Synthesis of monodispersed magnetite nanoparticles from iron pivalate clusters

Khadijat Abdulwahab; Mohammad A. Malik; Paul O'Brien; Kuveshni Govender; Christopher A. Muryn; Grigore A. Timco; Floriana Tuna; Richard E P Winpenny

doi:10.1039/c2dt32478d

Synthesis of monodispersed magnetite nanoparticles from iron pivalate clusters

Khadijat Abdulwahab, Mohammad A. Malik, Paul O'Brien, Kuveshni Govender, Christopher A. Muryn, Grigore A. Timco, Floriana Tuna, Richard E P Winpenny

Research output: Contribution to journal › Article › peer-review

Abstract

The iron pivalate clusters [Fe3O(O2C tBu)6(H2O)3](O2C tBu)·HO2CtBu (1), [Fe 8(OH)4(O2CtBu)12(OC 6H4C6H5)8] (2) and [Fe3O(O2CtBu)6(C5H 5N)3] (3) have been used as single source precursors to synthesise iron oxide nanoparticles by a hot injection thermal decomposition method in oleylamine, hexadecanol, oleic acid, oleylamine/oleic acid with dodecanol or octyl ether as solvent. The effect of the different reaction parameters such as temperature, reaction time and capping agents on the phase and morphology were studied. The reaction time was studied for (1) by thermolysis in a mixture of oleylamine, oleic acid, hexadecanol and dodecanol (solvent) at 260 °C. The results obtained showed that a mixture of maghemite-C (Fe2O3) and magnetite (Fe3O 4) were obtained for aliquots withdrawn for reaction times of less than 30 minutes whilst only magnetite was obtained after one hour. The nanoparticles were characterised by p-XRD, TEM and magnetic measurements. TEM showed that monodispersed magnetite particles were obtained when the precursor was injected at the boiling point of the solvent. The diameter of the monodispersed nanoparticles obtained by the thermolysis of [Fe 3O(O2CtBu)6(H2O) 3](O2CtBu)·HO2C tBu (1) in oleylamine, hexadecanol, oleic acid with dodecanol or octyl ether as solvent were 4.3 ± 0.4 and 4.9 ± 0.5 nm respectively. Magnetic measurements revealed that all the particles are superparamagnetic. © The Royal Society of Chemistry 2013.

Original language	English
Pages (from-to)	196-206
Number of pages	10
Journal	Dalton Transactions
Volume	42
Issue number	1
DOIs	https://doi.org/10.1039/c2dt32478d
Publication status	Published - 7 Jan 2013

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10.1039/c2dt32478d

CCDC 882331: Experimental Crystal Structure Determination
Abdulwahab, K. (Contributor), Malik, M. (Contributor), O'Brien, P. (Contributor), Govender, K. (Contributor), Muryn, C. A. (Contributor), Timco, G. (Contributor), Tuna, F. (Contributor) & Winpenny, R. (Contributor), Cambridge Crystallographic Data Centre, 1 Jan 2013
DOI: 10.5517/ccym49z, http://www.ccdc.cam.ac.uk/services/structure_request?id=doi:10.5517/ccym49z&sid=DataCite
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@article{af1b3312a47549bab2ad274d7b8f1900,

title = "Synthesis of monodispersed magnetite nanoparticles from iron pivalate clusters",

abstract = "The iron pivalate clusters [Fe3O(O2C tBu)6(H2O)3](O2C tBu)·HO2CtBu (1), [Fe 8(OH)4(O2CtBu)12(OC 6H4C6H5)8] (2) and [Fe3O(O2CtBu)6(C5H 5N)3] (3) have been used as single source precursors to synthesise iron oxide nanoparticles by a hot injection thermal decomposition method in oleylamine, hexadecanol, oleic acid, oleylamine/oleic acid with dodecanol or octyl ether as solvent. The effect of the different reaction parameters such as temperature, reaction time and capping agents on the phase and morphology were studied. The reaction time was studied for (1) by thermolysis in a mixture of oleylamine, oleic acid, hexadecanol and dodecanol (solvent) at 260 °C. The results obtained showed that a mixture of maghemite-C (Fe2O3) and magnetite (Fe3O 4) were obtained for aliquots withdrawn for reaction times of less than 30 minutes whilst only magnetite was obtained after one hour. The nanoparticles were characterised by p-XRD, TEM and magnetic measurements. TEM showed that monodispersed magnetite particles were obtained when the precursor was injected at the boiling point of the solvent. The diameter of the monodispersed nanoparticles obtained by the thermolysis of [Fe 3O(O2CtBu)6(H2O) 3](O2CtBu)·HO2C tBu (1) in oleylamine, hexadecanol, oleic acid with dodecanol or octyl ether as solvent were 4.3 ± 0.4 and 4.9 ± 0.5 nm respectively. Magnetic measurements revealed that all the particles are superparamagnetic. {\textcopyright} The Royal Society of Chemistry 2013.",

