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Magnesium borates are compounds including mainly magnesium (Mg), boron (B) oxygen (O), and hydrogen (H). Magnesium borates are traditionally famous for their strong thermoluminescence, mechanical and thermal features due to their high elasticity coefficient, corrosion, and heat resistance. Because of being beneficial, especially in the applications such as thermoluminescence and X-ray screening, and ease of synthesis, magnesium borates are produced by using different experimental procedures exhibiting different characteristics. Main traditional synthesis techniques can be classified as liquid state and solid-state synthesis methods. With the help of novelties in synthesis technology, new techniques are beginning to emerge in magnesium borate syntheses such as hybrid synthesis, ultrasound, microwave, and capping agent addition. The strengthened characteristics of the compounds would lead to new applications such as stomach cancer chemotherapy and wastewater treatment. In this chapter, it is aimed to make a comparison between the characteristics of synthesized magnesium borates and their properties. In addition, new types of magnesium borates obtained by various synthetic techniques are expected to be useful for industrial applications such as space technology, radiation dosimetry, X-ray screening, ion batteries, and hydrocarbon reaction catalysis. Such classification of properties and the synthesis techniques will enlighten the relationship between the characteristics and novel applications of magnesium borates.
*Address all correspondence to: fatma.senberber@nisantasi.edu.tr
1. Introduction
Magnesium is the third most abundant element by mass in Earth’s surface composition. Magnesium-based materials are preferable, especially for their lightweight. Magnesium is found in nature as the combination of oxygen to form different minerals such as sulfates, carbonates, nitrates, and borates [1, 2]. Some kinds of magnesium compounds can be soluble, such as magnesium sulfate, magnesium nitrate, and magnesium bromide. These compounds are generally hygroscopic. Other types of magnesium compounds are known as insoluble, such as magnesium borate, magnesium oxide, and magnesium phosphate. The salt group of magnesium is effective in the corrosive behavior of magnesium compounds [3]. Being insoluble in water makes magnesium borates production easier with developed technology, such as hybrid synthesis methods, the use of microwave and ultrasound technologies.
As a magnesium-based compound, magnesium borate can be utilized in the applications of X-ray screening, radiation permeation, catalysis of organic reactions, strengthening of plastics, and ion-battery systems. The studies on magnesium borates are generally focused on synthesis techniques. The common aim of the developed synthesis methods is to decrease energy consumption. However, the characteristics of the prepared sample are related to the designed experimental setup. A thorough understanding of the relationship between synthesis procedures and characteristics of the novel borates obtained will help increased the use of the correct form of magnesium borate in industry.
As being notable magnesium compounds, magnesium borates mainly include the atoms of Mg, B, O; however, other types of elements may be included according to the reserves they are mined. According to the conditions they formed in nature or fabricated in the laboratory, the magnesium borates can include crystal waters and/or hydroxyl groups. Therefore, this type of magnesium minerals can be classified as hydrated or dehydrated forms. The common examples of identified magnesium borates and their crystal systems are presented in Table 1.
The arrangement of functional groups in the molecule determines the properties of magnesium borate [5]. As a chemical compound, magnesium borates mainly include the functional groups of three and four coordinated borate anions (B(3)-O and B(4)-O) connected to the magnesium atoms (Figure 1). The typical symmetric and asymmetric stretching in a molecule can be determined by Fourier-transform infrared spectroscopy (FT-IR) and/or Raman Spectroscopy.
Figure 1.
The examples of boron-oxygen linkages B(3)-O and B(4)-O.
Spectral analyses result of Admontite (MgB6O10·7H2O) samples prepared at different reaction times in hydrothermal conditions were presented in Figure 2. In FT-IR analyses of magnesium borates, the spectrum begins with the peak around 3500 cm−1 which indicates the crystal water for the hydrated compounds. The region above the 1600 cm−1 is generally called as “free H2O zone”. The effects of hydroxyl anions are seen as “bending of hydroxyl groups in plane” and “bending of hydroxyl groups out of plane”. The peaks between 1400 and 1200 cm−1 indicate “bending of hydroxyl groups in plane” whereas the peaks between 950 and 750 cm−1 are related with the “bending of hydroxyl groups out of plane”. The stretching between boron and oxygen atom is commonly seen between 1600 and 650 cm−1. The peaks in the region of 1600–1400 cm−1 are related with the “asymmetric stretching of B(3)-O”. “Asymmetric stretching of B(4)-O” can be explained with the peaks in the range of 1200–950 cm−1. The peaks at the lower wavelength values of 750 cm−1 can be interpreted with the “bending of B(3)-O” [6, 7, 8].
Figure 2.
Spectral analyses result of Admontite prepared at different reaction times (a) FT-IR spectra, and (b) Raman spectra [6].
