Hot injection thermolysis of heterometallic pivalate clusters for the synthesis of monodisperse zinc and nickel ferrite nanoparticles

Abdulwahab, Khadijat O.; Malik, Mohammad Azad; O’Brien, Paul; Timco, Grigore A.; Tuna, Floriana; Winpenny, Richard E. P.; Pattrick, R. A. D.; Coker, Victoria S.; Arenholz, Elke

doi:10.1039/c4tc00832d

Cited by 14 publications

(10 citation statements)

References 55 publications

(64 reference statements)

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“…Various synthetic methods have been reported to produce M 3 NPs, which include nonaqueous and aqueous sol-gel, microemulsion, sonochemical, and the most popular hydrothermal/solvothermal techniques [3]. Of the many available approaches, two main synthetic solutionbased routes [4] have been popularized: (a) basic aqueous coprecipitation [5] of iron salts (as demonstrated by Massart) in the presence or absence of surfactants/polymers [6], (b) high-temperature thermal decomposition [7] of organometallic precursors (Fe(acac) 3 [8], Fe-oleate [9], Fe-carboxylate [10], Fe-pivalate [11], or heterodoped ferrite pivalate [12,13]) in high-boiling solvents at elevated temperatures (∼200-360 ∘ C). Despite the popularity of the conventional basic coprecipitation method, there remain difficulties in achieving size-controlled, narrowly dispersed, and reproducible nanocrystalline particles [1,3,4].…”

Section: Introductionmentioning

confidence: 99%

Ultra‐Small Fatty Acid‐Stabilized Magnetite Nanocolloids Synthesized by In Situ Hydrolytic Precipitation

El‐Boubbou

Al‐Kaysi

Al-Muhanna

et al. 2015

Journal of Nanomaterials

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Simple, fast, large-scale, and cost-effective preparation of uniform controlled magnetic nanoparticles remains a major hurdle on the way towards magnetically targeted applications at realistic technical conditions. Herein, we present a unique one-pot approach that relies on simple basic hydrolyticin situcoprecipitation of inexpensive metal salts (Fe2+and Fe3+) compartmentalized by stabilizing fatty acids and aided by the presence of alkylamines. The synthesis was performed at relatively low temperatures (~80°C) without the use of high-boiling point solvents and elevated temperatures. This method allowed for the production of ultra-small, colloidal, and hydrophobically stabilized magnetite metal oxide nanoparticles readily dispersed in organic solvents. The results reveal that the obtained magnetite nanoparticles exhibit narrow size distributions, good monodispersities, high saturation magnetizations, and excellent colloidal stabilities. When the [fatty acid] : [Fe] ratio was varied, control over nanoparticle diameters within the range of 2–10 nm was achieved. The amount of fatty acid and alkylamine used during the reaction proved critical in governing morphology, dispersity, uniformity, and colloidal stability. Upon exchange with water-soluble polymers, the ultra-small sized particles become biologically relevant, with great promise for theranostic applications as imaging and magnetically targeted delivery vehicles.

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Section: Introductionmentioning

confidence: 99%

Ultra‐Small Fatty Acid‐Stabilized Magnetite Nanocolloids Synthesized by In Situ Hydrolytic Precipitation

El‐Boubbou

Al‐Kaysi

Al-Muhanna

et al. 2015

Journal of Nanomaterials

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“…26 In recent years they have been widely used as precursors for synthesis of mixed metal oxide nanoparticles like CoFe 2 O 4 , NiFe 2 O 4 and spinel ferrite nanoparticles. [27][28][29][30][31] Zeolite-Y with high pore dimension of 7.4 Å is known to act as suitable host and also as support for transition metal complexes. 32 Zeolite-Y due to their special shape selectivity property allows a convenient route for encapsulation of transition metal complexes.…”

Section: Introductionmentioning

confidence: 99%

Oxidative coupling of 2-naphthol by zeolite-Y supported homo and heterometallic trinuclear acetate clusters

2014

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Two trinuclear acetate clusters of iron and cobalt of general formula [Fe 3 O(O 2 CCH 3 ) 6 (H 2 O) 3 ]NO 3 $2H 2 O and Fe 2 Co(O)[(OOCC 6 H 4 NO 2 ) 6 ]NO 3 $2H 2 O are synthesized and characterized. The synthesized trinuclear clusters are supported on zeolite-Y via an ion exchanged method. FTIR study reveals that the two complexes are tethered via formation of Si-O-H/O-H hydrogen bond linkages with a zeolite-Y matrix. Homogeneous and heterogeneous trinuclear catalysts are found to be efficient catalysts for oxidative coupling of 2-naphthol. Compared to homometallic oxo-clusters, bimetallic complexes are found toshow better catalytic activity. Besides obtaining BINOL as a major product, these metal clusters also lead to formation of the tautomeric form of BINOL. The crystal structure of the by-product indicates the formation of a tetrahedral chiral centre in the molecule via the attachment of the solvent. Density Functional Theory (DFT) calculations have been performed to elucidate the structural and electronic properties of both homogeneous and heterogeneous complexes.

