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Synthesis Methods and Favorable Conditions for Spherical Vaterite Precipitation: a Review

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Synthesis Methods and Favorable Conditions for Spherical Vaterite Precipitation: a Review crystals Review Synthesis Methods and Favorable Conditions for Spherical Vaterite Precipitation: A Review Donata Konopacka-Łyskawa Department of Process Engineering and Chemical Technology, Faculty of Chemistry, Gda´nskUniversity of Technology, Narutowicza 11/12, 80-233 Gda´nsk,Poland; [email protected]; Tel.: +48-58-347-2910 Received: 15 March 2019; Accepted: 18 April 2019; Published: 25 April 2019 Abstract: Vaterite is the least thermodynamically stable anhydrous calcium carbonate polymorph. Its existence is very rare in nature, e.g., in some rock formations or as a component of biominerals produced by some fishes, crustaceans, or birds. Synthetic vaterite particles are proposed as carriers of active substances in medicines, additives in cosmetic preparations as well as adsorbents. Also, their utilization as a pump for microfluidic flow is also tested. In particular, vaterite particles produced as polycrystalline spheres have large potential for application. Various methods are proposed to precipitate vaterite particles, including the conventional solution-solution synthesis, gas-liquid method as well as special routes. Precipitation conditions should be carefully selected to obtain a high concentration of vaterite in all these methods. In this review, classical and new methods used for vaterite precipitation are presented. Furthermore, the key parameters affecting the formation of spherical vaterite are discussed. Keywords: vaterite; calcium carbonate; polymorph; precipitation; synthesis; carbonation 1. Introduction Vaterite is the least thermodynamically stable anhydrous calcium carbonate polymorph and it easily transforms into more stable calcite or aragonite in the presence of water. This form of calcium carbonate mineral was named to honor the German chemist and mineralogist, Heinrich Vater, in 1903. Because of its instability, the existence of vaterite is very rare in nature. It have been found in some sediments and rocks [1], e.g., as a major constituent of a carbonated calcium silicate hydrogel complex formed from larnite in Ballycraigy, Ireland [2]. Vaterite can be precipitated in some mineral springs when specific glacial conditions take place [3]. Also, vaterite crystals have been identified in materials produced by living organisms, e.g., otolith organs of fishes [4–6], spicules of the ascidian Herdmania momus [6,7], freshwater pearls, crustacean tissues, or bird eggs [6,8] as well as the chalky crust on the surface of leaves of the alpine plant, Saxifraga scardica [9]. Synthetic vaterite particles have been used as a carrier of active compounds for medical treatments [10–14]. They have been tested as a template for biodegradable polymer capsules, which can be used for applications in nanomedicine [10,11,15]. Also, vaterite particles are added to personal care products as abrasives, adsorbents, anticaking agents, buffers, or dyes [15]. Due to their unique optical properties, vaterite microspheres has been useful in microrheology and microfluidics [16]. Spherical vaterite particles have been used to generate flow within microfluidic channels that has allowed the creation of an optical driven pump [17]. This polymorphic CaCO3 form has been proposed as a coating pigment for ink jet paper [18]. The main advantages of vaterite particles are their easy and low-cost preparation, ability to design particles with defined characteristics, porous structure, mild conditions for decomposition, non-toxicity, and biocompatibility [11,15]. Crystals 2019, 9, 223; doi:10.3390/cryst9040223 www.mdpi.com/journal/crystals Crystals 2019, 9, x FOR PEER REVIEW 2 of 16 Crystals 2019, 9, 223 2 of 16 CrystalsRecently, 2019, 9, x FORthis PEER unstable REVIEW mineral was widely investigated to identify the favorable conditions2 of 16 for its production as well as to verify its usefulness for various applications. Therefore, the current opinionsRecently, on vaterite thisthis unstableunstable synthesis mineralmineral as well waswas widelyaswidely a discussion investigatedinvestigated on the toto identify identifyvariables the the affecting favorable favorable its conditions conditions formation for for are its productionoverviewed.its production as Thewell as issues well as to asraised verify to verify in its this usefulness its review usefulness forare variouspresented for various applications. in the applications. diagram Therefore, in Therefore, Figure the current1. the current opinions onopinions vaterite on synthesis vaterite synthesis as well as as a discussionwell as a discussion on the variables on the a variablesffecting its affecting formation its areformation overviewed. are Theoverviewed. issues raised The issues in this raised review in are this presented review are in presented the diagram in the inFigure diagram1. in Figure 1. Figure 1. Diagrammatic representation of raised issues. Figure 1. Diagrammatic representation of raised issues. 