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Preparation of Salt⁃Inclusion Materials in High⁃Temperature Molten Salt System and Their Potential Application

Xu Zhang , Lei Zhang , Shanen Huang , Zhifang Chai , Weiqun Shi

Progress in Chemistry ›› 2022, Vol. 34 ›› Issue (9) : 1947 -1956.

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Progress in Chemistry ›› 2022, Vol. 34 ›› Issue (9) : 1947-1956 DOI: 10.7536/PC211125
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Preparation of Salt⁃Inclusion Materials in High⁃Temperature Molten Salt System and Their Potential Application
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Abstract

Salt⁃inclusion materials (SIMs), novel crystal materials with a unique host structure and guest salt inclusion, are of great interest to researchers due to their excellent porous, packable and flexible structure. The synthesis of SIMs is very challenging, as most of them are obtained serendipitously. To develop these materials for further application, it is important to understand their crystal chemistry, synthesis mechanism and relevant properties. In this work, we review typical SIMs synthesized in high⁃temperature molten salt system in recent years, classify them by their crystal frameworks, discuss some SIMs with unique structures and summarize their characteristics. This paper also introduces the potential application of SIMs in the environmental, photoelectric, thermoelectric and fluorescence fields. For the future development of SIMs, further investigation of their crystal chemistry is still needed to explore their applications

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salt⁃inclusion materials (SIMs) / molten salt method / framework structure / application

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Xu Zhang, Lei Zhang, Shanen Huang, Zhifang Chai, Weiqun Shi. Preparation of Salt⁃Inclusion Materials in High⁃Temperature Molten Salt System and Their Potential Application. Progress in Chemistry, 2022, 34(9): 1947-1956 DOI:10.7536/PC211125

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Contents

1 Introduction
2 Characteristics of molten salt method
3 The structure of salt⁃inclusion materials
3.1 Silicates⁃based SIMs
3.2 Germanates⁃based SIMs
3.3 Phosphates⁃based SIMs
3.4 Vanadates⁃based SIMs
3.5 Borates⁃based SIMs
3.6 Salt⁃inclusion chalcogenide
4 Potential applications of the SIMs
5 Conclusion and outlook

1 Introduction

Salt Inclusion Materials (SIMs) are a new class of inorganic hybrid compounds with covalently bonded metal frameworks filled with simple ionic salts of 0 D, 1 D, or 2 D[1]. Its unique structural characteristics can realize the flexible collocation and optimization of "host skeleton" and "guest salt", thus creating more substances with excellent properties[2]. SIMs have attracted much attention among many new materials because of their unique characteristics, and have good performance in the fields of optoelectronic devices, fluorescent materials, radioactive nuclear waste disposal, thermoelectric materials and magnetic materials[3⇓⇓⇓~7].
At present, the main synthesis methods of SIMs are hydrothermal method, molten salt method and high temperature and high pressure method, among which the molten salt method is the most commonly used method[8,9]. The process of SIMs growth by molten salt method is usually as follows: the reactant is put into a certain proportion of eutectic salt, the salt is melted by high temperature heating, and the reactant reacts with the molten salt to crystallize and form SIMs in the cooling stage. The high temperature molten salt makes the reaction system have excellent fluidity, which can promote the diffusion of reactants. It can also participate in the reaction and get the target product more easily.
According to the existing reports, the synthesis of SIMs is very challenging. Many reported SIMs were obtained by accidental growth in the process of exploration, and the more commonly used molten salt system is alkali halide[10⇓~12]. The common synthesis method is to replace the ionic salt and/or skeleton components in the known structure by the chemical similarity of the elements to obtain new SIMs, although in practice, the change of size and charge may lead to the emergence of new structures.
The special structure and potential applications of SIMs have attracted more and more attention, but there is no review on all aspects of SIMs. In this paper, the synthesis routes, structural types, and potential applications of SIMs in molten salt systems will be reviewed.