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“…Methods for synthesizing spinel ferrite nanocrystals include the coprecipitation of metal salts from alkaline aqueous solutions, , sol–gel methods, , and thermal decomposition of a mixture of two different metal complexes or one heterobimetallic single-source precursor via (i) heat-up or hot-injection methods at ambient pressure, ,, (ii) a solvothermal reaction at elevated pressure, ,, or (iii) microwave-assisted heating. , Spinel ferrite nanocrystals have also been obtained via mechanochemical processing of bulk materials using methods such as ball-milling in which solid–solid diffusion processes govern the conversion of two binary oxide materials (e.g., ZnO and Fe 2 O 3 ) into one ternary oxide material (e.g., ZnFe 2 O 4 ) and influence the final cation distribution. , Solid–solid diffusion processes, such as cation hopping, can also drive cation redistribution in hybrid core/shell nanocrystals during the high-temperature solution-phase shell growth reaction . In general, solution-phase synthetic approaches present a major advantage over their solid-state counterparts by providing the opportunity to use surface ligands and precursor solution chemistry to control the size and shape of the nanocrystals while achieving high monodispersity. − …”

Section: Synthetic Control Over Cation Distribution In Spinel Ferrite...mentioning

confidence: 99%

“…Another method that enables access to partially inverted NiFe 2 O 4 and ZnFe 2 O 4 nanocrystals is the use of a heterobimetallic single-source precursor. Abdulwahab et al synthesized heterobimetallic pivalate complexes Zn 4 Fe 2 O 2 (O 2 C(CH 3 ) 3 ) 10 and NiFe 2 O(O 2 C(CH 3 ) 3 ) 6 (HO 2 C(CH 3 ) 3 ) 3 and used them as precursors for ZnFe 2 O 4 and NiFe 2 O 4 nanocrystals, respectively . Injection of the precursors into a solution of oleylamine, oleic acid, and diphenyl ether at 260 °C produced nanocrystals with the nearly statistically random inversion parameters of 0.66 for ZnFe 2 O 4 and 0.69 for NiFe 2 O 4 .…”

Section: Synthetic Control Over Cation Distribution In Spinel Ferrite...mentioning

confidence: 99%

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Cation Distribution in Spinel Ferrite Nanocrystals: Characterization, Impact on their Physical Properties, and Opportunities for Synthetic Control

2021

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Metal oxide materials that adopt the spinel crystal structure, such as metal ferrites (MFe2O4), present tetrahedral (A) and octahedral [B] sublattice sites surrounded by oxygen anions that provide a relatively weak crystal-field splitting. The formula of a metal ferrite material is most precisely described as (M1–x Fe x )[M x Fe2–x ]O4, where the parentheses and square brackets denote the tetrahedral and octahedral sites, respectively, and x is the inversion parameter quantifying the distribution of M2+ and Fe3+ cations among these sites. The electronic, magnetic, and optical properties of spinel ferrites all depend on the magnitude of x, which, in turn, depends on the relative sizes of the cations, their charge, and the relative crystal-field stabilization afforded by tetrahedral or octahedral coordination. Compared to bulk spinel ferrites, the large surface-area-to-volume ratio of spinel ferrite nanocrystals provides additional structural degrees of freedom that enable access to a broader range of x values. Achieving synthetic control over the degree of inversion in addition to the size and shape is critical to tuning the properties of spinel ferrite nanocrystals. In this Forum Article, we review physical inorganic methods used to quantify x in spinel ferrite nanocrystals, describe how the electronic, magnetic, and optical properties of these nanocrystals depend on x, and discuss emerging strategies for achieving synthetic control over this parameter.

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Hot injection thermolysis of heterometallic pivalate clusters for the synthesis of monodisperse zinc and nickel ferrite nanoparticles

Abstract: The heterometallic pivalate clusters have been used as single source precursors to synthesise zinc ferrite or nickel ferrite nanoparticles. The different reaction parameters, magnetic properties and XMCD were studied.

Cited by 14 publications

References 55 publications

Ultra‐Small Fatty Acid‐Stabilized Magnetite Nanocolloids Synthesized by In Situ Hydrolytic Precipitation

Ultra‐Small Fatty Acid‐Stabilized Magnetite Nanocolloids Synthesized by In Situ Hydrolytic Precipitation

Oxidative coupling of 2-naphthol by zeolite-Y supported homo and heterometallic trinuclear acetate clusters

Cation Distribution in Spinel Ferrite Nanocrystals: Characterization, Impact on their Physical Properties, and Opportunities for Synthetic Control

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