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Inorganic Chemistry Frontiers INORGANIC CHEMISTRY FRONTIERS View Article Online REVIEW View Journal | View Issue Low-temperature wet chemistry synthetic approaches towards ferrites† Cite this: Inorg. Chem. Front., 2020, 7, 3282 Stefano Diodati,a Richard I. Walton, b Simone Mascotto c and Silvia Gross *a Ferrites are a broad class of iron-containing oxides that includes spinel ferrites MFe2O4, perovskites MFeO3, and hexagonal ferrites (hexaferrites) such as BaFe12O19. These materials have a wide array of appli- cations owing to their diverse properties: notable instances include catalysis, piezoelectric components, magnetic components, biomedical applications, heterogeneous catalysis and photocatalysis. Given the growing importance of environmentally friendly, low-temperature methodologies to obtain functional materials, there is a growing interest in synthetic approaches which are compatible with the principles of “green chemistry”. In this context, wet chemistry represents an attractive choice, and furthermore offers the possibility of scale-up for manufacture of materials in volumes for practical application. Though there is a sizeable amount of literature on the synthesis of ferrites, the most common approaches require treat- ments at temperatures above 200 °C, either as the main synthetic procedure itself (thermal decompo- sition), or as a post-synthetic step (for example, calcination after sol–gel autocombustion). This review Received 9th March 2020, aims at summarising, categorising, classifying and critically discussing the different low-temperature Accepted 11th May 2020 (<200 °C), wet chemistry approaches employed in recent years for the synthesis of ferrites. This will DOI: 10.1039/d0qi00294a include hydrothermal, solvothermal, sonochemical, and microwave methods, with examples taken from rsc.li/frontiers-inorganic literature making reference to the various sub-classes of ferrites. their specific structure – vide infra) have been shown to display Ferrites: a useful and multifaceted 6 33 class of compounds both hard (CoFe2O4) and soft magnetic behaviour, making Published on 12 2020. Downloaded 07.10.2021 03:28:02. them very attractive materials in applications ranging from Ferrites are a broad class of oxides containing iron which in magnetic recording to magnetic resonance imaging (MRI).6,34,35 general include spinel ferrites MFe2O4, perovskites, ilmenite Given the importance of ferrites in a wide variety of fields, (FeTiO3) and hexagonal ferrites (or hexaferrites). These numerous works have been dedicated to the synthesis and materials have a wide array of applications owing to their – – – 1,3,18,33,34,36 46 diverse properties.1 10 Notable examples include catalysis,11 15 study of these materials. The present review will, – piezoelectric components,16,17 magnetic components,18 21 bio- however, focus specifically on wet chemistry methods which – ff medical applications22,23 and photocatalysis,24 29 photo- not only a ord the desired materials, but also comply with the 47 anodes30 and photocathodes.31 In particular, their magnetic principles of Green Chemistry and can be achieved whilst ≤ properties make them convenient materials for heterogeneous maintaining low temperatures ( 200 °C) of synthesis, due to catalysis as they greatly simplify catalyst isolation and recovery the importance for industry to steadily move towards greener operations. In general, the nature of ferrites as iron-containing and more environmentally friendly approaches (vide infra “ oxides endows them with important magnetic properties, Green chemistry: the need for low-temperature wet synthesis ” which vary depending on the specific structure and nature of approaches ). non-iron metals involved.32,33 Spinels in particular (due to Spinels In general, spinel ferrites can be described as ferrites having aDipartimento di Scienze Chimiche – Università degli Studi di Padova, Via Marzolo the formula MFe2O4, where M is a divalent metal species (such 32,48–51 1, 35131 Padova, Italy. E-mail: [email protected] as Fe, Co, Zn, Ni Cu or others). From a crystallographic bDepartment of Chemistry, University of Warwick, Gibbet Hill Road, Coventry, CV4 point of view, spinel ferrites crystallise in a cubic close-packed 7AL, UK structure32,34 having Fdˉ3m symmetry with a unit cell contain- cInstitut für Anorganische und Angewandte Chemie, Universität Hamburg, Martin- ing 8 formula units (M Fe O ).21,34 In particular, metal ions Luther-King-Platz 6, 20146 Hamburg, Germany 8 16 32 †Electronic supplementary information (ESI) available: Table summarising within this structure occupy 1/8 of the tetrahedral and 1/2 of 32,48–50,52 examples of hydrothermal syntheses of BiFeO3. See DOI: 10.1039/d0qi00294a the octahedral sites. Spinel structures are divided 3282 | Inorg. Chem. Front.,2020,7,3282–3314 This journal is © the Partner Organisations 2020 View Article Online Inorganic Chemistry Frontiers Review between normal, inverse and partially inverse spinels. In 53 normal spinel ferrites (such as for instance ZnFe2O4) the tri- valent metal (i.e. Fe) occupies octahedral sites, whereas the divalent metal ions (Zn) lie in tetrahedral sites (Fig. 1). A second class of spinels are known as inverse spinels (such as 52 NiFe2O4); in inverse ferrites the iron cations are equally split between tetrahedral and octahedral sites, whereas the divalent atoms occupy in turn the octahedral sites vacated by iron. A third (much broader) subset of spinels exists where the structure is intermediate between normal and inverse, these are known as partially inverse spinels. In general, therefore, the chemical formula for a spinel ferrite may be written as TET OCT [M1−iFei] (MiFe2−i) O4 where the square and curved brackets labelled TET and OCT represent the tetrahedral and octahedral environments of the ions, respectively and i (where 0 ≤ i ≤ 1) is known as degree of inversion (with 0 indi- cating a normal and 1 indicating an inverse spinel ferrite structure).52 This distinction is very important because many of the par- ticular properties which make spinel ferrites such interesting Fig. 1 Crystal structure of normal spinel ferrite ZnFe2O4 highlighting functional materials arise directly from this distribution of the octahedral Fe (blue) and tetrahedral Zn sites (green) with red oxide – metal species over crystal sites.52,54 58 Many studies have been anions. carried out on how to control the cation distribution in spinels – to affect the final properties of the resulting material.52,54 56,58 While bulk ferrites have a typical degree of inversion, depend- has its own characteristic electronic structure, the oxides may – ing on the nature of the M metal, the value of i in nanosized feature novel or enhanced properties.68 71 ferrites may vary based upon the synthetic history of the This great variety of structural and compositional possibili- material; in particular, low temperature synthesis may allow ties endows spinel ferrites with a very broad spectrum of mag- – access to a different distribution of cations than can be netic, electric and functional properties,6,55,56,72 75 making – accessed at high temperatures.54,58 60 them materials of great interest in a high number of applicat- A subclass of spinel ferrites includes more than one metal. ive avenues. Nickel and magnesium ferrites have been reported “ ” “ ” ′ These doped or quaternary ferrites MxM 1−xFe2O4 can as potential catalysts for water splitting and CO2 25,76 Published on 12 2020. Downloaded 07.10.2021 03:28:02. therefore take advantage of the properties of both “parent fer- decomposition. The magnetic properties of spinel ferrites 19,42,61–67 rites” (MFe2O4 and M′Fe2O4). Because each M species have furthermore attracted interest in the fields of spintro- Stefano Diodati is a postdoc Richard Walton is Professor of fellow in the workgroup of Prof. Chemistry at the University of Silvia Gross. His field of research Warwick and his research group concerns the synthesis of crystal- is working in the field of in- line inorganic nanostructures organic materials, focussed on (ferrites, oxides, sulphides) the use of innovative synthesis through wet chemistry method- methods for functional solids. ologies, with a particular focus This spans zeotypes and metal– on low temperature, green organic frameworks through to methods such as subcritical condensed oxides, with an hydrothermal synthesis. A emphasis on solution-based syn- further focus of his research is thesis routes and characteris- Stefano Diodati the characterisation of inorganic Richard I. Walton ation using diffraction and spec- materials from the compositional troscopy including at synchro- (XPS, ICP-MS), structural (powder XRD) and morphological (SEM, tron and neutron facilities. Practical applications are explored and AFM) point of view. Most recently he worked on the statistical exploited through various industrial collaborations including in characterisation of coffee extracts through comparative NMR and areas such as heterogeneous catalysis and ionic conductors. He is other complementary techniques. presently an editor of the Inorganic Materials Series published by the Royal Society of Chemistry. This journal is © the Partner Organisations 2020 Inorg. Chem. Front.,2020,7,3282–3314 | 3283 View Article Online Review Inorganic Chemistry Frontiers – nics77 and biomedicine,78 81 where they can act as either drug carriers or as foci for hyperthermia treatments. Spinels have further found applications in the fields of sensors,82,83 mag- netic adsorbers,21,84 antiparasitic agents85 and as components – for magnetic devices.86
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