2 Characteristics of Molten Salt Method

Molten salt method is usually a method of mixing reactants and molten salt in a certain proportion and melting them at high temperature. The reactants can be fully reacted in the molten salt, and the target product can be crystallized and separated out after cooling. Compared with the traditional solid phase and liquid phase synthesis methods, the molten salt method has many outstanding advantages, such as: (1) The molten salt method has a wide electrochemical window, which can produce some abnormal valence States and ion species that are unstable in traditional solvents, and many discoveries have proved the extended application of the molten salt method in the synthesis of special framework structures[13,14]. For example, the solubility of metal oxides in molten salts can promote the formation of various new complex oxides, such as transition metal phosphates, arsenates, and silicates[15,16]. (2) The molten salt method is beneficial to the growth of crystals. In the reaction process, the molten salt can provide a stable liquid phase environment for the reactants to fully mix them, thus increasing the diffusion rate of the reactants and the collision between ions to improve the reaction efficiency[17]. (3) There are many molten salt systems to choose from, such as nitrate, chloride, sulfate, etc. In addition, various mixed eutectic salts can be selected to reduce the reaction temperature and reduce the reaction consumption[18⇓~20].

3 Structure of SIMs

SIMs have a covalent mixed oxide framework with simple ionic salts filling the framework voids. The framework structure of traditional SIMs is usually composed of transition metal oxides interconnected with group 14 and 15 (Si, Ge, As, P, etc.) oxygen ion units. The framework has good structural variability, and the transition metal elements can be extended to actinides to form three-dimensional spatial networks with different sizes, such as uranium-based silicates, germanates, vanadates, phosphates, borates or chalcogenides[12,21⇓⇓ ~24][25⇓⇓~28][29⇓⇓~32][16,33⇓ ~35][36⇓~38][7,39⇓⇓⇓ ~43]. The interstices of these frameworks can be filled with ionic salts such as alkali metals and halogen ions, so that SIMs can be ion-exchanged to expand the variety of materials[1]. For example, the probability of forming non-centrosymmetric (NCS) materials can be greatly increased by flexibly configuring and optimizing halide ion salts to construct secondary units as centers and then form acentric polycation templates[4,44].
In this section, some reported SIMs (see Table 1) will be summarized and classified according to their framework.

3.1 Silicate-based SIMs

In earlier reports, silicate-like SIMs have been extensively studied in the field of NCS materials[45,46,54]. Mo et al. Found the orientational effect of halide salts on the porous structure from the SIMs of some phosphate and arsenate phases[45]. Based on this rule, they carried out a series of studies on silicate systems and reported the first silicate-like SIMs structure formed by the non-bonding electron guidance of the central chloride ion, with the chemical formula of [Ba6Cl3] [ M 4 + x Si12-xO34](M=Fe, Mn) (see compounds 1 and 2 in Table 1). Such crystals were grown in a BaCl2/NaCl molten salt system, consisting of a mixed metal oxide network and a barium chloride ion salt (as shown in Fig. 1).
According to the principle that polar structures can be obtained by using asymmetric units and monoatomic halides as templates, Lin et al. Prepared a new polar crystal of Ba4(BO3)3(SiO4)·Ba3X (see compounds 4 and 5 in Table 1)[47]. The coordination structure of B atom and Si atom is beneficial to the formation of NCS structure, which acts as a structure directing agent[54,55]. The addition of halide anions to borosilicate can also reduce the viscosity of the solution to avoid the formation of glass, which is more conducive to crystal growth.
Zur Loye et al. Used UF4, SiO2 and TiO2 to synthesize the [Cs8Cs8Cl1.4F0.6][(TiO)4(Ti6Si14O51)] silicate structure in CsCl/CsF molten salt (see Table 1). The compound 6),TiO2 was used as a structure-directing agent to participate in the synthesis of the framework[48]. As shown in Fig. 2, two Si6O17 chains in opposite positions along the a-axis direction share with the titanium oxide square pyramidal structure to form a 14-membered ring channel, which is connected in the c-axis direction by TiO4 and Ti4O14 titanate units, and the channel is filled with Cs6X(X=F, Cl) salts. This work illustrates the importance of transition metal units as structure directing agents for SIMs, which can be further developed to expand the class of SIMs.
Zur Loye et al. Synthesized two SIMs structures [NaK6F][(UO2)3(Si2O7)2] and [KK6Cl][(UO2)3(Si2O7)2] under KF/NaF, KF/KCl systems (see compounds 7 and 8 of Table 1)[49]. Taking [NaK6F][(UO2)3(Si2O7)2] as an example (shown in Figure 3A), UO6 and SiO4 constitute the [(UO2)3(Si2O7)2] channel, which is filled with halide ion salt octahedra. In the experiment, they used three crucibles with different surface area/volume ratios (Sa/Vol) to study their effects on the synthesis products. The experimental results show that with the decrease of Sa/Vol, the proportion of SIMs in the product is larger. They suggested that the smaller Sa/Vol reduced the availability of oxygen in the reaction, favoring other anions to be incorporated into the crystal. Based on this conclusion, they also reported an enhanced flux growth method for directional synthesis of SIMs, in which four new types of SIMs (see compounds 9 ~ 12 in Table 1) were grown using the Cs-X-U-Si-O (X = F, Cl) quinary phase space as a model system[50]. As shown in Fig. 3 B – e, their frameworks are all multi-membered ring channels with different topological structures formed by uranyl square double pyramids UO6 a nd SiO4 t etrahedra, and the channels are filled with CsxF ion salts to play the role of charge neutralization for the framework structure. They used UF4 and UO2 under the same conditions, and the results showed that it was easier to obtain SIMs and larger crystals by using UF4. Through a simple analysis of the pore charge, it is concluded that the framework with low negative charge density is easier to obtain large pores to accommodate ionic salts to achieve charge balance.

