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Orthorhombic (Fe2tio5)-Monoclinic (Cr2tio5) Solid Solution Series

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Orthorhombic (Fe2tio5)-Monoclinic (Cr2tio5) Solid Solution Series Ceramics International xxx (xxxx) xxx–xxx Contents lists available at ScienceDirect Ceramics International journal homepage: www.elsevier.com/locate/ceramint Orthorhombic (Fe2TiO5)-monoclinic (Cr2TiO5) solid solution series: Synthesis by gel routes, coloring and NIR reflectivity evaluation ⁎ S. Cerro, C. Gargori, M. Llusar, G. Monrós Dpt. of Inorganic and Organic Chemistry, Jaume I University, Av. de Vicent Sos Baynat, s/n., 12071 Castellón, Spain ARTICLE INFO ABSTRACT Keywords: CrxFe2-xTiO5 compositions of the solid solutions series from pseudobrookite Fe2TiO5 to monoclinic Cr2TiO5 have Solid solution been prepared by the ceramic route and gel methods. At 1400 °C, pseudobrookite crystallizes in the x = 0–0.4 Pseudobrookite Fe TiO 2 5 range, both pseudobrookite and monoclinic Fe-Cr2TiO5 coexist at x = 0.5, while in the range x = 0.7–1.5 Monoclinic Cr2TiO5 monoclinic Fe-Cr2TiO5 crystallizes. Powders were 5 wt% glazed within a double-firing frit and the composition Cool pigment with x = 0.1 fired at 1000 °C exhibits the best red color (L*a*b* = 43.2/18.8/12.5), showing an intense band at 520 nm in the UV–Vis–NIR absorption spectrum associated with Cr4+ in octahedral coordination. The unit cell volume of the pseudobrookite decreases smoothly with the chromium amount, associated with the entrance of 4+ 4+ 3+ Cr replacing Ti , while the volume of the Fe-Cr2TiO5 unit cell increases with the entrance of Fe replacing Cr3+. The use of flux agents, the compaction pressure and the gel methods increase the crystallization of pseudobrookite but do not improve the reddish color, which is associated with the concentration of Cr4+ in the pigment. The optimized pigment composition Cr0.1Fe1.9TiO5 also shows a high NIR reflectance (55% in powder, 54% in glazed sample). 1. Introduction stabilize pseudobrookite phase at high temperatures. By decreasing the temperature, pseudobrookites decompose in the thermodynamically Pseudobrookite Fe2TiO5 is a reddish brown to ochre-yellow colored most stable phases, either a mixture of binary oxides M2O3 and TiO2 3+ 4+ mineral that was first described by Pauling [1] in 1930. The structure of (pseudobrookites M2 Ti O5), a mixture of ilmenite MTiO3 and rutile 2+ 4+ pseudobrookite (general formula AB2O5) shows orthorhombic sym- TiO2 (pseudobrookites M Ti2 O5) [12], or giving rise to a smaller metry (Cmcm space group) and gives its name to a large group of iso- symmetry phase (Ti3O5 case) [13]. In this regard, the higher or lower structural phases. The group of Ti pseudobrookites, including FeTi2O5, thermal stability of pseudobrookites is strongly dependent on its com- MgTi2O5,Fe2TiO5,Al2TiO5,Ga2TiO5 and Ti3O5, have an extraordinary position; this decomposition can be inhibited obtaining stabilized structure flexibility to accommodate many distinct metals (with +2, pseudobrookite at low temperatures or even at room temperature by +3 or +4 oxidation states) in their two different and distorted octa- adding different dopants or forming solid solutions. hedral cationic sites, A (4c) and B (8 f), giving rise to a number of solid The solid solution from Fe2TiO5 to FeTi2O5 was studied by Gray and 3+ 2+ A 2+ 3+ B solutions with general formula [M ,M ,Ti] [Ti,M ,M ]2O5. This Ward [14] and also by Navrotsky [15]. It has commonly been observed property, along with their high melting point and high refractive index that naturally occurring minerals with pseudobrookite structure have (2.4 for Fe2TiO5) [2], allow Ti pseudobrookites to be excellent candi- intermediate compositions; thus, in addition to varying proportions of dates for the development of new pigments. Indeed, some patents about Fe2+ and Fe3+ [16], other ions such as Mg2+,Mn2+/Mn3+,Al3+, and yellow pigments based on Ti pseudobrookites have been already de- Cr3+/Cr4+ frequently occur. It is well known that for the synthesis of veloped (Rademachers [3], Maloney [4], Katamoto [5] and Suzuki [6]), iron pseudobrookite Fe2TiO5 from anatase an iron (III) oxide, a sig- basically for low-temperature applications (paints, plastics, resins, etc.). nificant excess of titania with respect to the Fe2TiO5 stoichiometry is Moreover, some recent studies show that Ti pseudobrookites may also needed, in order to “achieve a complete reaction of the iron oxide” and be used as ceramic pigments for the coloration of glazes under more to obtain a hematite-free pseudobrookite [17].Ineffect, Seitz et al. [18] severe firing treatments [7–10]. conclude from Rietveld analyses that the stoichiometry of hematite-free Pseudobrookites are entropy-stabilized phases [11,12], that is to pseudobrookite is Fe1.94Ti1.06O5 at 900 °C and Fe1.91Ti1.09O5 at 1400 °C. say, the cationic disorder contributes the entropic component to Furthermore, the pseudobrookite phase obtained by sintering under air ⁎ Corresponding author. E-mail address: [email protected] (G. Monrós). https://doi.org/10.1016/j.ceramint.2018.04.167 Received 6 November 2017; Received in revised form 18 April 2018; Accepted 18 