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Solvothermal Synthesis Routes to Substituted Cerium Dioxide Materials

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Solvothermal Synthesis Routes to Substituted Cerium Dioxide Materials inorganics Review Solvothermal Synthesis Routes to Substituted Cerium Dioxide Materials James W. Annis 1 , Janet M. Fisher 2, David Thompsett 2 and Richard I. Walton 1,* 1 Department of Chemistry, University of Warwick, Coventry CV4 7AL, UK; [email protected] 2 Johnson Matthey Technology Centre, Sonning Common, Reading RG4 9NH, UK; janet.fi[email protected] (J.M.F.); [email protected] (D.T.) * Correspondence: [email protected] Abstract: We review the solution-based synthesis routes to cerium oxide materials where one or more elements are included in place of a proportion of the cerium, i.e., substitution of cerium is performed. The focus is on the solvothermal method, where reagents are heated above the boiling point of the solvent to induce crystallisation directly from the solution. This yields unusual compositions with crystal morphology often on the nanoscale. Chemical elements from all parts of the periodic table are considered, from transition metals to main group elements and the rare earths, including isovalent and aliovalent cations, and surveyed using the literature published in the past ten years. We illustrate the versatility of this synthesis method to allow the formation of functional materials with applications in contemporary applications such as heterogeneous catalysis, electrodes for solid oxide fuel cells, photocatalysis, luminescence and biomedicine. We pick out emerging trends towards control of crystal habit by use of non-aqueous solvents and solution additives and identify challenges still remaining, including in detailed structural characterisation, the understanding of crystallisation mechanisms and the scale-up of synthesis. Citation: Annis, J.W.; Fisher, J.M.; Thompsett, D.; Walton, R.I. Keywords: ceria; hydrothermal; catalysis; nanomaterials; crystallisation Solvothermal Synthesis Routes to Substituted Cerium Dioxide Materials. Inorganics 2021, 9, 40. https://doi.org/10.3390/ 1. Introduction inorganics9060040 Cerium dioxide, ceria, is well known for significant applications in heterogeneous catal- ysis, where it is frequently used as a redox-active support [1,2]. This chemistry is exploited Academic Editor: Duncan H. Gregory in numerous practical applications, exemplified by its use as the oxygen storage component in three-way catalytic convertors, as a support for precious metals for destruction of CO, Received: 22 April 2021 NO and hydrocarbon emissions in automotive exhausts [3–5]. There are many emerging Accepted: 11 May 2021 x Published: 21 May 2021 applications of ceria in catalysis and these include use in steam reforming [6], soot oxida- tion [7], water–gas shift [8], oxidation of volatile organics [9] and thermochemical water Publisher’s Note: MDPI stays neutral splitting [10]. All of these rely on the ease of reversible release of oxygen from the solid with regard to jurisdictional claims in that has the cubic fluorite structure type, which is well known for its oxide ion migration 4+ 3+ published maps and institutional affil- properties, accompanied by the reversible reduction of Ce to Ce . iations. Another important developing application of ceria is as an oxide-conducting elec- trolyte in solid oxide fuel cells [11]. Ceria-based solid electrolytes show promising con- ductivity in the temperature range 500–700 ◦C, and here, oxide ion vacancies are vital to optimise the hopping of ions to carry charge. Beyond heterogeneous catalysis and ionic conductors, biomedical applications of ceria are under development, such as in antioxi- Copyright: © 2021 by the authors. Licensee MDPI, Basel, Switzerland. dant defense [12–14]. The material also finds use in UV shielding [15–17], as an abrasive This article is an open access article agent [18] and in humidity sensors [19]. distributed under the terms and For most real samples of ceria, the ideal formula CeO2 is not found: in reality, there are 3+ conditions of the Creative Commons typically some levels of oxide defects and hence the presence of Ce to give the formula Attribution (CC BY) license (https:// CeO2−δ [20]. These intrinsic defects are inherently beneficial for the oxide ion migration that creativecommons.org/licenses/by/ gives rise to many of the materials’ useful properties, since bulk oxygen mobility is enhanced, 4.0/). but in order to further enhance defects, partial substitution of Ce by a second cation, M, to Inorganics 2021, 9, 40. https://doi.org/10.3390/inorganics9060040 https://www.mdpi.com/journal/inorganics Inorganics 2021, 9, x FOR PEER REVIEW 2 of 35 Inorganics 2021, 9, 40 2 of 34 is enhanced, but in order to further enhance defects, partial substitution of Ce by a second cation, M, to give ternary materials Ce1−xMxO2−δ is a common strategy. (Note that in this article,give ternary we refer materials to this replacement Ce1−xMxO2− asδ issubstitu a commontion to strategy. indicate (Note that a thatproportion in this article,of cerium we isrefer swapped to this replacementfor a second as cation, substitution rather tothan indicate “doping”, that