3.2 Germanate-based SIMs

Germanates have been relatively less studied than uranium-based silicate SIMs. In terms of the coordination mode of silicon, the most common is 4-coordinated SiO4 tetrahedron; Germanium has more abundant oxygen coordination environments, such as Ge2O7 tetrahedral, GeO4 square pyramidal, GeO5 trigonal bipyramidal, and GeO6 octahedral, which leads to the rich chemical structure and properties of germanates. Zur Loye et al. Synthesized 12 one-dimensional uranyl Germanic acid SIMs (see compounds 13 and 14 in Table 1) in a variety of halide molten salt systems[26]. Taking [KK6Cl][(UO2)3(Ge2O7)2] as an example (as shown in Figure 4A), its skeleton is [Ge2O7, and a 12-membered ring channel is formed by alternating uranyl square double pyramids and Ge2O7 tetrahedra. In the synthesis process, it is found that the molten salt can affect the type of ionic salt in the structural framework: in pure fluoride, chloride or eutectic salt, the framework is easily formed, but it cannot be synthesized in pure bromine or iodine molten salt system. However, this structure can be successfully synthesized using CsI/CsCl and KF/KBr eutectic salts. Because of the large radius of the iodide ion, Cs, Rb, K, Na, Ag, Br, Cl, and F are all accommodated into the salt lattice in addition to I. As shown in Figure 4 B, the framework is formed by alternating uranyl square double pyramids and (Ge2O7)6- dimers to form a 12-membered ring channel. Unlike Figure 4A, the uranyl polyhedral angle sharing makes the 1 D chain down the C axis.

