thermal ageing XRD Hydrothermal growth Crystallites Iron hydroxide Iron compounds Growth mechanism Microstructure Crystal morphology Goethite
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Snippet	The influence of the aging in a highly alkaline medium at 160 °C on the microstructural properties of α-FeOOH was monitored by XRD, 57Fe Mössbauer and FT-IR... The influence of the aging in a highly alkaline medium at 160 deg C on the microstructural properties of alpha-FeOOH was monitored by XRD, 57Fe Mossbauer and...
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SubjectTerms	A1. Crystal morphology A2. Hydrothermal crystal growth B1. Goethite Cross-disciplinary physics: materials science; rheology Exact sciences and technology Growth from solutions Materials science Methods of crystal growth; physics of crystal growth Physics Theory and models of crystal growth; physics of crystal growth, crystal morphology and orientation
Title	Influence of aging in an alkaline medium on the microstructural properties of α-FeOOH
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