April 2018 0272-8842/ © 2018 Published by Elsevier Ltd. Please cite this article as: Cerro, S., Ceramics International (2018), https://doi.org/10.1016/j.ceramint.2018.04.167 S. Cerro et al. Ceramics International xxx (xxxx) xxx–xxx atmosphere does not have the Fe2TiO5 stoichiometric composition (it various amounts of the basic oxides and characterized by Mössbauer shows iron/titanium ratio lower than 2) and, moreover, this composi- spectroscopy [24], but the occurrence of this controverted polymorph tion varies with the temperature of thermal treatment. Seitz et al. from a solid state reaction is unusual. The most comprehensive work on propose two hypotheses to explain this variation of stoichiometric orthorhombic Fe2TiO5 and its solid solution with FeTi2O5 is the paper of composition: (i) the thermal treatment under air leads to an average Guo et al. [25], which shows that the whole solid-solution series has the oxidation number intermediate between 2 and 3 for the iron ions, and pseudobrookite (Cmcm) structure type. Guo et al. emphasize that no (ii) the occurrence of cation vacancies, concomitantly to a dense an- diffraction peaks associated to monoclinic specimen were detected in ionic subnetwork. However, the Mössbauer study performed on sam- any of the samples prepared for their study. Therefore Guo et al. found ples constituted by a single pseudobrookite phase strongly suggests that no evidence for the monoclinic phase reported by Shiojiri et al. [21]. crystallization of a pure pseudobrookite phase from iron-deficient The monoclinic Cr2TiO5, unstable at room temperature, is iso- chemical compositions (iron/titanium < 2) is not due to stabilization of structural with V3O5-type gamma-Ti3O5, CrFeTiO5 and V2TiO5 [26].In Fe2+ into the bulk but to the occurrence of cation vacancies [18]:a this communication chromium-doped pseudobrookite compositions of 3+ 4+ proposed formulation can be written as (Fe2−xTi1+x)1−zVzO5, with the the CrxFe2-xTiO5 solid solutions series from pseudobrookite Fe2TiO5 electroneutrality of the composition leading to the vacancy concentra- (x = 0) to Cr2TiO5 (x = 2) have been studied in order to stabilize a red- tion z = x/(x + 10); for instance, z∼0.006 (x∼0.06) and z∼0.009 brown pigment in CaO-ZnO-SiO2 ceramic matrices. The effect of several (x∼0.09) for the hematite-free pseudobrookite at 900 and 1400 °C re- flux agents as mineralizers and the use of non-conventional synthesis spectively. methods such as ammonia coprecipitation (CO), citrate route or metal- Yellow-ochre to reddish maroon or brown hues can be obtained by organic decomposition method (MOD) and a polymeric gel (GP) substituting iron or titanium ions with other metallic cations in pseu- method have also been studied. dobrookite (e.g., Mg2+). Pseudobrookite-based pigments were first On the other hand, the synthesis of pigments showing high NIR developed in the 1970s in order to get heat-resistant colorants for reflectance (the so-called “cool pigments”) is highly demanded nowa- thermoplastics, industrial paints, and other applications involving low- days, since they can help reduce the temperature of the external walls temperature treatments [18]. Dondi et al. [8] have studied the po- and therefore the temperature inside of buildings, thus reducing the tentialities of these types of compounds for ceramic pigment applica- power consumption during hot weather. Therefore, the NIR reflectance tions, i.e., applications involving high-temperature treatment. The of an optimized CrxFe2-xTiO5 composition is compared with a com- colors achievable with pseudobrookite pigments are significantly de- mercially available (Zn-Fe-Cr) brown spinel (CPMA 13-37-7) [27] in pendent on the composition of ceramic matrices, varying from satu- order to evaluate the pigment suitability as an energy-saving material. rated brown shades achieved in low temperature glasses to a lighter brown in stoneware glazes, while the colors fade to a light gray in 2. Materials and methods highly opacified glazes for wall tiles, where the high CaO and ZnO content contributes to rapid dissolution of the pigment [8]. According 2.1. Samples preparation to Dondi et al., the color is originated by several light absorptions in the 5 visible spectrum due to both d electrons transitions and a magneti- CrxFe2-xTiO5 compositions have been prepared by the ceramic route cally-coupled paired transition between iron ions in adjacent lattice (or solid state reaction method), using as precursors Fe2O3 and TiO2 6 4 4 sites. A doubling of the A1→ T1 and T2 bands is related to the oc- (anatase) supplied by Panreac S.A., and Cr2O3 supplied by Riëdel. In currence of Fe3+ in both octahedral sites of pseudobrookite [5]. Re- this ceramic method the precursors were homogenized in a planetary cently, Gargori et al. [19] described a red-brown ceramic pigment mill in acetone media. Once acetone was evaporated the raw powders based on chromium-doped ferrian armalcolite (MgFe)(FeTi3)O10, which were fired successively at 1000, 1200 and 1400 °C with a soaking time belongs to the pseudobrookite group X2YO5, with X and Y being usually of 3 h and with free cooling to room temperature.
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