author = "Khadijat Abdulwahab and Malik, {Mohammad A.} and Paul O'Brien and Kuveshni Govender and Muryn, {Christopher A.} and Timco, {Grigore A.} and Floriana Tuna and Winpenny, {Richard E P}",

year = "2013",

month = jan,

day = "7",

doi = "10.1039/c2dt32478d",

language = "English",

volume = "42",

pages = "196--206",

journal = "Dalton Transactions",

issn = "1477-9226",

publisher = "Royal Society of Chemistry",

number = "1",

}

TY - JOUR

T1 - Synthesis of monodispersed magnetite nanoparticles from iron pivalate clusters

AU - Abdulwahab, Khadijat

AU - Malik, Mohammad A.

AU - O'Brien, Paul

AU - Govender, Kuveshni

AU - Muryn, Christopher A.

AU - Timco, Grigore A.

AU - Tuna, Floriana

AU - Winpenny, Richard E P

PY - 2013/1/7

Y1 - 2013/1/7

N2 - The iron pivalate clusters [Fe3O(O2C tBu)6(H2O)3](O2C tBu)·HO2CtBu (1), [Fe 8(OH)4(O2CtBu)12(OC 6H4C6H5)8] (2) and [Fe3O(O2CtBu)6(C5H 5N)3] (3) have been used as single source precursors to synthesise iron oxide nanoparticles by a hot injection thermal decomposition method in oleylamine, hexadecanol, oleic acid, oleylamine/oleic acid with dodecanol or octyl ether as solvent. The effect of the different reaction parameters such as temperature, reaction time and capping agents on the phase and morphology were studied. The reaction time was studied for (1) by thermolysis in a mixture of oleylamine, oleic acid, hexadecanol and dodecanol (solvent) at 260 °C. The results obtained showed that a mixture of maghemite-C (Fe2O3) and magnetite (Fe3O 4) were obtained for aliquots withdrawn for reaction times of less than 30 minutes whilst only magnetite was obtained after one hour. The nanoparticles were characterised by p-XRD, TEM and magnetic measurements. TEM showed that monodispersed magnetite particles were obtained when the precursor was injected at the boiling point of the solvent. The diameter of the monodispersed nanoparticles obtained by the thermolysis of [Fe 3O(O2CtBu)6(H2O) 3](O2CtBu)·HO2C tBu (1) in oleylamine, hexadecanol, oleic acid with dodecanol or octyl ether as solvent were 4.3 ± 0.4 and 4.9 ± 0.5 nm respectively. Magnetic measurements revealed that all the particles are superparamagnetic. © The Royal Society of Chemistry 2013.

AB - The iron pivalate clusters [Fe3O(O2C tBu)6(H2O)3](O2C tBu)·HO2CtBu (1), [Fe 8(OH)4(O2CtBu)12(OC 6H4C6H5)8] (2) and [Fe3O(O2CtBu)6(C5H 5N)3] (3) have been used as single source precursors to synthesise iron oxide nanoparticles by a hot injection thermal decomposition method in oleylamine, hexadecanol, oleic acid, oleylamine/oleic acid with dodecanol or octyl ether as solvent. The effect of the different reaction parameters such as temperature, reaction time and capping agents on the phase and morphology were studied. The reaction time was studied for (1) by thermolysis in a mixture of oleylamine, oleic acid, hexadecanol and dodecanol (solvent) at 260 °C. The results obtained showed that a mixture of maghemite-C (Fe2O3) and magnetite (Fe3O 4) were obtained for aliquots withdrawn for reaction times of less than 30 minutes whilst only magnetite was obtained after one hour. The nanoparticles were characterised by p-XRD, TEM and magnetic measurements. TEM showed that monodispersed magnetite particles were obtained when the precursor was injected at the boiling point of the solvent. The diameter of the monodispersed nanoparticles obtained by the thermolysis of [Fe 3O(O2CtBu)6(H2O) 3](O2CtBu)·HO2C tBu (1) in oleylamine, hexadecanol, oleic acid with dodecanol or octyl ether as solvent were 4.3 ± 0.4 and 4.9 ± 0.5 nm respectively. Magnetic measurements revealed that all the particles are superparamagnetic. © The Royal Society of Chemistry 2013.

U2 - 10.1039/c2dt32478d

DO - 10.1039/c2dt32478d

M3 - Article

VL - 42

SP - 196

EP - 206

JO - Dalton Transactions

JF - Dalton Transactions

SN - 1477-9226

IS - 1

ER -

Synthesis of monodispersed magnetite nanoparticles from iron pivalate clusters

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CCDC 882331: Experimental Crystal Structure Determination

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