3.3 Phosphate-based SIMs

Phosphate-based SIMs are of great significance to the discovery of SIMs materials. Hwu et al. Of Clemson University focused on obtaining open-framework structural materials with large pore size, and they first used the high-temperature molten salt method to synthesize a series of phosphate SIMs structures with open frameworks, which are the first examples of SIMs CU⁃2[K2Cs3Cu3(P2O7)2Cl3] and CU⁃4[Na2Cs2Cu3(P2O7)2Cl2] (see compounds 15 and 16 in Table 1)[51,52]. As shown in Fig. 5, both Cu ² 2 and CU ² 4 have 8-membered ring and 16-membered ring microporous frameworks composed of oxide units of CU and P, with pore sizes of 5.3×5.3Å2, 12.7×12.7Å2, 5.3×5.3Å2, 4.9×17.2Å2, respectively. CU-4 can be converted to CU-2 in KCl/CsCl molten salt system at 600 ℃, indicating the possibility of ion exchange in SIMs. Hwu et al. Predicted that the molten salt method could be applied to the synthesis of more new phases with large pore sizes, and since then SIMs have attracted the interest of many researchers.
Hwu et al. Synthesized a series of M3(P2O7)22-SIMs with complex structures (see compounds 17 ~ 19 in Table 1), the structural formula is A2M3(P2O7)2·A'Cl(M=Mn, Fe; A = Rb, Cs),For the first time, a new series of open frameworks of the type M3(P2O7 ) 2 2 - constructed from dimeric [M2O8] and trimeric [M3O12] units was realized[35]. They first synthesized Na2Mn3(P2O7)2·RbCl (shown in Figure 6A), whose skeleton is composed of P2O7 units and [M3O12] trimers, and the pore channels along the c-axis direction are filled with one-dimensional NaCl ion salt chains. K2Mn3(P2O7)2·CsCl and K2Fe3(P2O7)2·CsCl (shown in Figure 6B and C) were obtained by synthesizing the K derivative of Na2Mn3(P2O7)2·RbCl crystal, both of which are composed of P2O7 units and [Mn(1)2O8] dimers, and the difference between them lies in the stacking direction of the covalent framework: the former is superimposed along the b-axis direction, while the latter is superimposed along the a-axis direction. It can be seen from the three structures that when the A-site cation size is small (such as Na+), the transition metal oxide unit is more likely to form trimers, resulting in larger channels.

3.4 Vanadate-based SIMs

Structurally, vanadium can form vanadate units of different sizes and geometries, such as dimers, trimers, chains, and rings. Hwu et al. First reported a series of vanadic acid SIMs (see compound 20 in Table 1) with the general structural formula of [(AX)2B(VO3)2](A=Cs, Rb, X = Br, Cl, B = Mn, Cu), all of which are chain-linked and have a six-membered ring framework filled with CsCl ion salts[31]. As shown in Fig. 7 a and B, both (CsCl)2Mn(VO3)2 and (CsCl)2Cu(VO3)2 are BCl chains linked to vanadite chains, the difference being that the former are linked along the a direction and the latter along the ab diagonal. As shown in Figure 7 C, (CsCl)Mn(V2O7) is the [Mn2O6Cl2] chain and the VO4 unit are connected. Mahjoor et al. Grew a new single crystal of Cs5FeV5O13Cl6 vanadate (see compound 21 of Table 1) in CsCl/NaCl molten salt using metal oxides V2O5 and Fe2O3[30]. As shown in Fig. 7 d, there are two different vanadium sites in [V5O13]2-, which are square pyramidal and tetrahedral, respectively, sharing oxygen atoms to form a layered structure and stacking along the C axis, and Cs+ and [FeCl6]3- are distributed between the vanadate layers to form an ionic salt layer.
Hwu et al. Also used the molten salt method to synthesize the first example of water-soluble SIMs structure Cs11Na3(V15O36)Cl6 with transition metal oxide clusters (see compound 22 of Table 1), which consists of isolated [V15O36Cl]9- clusters and [Cs9Na3Cl5]7+ ion salts[32]. Fig. 8 shows the structure of the [Cs9Na3Cl5]7+ cation unit, which consists of two Cl@Na3Cs3 inverse triangular prisms and three Cl@Na2Cs4 octahedra, and the surrounding six [V15O36Cl]9- clusters,And three [V15O36Cl]9- clusters are connected, and the charge of the [V15O36Cl]9- anion cluster is balanced with a separate Cs+.