2. Vaterite Properties Figure 1. Diagrammatic representation of raised issues. 2. Vaterite Synthetic Properties vaterite particles are usually produced as polycrystalline spheres. The main advantages of such particles’ morphology are the porous structure, large surface area, and greater Synthetic vateritevaterite particles particles are are usually usually produced produced as polycrystalline as polycrystalline spheres. spheres. The main The advantages main hydrophilicity in comparison to more stable calcite or aragonite [10,19,20]. Other morphological ofadvantages such particles’ of such morphology particles’ morphology are the porous are structure, the porous large structure, surface large area, surface and greater area, hydrophilicityand greater forms of vaterite can be also obtained, i.e., plates [21], hexagonal crystals [22], lenses [23], lamellar inhydrophilicity comparison toin morecomparison stable calcite to more or aragonite stable calc [10ite,19 or,20 aragonite]. Other morphological [10,19,20]. Other forms morphological of vaterite can aggregates [24], florets, or rosettes [21,25] as well as microtablets [26]. Examples of vaterite particles beforms also of obtained, vaterite can i.e., platesbe also [ 21obtained,], hexagonal i.e., plates crystals [21], [22 hexagonal], lenses [23 crystals], lamellar [22], aggregates lenses [23], [24 lamellar], florets, are shown in Figure 2. oraggregates rosettes [[24],21,25 florets,] as well or asrosettes microtablets [21,25] [as26 ].well Examples as microtablets of vaterite [26]. particles Examples are of shown vaterite in Figureparticles2. are shown in Figure 2. Figure 2. a b c Figure 2. Vaterite particles: ( a)) and and ( (b)) typical typical spherical spherical particles; particles; ( (c)) spherical spherical and and lens-like lens-like particles; particles; (d) deformed lens-like and crossed lens-like particles. (Figured) deformed 2. Vaterite lens-like particles: and (crosseda) and ( lens-likeb) typical particles. spherical particles; (c) spherical and lens-like particles; (d) deformed lens-like and crossed lens-like particles. Vaterite has a hexagonal crystal system, but the exact crystal structure of vaterite is still under Vaterite has a hexagonal crystal system, but the exact crystal structure of vaterite is still under discussion. The analysis of experimental data is consistent in that all vaterite structures belong to discussion.Vaterite The has analysis a hexagonal of experimental crystal system, data but is consis the exacttent incrystal that allstruct vateriteure of structures vaterite is belong still under to the the order-disorder (OD) family [27]. It means that the occurrence of multiple polytypes on the micro- order-disorderdiscussion. The (OD)analysis family of experimental [27]. It means data that is theconsis occurrencetent in that of allmultiple vaterite polytypes structures on belong the micro- to the to to macroscopic scale, as well as considerable stacking disorder, are both to be expected. Recently macroscopicorder-disorder scale, (OD) as family well [27].as considerable It means that stacki the occurrenceng disorder, of multiple are both polytypes to be expected. on the micro- Recently to macroscopic scale, as well as considerable stacking disorder, are both to be expected. Recently Crystals 2019, 9, 223 3 of 16 Burgess and Bryce [28] used the combined 43Ca solid-state nuclear magnetic resonance spectroscopic and computational method to indicate two crystal structures, i.e., the hexagonal lattice, P3221, and monoclinic lattice, C2, which have the best agreement between the simulated spectra and diffractograms with the experimental data. Selected properties of the vaterite are summarized in Table1. Table 1. Selected properties of vaterite. Properties Values Ref. 2.54 g/cm3 [2] Density 2.65 g/cm3 [27] 1 8 Ksp at 25 C 1.22 10 [29] ◦ · − Ksp for t = 0–90 C Ksp = 172.1495–0.077993T + 3074.688/T + 71.595logT [29] ◦ − Optical properties Semitransparent, colorless [17] Effective birefringence Dn = 0.06–0.1 [17] Refractive index n! = 1.55, n" = 1.65 [27] α 2 at 25 C 35.5 10 6 K 1 [30] V ◦ · − − Surface energy Calculated: 90 mJ/m2; experimental 34–73 mJ/m2 [31] 1 Solubility product; 2 Volumetric thermal expansion coefficient. The surface of the vaterite particles is usually hydrophilic. The hydrophobic vaterite can be obtained by the adsorption of amphiphilic molecules, e.g., oleic acid, at the interface of the produced vaterite [32]. The charge of vaterite particles depends on the composition of the solution and its pH. The values of the ζ-potential were negative when the vaterite particles were dispersed in saturated CaCO3 solution
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