a which proportion implies of cerium the addition is swapped of a secondfor a second species.) cation, If M rather is aliovalent than “doping”, (a trivalent which cation implies or thedivalent addition cation), of a second then a species.)greater proportionIf M is aliovalent of oxide (a trivalention vacancies cation are or divalentneeded to cation), balance then the a charge, greater Figure proportion 1. However, of oxide evenion vacancies replacement are of needed Ce by toan balance isovalent the cation charge, (such Figure as Zr1.4+ However,or Hf4+) engenders even replacement useful prop- of erties:Ce by the an local isovalent distortion cation of (such the structure as Zr4+ ordue Hf to4+ the) engenders size mismatch useful of properties: the ions introduces the local highdistortion lattice ofstrain the structure[5]. This makes due to these the sizesolid mismatch solutions ofhighly the ionsreducible introduces with a high significant lattice proportionstrain [5]. This of the makes bulk these cerium solid being solutions reduced highly at moderate reducible temperatures, with a significant with proportion redox prop- of ertiesthe bulk maintained cerium being over reduced many cycles at moderate of reduct temperatures,ion–oxidation. with Hence, redox propertiesceria-zirconia maintained has be- comeover manyone of cycles the most of reduction–oxidation. widely studied materials Hence, for ceria-zirconia redox catalysis, has becomeespecially one as of a thesupport most forwidely precious studied metals materials [21]. for redox catalysis, especially as a support for precious metals [21]. Figure 1. Schematic of of crystal crystal structure structure and and defects defects for for ceria ceria and and substituted variant variant [20]. [20]. ( (aa)) The The fluorite fluorite ceria ceria unit unit cell, cell, containingcontaining 8 8 oxygen oxygen atoms atoms (red) (red) forming a simple cube embedde embeddedd inside a face-centred cubic (FCC) array of Ce cations (green). Every Every second second oxygen oxygen cube cube contains contains a a Ce Ce cation, cation, as as il illustratedlustrated by by the the 4 4 semi-transparent semi-transparent oxygen oxygen atoms atoms on on the the right, right, belonging to the next unit cell. Overall, the fluorite unit cell has 8 oxygen atoms and 4 cerium atoms. (b,c) Illustration of belonging to the next unit cell. Overall, the fluorite unit cell has 8 oxygen atoms and 4 cerium atoms. (b,c) Illustration of the two main point defects which may or may not be preferentially nearest neighbours, depending on the dopant type the two main point defects which may or may not be preferentially nearest neighbours, depending on the dopant type and prevalence of oxygen deficiency. Cation defects, Ce3+ (in oxygen-deficient ceria) and Do3+ (in substituted ceria), sit in 3+ 3+ aand Ce4+ prevalence cubic site ofof oxygenOh symmetry deficiency. with Cation 8-fold defects,oxygen Cecoordination(in oxygen-deficient. Every two cation ceria) anddefects Do in (inthesubstituted structure are ceria), balanced sit in 4+ bya Ce one cubicoxygen site vacancy of Oh symmetry defect, VO with, which 8-fold sits oxygenin a tetrahedral coordination. site of Every Td symme two cationtry, with defects 4-fold in thecation structure coordination. are balanced Repro- by ducedone oxygen from vacancySchmitt, defect,R.; Nenning, VO, which A.; Kraynis, sits in a tetrahedral O.; Korobko, site R.; of TdFrenkel, symmetry, A.I.; Lubomirsky, with 4-fold cation I.; Haile, coordination. S.M.; Rupp, Reproduced J.L.M. A reviewfrom Schmitt, of defect R.; structure Nenning, and A.; Kraynis,chemistry O.; in Korobko, ceria and R.; its Frenkel, solid solutions. A.I.; Lubomirsky, Chem. Soc. I.; Rev. Haile, 2020 S.M.;, 49 Rupp,, 554–592, J.L.M. Published A review by of Thedefect Royal structure Society and of chemistryChemistry in[20]. ceria and its solid solutions. Chem. Soc. Rev. 2020, 49, 554–592, published by The Royal Society of Chemistry [20]. Coupled with substitutional chemistry is the effect of texture and crystal morphology on theCoupled properties with of substitutionalcerium oxide chemistrymaterials. isFo ther catalysis, effect of the texture highand surface crystal area morphology offered by smallon the crystallites properties is of desirable, cerium oxide but materials.the shape Forand catalysis, crystal habit the high can surfacealso affect area properties, offered by andsmall for crystallites ceria, this is includes desirable, the but redox the shapeassoci andated crystal with oxygen habit can loss also and affect gain. properties, Thus, the andac- tivityfor ceria, of ceria this includesin catalysis the may redox depend associated crucia withlly oxygenon crystal loss habit, and gain.particularly Thus, the when activity na- noscaleof ceria crystallites in catalysis are may considered depend crucially[22–26], and on crystalwhen the habit, material particularly is used whenas a support nanoscale for crystallites are considered [22–26], and when the material is used as a support for precious precious metals, when specific crystal faces may offer favourable interactions. Similar re- metals, when specific crystal faces may offer favourable interactions.
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