3.5 Borate-based SIMs

Borate is an ideal nonlinear optical (NLO) material due to its excellent optical properties and rich crystal chemistry. According to the anionic group theory, the B O unit is usually an NLO active group with excitation energy near the UV, which is beneficial to a wide transparency window[37,56]. When the B: O units are arranged in a π-delocalized BO3 triangle or a B3O6 coplanar arrangement, the borate has a larger second harmonic response (SHG), a wider transmittance, and a larger birefringence[57,58]. These properties can be enhanced by the introduction of halide anions during the synthesis process, which can act as an ionic lattice and make it easier to synthesize SIMs structures.
Yu et al. Introduced coplanar BO3 triangles in mixed alkali and alkaline earth fluoroborates to synthesize a boronate SIMs[Li3Ca9(BO3)7]·2[LiF](LCBF) (see compound 23 of Table 1), which has a one-dimensional open framework in which Li F chains exist[38]. As shown in Fig. 9, the polyhedra centered at Li, Ca and isolated BO3 triangles share vertices or share edges to connect with each other, forming a three-dimensional network structure. Along the a-axis direction, the LiF chain fills the gap of the channel. All B _ O groups in the crystal structure are isolated BO3 coplanar triangles, and these high density and coplanar arrangement of BO3 triangles can make LCBF show relatively large SHG response and birefringence properties.

3.6 Chalcogen SIMs

In addition to the metal oxide framework, there is also a kind of metal sulfide framework structure in SIMs, namely chalcogen SIMs. Chalcogenide SIMs also exhibit host framework and guest ion salt structures, and their host frameworks are all composed of [MxQy] polyhedra (M = main group or/and transition metal; Q = sulfur source), and the guest salt is composed of alkali metal (A), alkaline earth metal (AE), rare earth metal (RE) and halogen (X), which can also form abundant polymer clusters, one-dimensional chains, two-dimensional layers and three-dimensional framework structures[39,41,43]. Lin et al., from Fujian Institute of Material Structure, Chinese Academy of Sciences, have been devoting themselves to the structural synthesis of chalcogenide SIMs and the development of their potential properties, and have carried out a series of reports on the synthesis of chalcogenide SIMs by high temperature solid state method[39,41,43]. In addition, they used the molten salt method to synthesize a new compound [Ga2Se6]6- (see compound 24 in Table 1) with a unique long period stacking structure in CsCl system, in which the [Ga2Se6]6- dimer constructed the [Ga53Se96]33- layer through cis or trans intralayer connection (Figure 10 B), and the sufficiently long C axis (C = 50.012 (4) Å) satisfied the unique stacking structure of the two-dimensional [Ga53Se96]33- layer (Figure 10 a). It is worth mentioning about the synthesis method that it was only available in the presence of Mn (Cs6Cl)6Cs3[Ga53Se96], which they speculated acted as a catalyst.
In addition, they synthesized [Ga4S10]8- with a three-dimensional open [ZnGa4S10]6- rhombic framework structure (see compound 25 of Table 1) in a BaCl molten salt system, whose framework is composed of [Ga4S10]8- clusters and [ZnS4]6- tetrahedra sharing corners and achieving charge balance with one-dimensional [Ba4Cl2]6- chains in the pore channels (as shown in Fig. 11).

4 Potential applications of SIMs

SIMs have attracted wide attention in the fields of environmental, optoelectronic and fluorescent materials due to their unique chemical structures. Alkaline earth borates have excellent second harmonic response (SHG) and short ultraviolet edge, which can be applied to ultraviolet nonlinear optical (UVNLO) materials. Lin et al. Synthesized two new types of borosilicate SIMs Ba4(BO3)3(SiO4)·Ba3X(X=Cl, Br) (see compounds 4 and 5 of Table 1), as shown in Fig. 12, whose framework is a one-dimensional channel in which [Ba4(BO3)3(SiO4)],Ba3X chains exist[47]. They found that the way in which the BO3 triangular, SiO4 tetrahedral, and BaOn coordination polyhedral building blocks are filled may affect the macroscopic SHG coefficient. Its SHG effect is moderate, probably because all the BO3 triangles in the structure are helically arranged around the C axis, which is not conducive to the superposition of second-order susceptibility.
Aiming at the problem that infrared nonlinear optical (IRNLO) materials are difficult to have both large NLO coefficient (dij) and wide band gap, Liu et al. Successfully synthesized a sulfide SIMs Li[LiCs2Cl][Ga3S6] using CsCl molten salt (see compound 26 of Table 1)[59][2]. As shown in Fig. 13, this structure is the first example of a nanotunnel framework constructed by monosulfide tetrahedra, and the highly oriented GaS4 tetrahedra in the host framework can produce a moderate second harmonic response (0.7×AgGaS2), and the ionic salt in the framework enlarges the band gap to 4.18 eV, which reaches the maximum value of chalcogenide IRNLO, indicating that SIMs is a very promising IRNLO material.
SIMs have also demonstrated their applicability in the field of fluorescent materials, and as shown in fig. 14, Ju et al. Synthesized a series of Ba7B3SiO13Br:Dy3+ silicate SIMs structures (see compound 27 in Table 1) that crystallize in the hexagonal system with P63mc space groups[53]. The luminescence spectrum shows a strong blue emission band at 478 nm, a strong yellow emission band at 575 nm, and a weak emission band at 665 nm. According to the emission spectrum of Ba6.92B3SiO13Br:0.08Dy3+ excited at 349 nm, the chromaticity coordinates were calculated to be (0.317, 0.358) and located in the white light region. These results indicate that the material can be used as a white phosphor for white light emitting diodes.
SIMs have also shown new application potential in the field of thermoelectric materials. Chen et al. Have devoted themselves to the study of the structure and properties of new metal polychalcogenides grown by molten salt method[7]. They found a new type of chalcogenide SIMs,[Rb6Cl][RE23Mn7Se44](RE=Ho⁃Yb) with ultralow thermal conductivity under the RbCl molten salt system, which all crystallize in the space group of R ∥ 3m (no.166), and the two basic building units [RESe6] and [MSe6](M=RE/Mn) octahedra compose a unique framework according to the NaCl-like structure. The structural combination of the covalent host framework [RE23Mn7Se44]5- and the guest ionic salt [Rb6Cl]5+ results in an ultralow thermal conductivity (0.47~0.28 W·m-1·K-1) in the temperature range of 300 – 673 K (as shown in Fig. 15). This is the first report on the application of SIMs in the field of thermoelectricity, which shows that the new chalcogenide SIMs have great reference value for exploring materials with extremely low thermal conductivity.
In the environmental field, uranyl SIMs materials are gradually being studied for the disposal of nuclear waste[23]. Compared with traditional glasses, SIMs have more stable crystal materials, their covalent framework can fix actinides (such as U and Tc), and the ionic salts in the channels can contain ionic salts with radionuclides (such as Cs and I)[60,61]. Researchers hope to obtain uranium-based SIMs that can fix a variety of radionuclides, and further explore their thermal stability and leaching rate to achieve their application in nuclear waste disposal[62,63].

5 Conclusion and prospect

In this paper, the synthesis of SIMs by high temperature molten salt method is summarized from the aspects of synthesis route, structure and application. In the synthesis route, the high temperature molten salt method can provide a stable liquid environment for the reaction to prevent particle agglomeration and obtain a uniformly distributed SIMs crystal structure. The chemical structures and characteristics of SIMs of silicate, phosphate, germanate, vanadate, borate and chalcogenide were introduced, and the effects of charge density and the ratio of reaction surface area to volume on the preparation of SIMs of uranium-based silicate were summarized, which provided ideas for the follow-up study. In terms of application fields, its potential applications in the fields of photoelectricity, thermoelectricity and environment are listed.
At present, SIMs has made a series of progress, but there is still a lot of research space. The biggest challenge in the research is to stably synthesize a large number of SIMs single crystals, because the synthesis mechanism is similar to a "black box", and researchers have not been able to find a suitable synthesis method for SIMs. Monitoring the nucleation and growth of SIMs by in situ characterization at high temperatures may provide researchers with the optimal conditions to effectively control the synthesis of SIMs. Using DFT and VBT thermodynamic calculations to predict the new phase of SIMs can provide theoretical support for the experiment. The future development of SIMs is facing great challenges, and researchers still need to continue to explore their crystal chemistry, understand their synthesis rules, and further explore their properties and potential applications.

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Funding

National Science Foundation for Distinguished Young Scholars(21925603)

Major Program of the National Natural Science Foundation of China(21790373)

National Natural Science Foundation of China(U20B2020)

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