In Raman analyses of magnesium borates, the characteristic peaks are seen in the wavelength region of 1200–250 cm−1. The peaks between 1200 and 1050 cm−1 are interpreted with the “asymmetric stretching of B(4)-O”. “Symmetric stretching of B(3)-O” and “symmetric stretching of B(4)-O” are seen in the range of 1050–900 cm−1 and 900–750 cm−1, respectively. For the hydrated forms of magnesium borates, the stretching for polyanion of [B6O7(OH)6]−2 and [B3O3(OH)4]−2 is seen between 750 and 620 cm−1. The “bending of B(3)-O” and “bending of B(4)-O” can be seen in the Raman shift wavelength ranges of 620–500 cm−1 and 500–250 cm−1, respectively [6, 7, 9].
2.1 Properties
The characterization studies on magnesium borates make them preferable in industrial applications. These compounds are known for their superior thermal and mechanical strength, stability, and high coefficient elasticity. According to their specific characteristics, magnesium borates can be used as anticorrosive agent, catalyst, lubricant, and adsorbent. Due to their thermoluminescence properties, they also have applications in radiation dosimetry, X-ray screens, space research, and nonlinear optic laser systems [10, 11, 12, 13, 14, 15, 16].
Magnesium borates can be utilized in hydrogen storage systems, acoustic insulation, and ion-battery systems thanks to their high corrosion resistance. The viscosity of melted magnesium borates is relatively low and exhibits excellent electro-conductivity. Therefore, magnesium borates can be used as either a coating agent on lithium-ion batteries or as an additive for electrolyte solutions [17, 18, 19, 20].
For being of biocompatible properties of magnesium, magnesium borate compounds have also begun to be evaluated as a biomaterial for being unhazardous to the environment and human health. The eco-friendly behavior of these compounds increased their applications in health and wastewater treatments. Fan et al., studied the role of magnesium borate on stomach cancer chemotherapy as a hydrogen release agent [21]. Ma and Liu [22] experimented with the Congo Red adsorption from wastewater by using the sample of 2MgO·B2O3·H2O [22].
2.1.1 Thermoluminescence
In nuclear research, dehydrated forms of magnesium borates such as MgB4O7, Mg2B2O5, and MgB2O4 are generally preferred. This can be explained by the decreasing hygroscopicity at reaction temperatures higher than 950°C and the ease of solid-state synthesis methods [11, 23, 24, 25]. Souza et al. [26] compared the thermoluminescence features of the synthesized magnesium borates in liquid-state and solid-state conditions and indicated better results of dehydrated samples [26]. MgB4O7 is the most studied composition among the magnesium borates, due to its thermoluminescence behavior. The studies on the thermoluminescence behavior of magnesium borates indicated their suitability of them in beta, neutron, and radiation dosimetry. Several rare earth elements of Cerium, Dysprosium, Samarium, Silver, Terbium, Thulium, have been doped to increase their efficiency in applications [23, 26, 27, 28, 29]. Also, Prokic and Christeen [30] and Pellicioni et al. [31] experimented with the beneficial effects of graphite addition to magnesium borates; and the 3% graphite content was determined suitable for the optimum thermoluminescence [30, 31].
2.1.2 Mechanical strength
Modification of thermoplastic materials with dehydrated magnesium borates can strengthen the tensile strength and strain failure. This situation can be explained with the increased physical crosslinking density and decrease in the size of bubble growth. For the mechanical strength increase, Mg2B2O5 is commonly preferred in literature [32]. Zhang et al. [33], analyzed the strengthening effects of magnesium borate addition on aluminum-based composites [33]. Baghebanadi et al., indicated the beneficial effects of dehydrated magnesium borates (Mg2B2O5 and Mg3B2O5) in addition to the cold crushing strength of magnesium-graphite composite [34].
2.1.3 Catalyst effect in reactions
Catalyst effect of magnesium borates can be utilized to both increase reaction conversion in the reactions of hydrocarbon and/or they can also be evaluated to catalyze the other types of inorganic borates such as boron nitride [35, 36]. In the catalytic utilization of magnesium borate, the purity and the morphology of prepared magnesium borate are notable. In this case, the synthesis of magnesium borate at different morphologies will promote the comprehensive use of this type of compound.
Ahmad et al. [10], studied the catalyst effect of rod-like magnesium borates on the electrochemical activity of the dopamine enzyme [10]. Intemann et al. [13], used magnesium borates to catalyze the selective reduction of pyridine [13]. Loiland et al. [35], investigated the catalysis effect of magnesium borate complexes on the oxidative dehydrogenation of ethane and propane mixtures [35].
2.1.4 Adsorption behavior
The determination of the adsorption behavior of magnesium borates is an up-and-coming practice among its applications. The few researches on the adsorption behavior of these compounds include the azo anionic dye of Congo red adsorption on the hierarchic porous particles of magnesium borates. According to the isothermal and kinetic estimations of the adsorption study, the adsorption mechanism can be explained with the Langmuir isotherm and Pseudo second-order kinetic model. The results also showed that adsorbents can be recycled with calcination at 400°C [22, 37, 38]. The comparison of maximum adsorbent capacity values (qM) for magnesium borates is presented in Table 2.
Type
Mineral name
Chemical formula
Crystal system
Hydrated
Admontite
MgB6O10·7H2O
Monoclinic
Aksaite
Mg[B6O10(OH)6]·2H2O
Orthorhombic
Halurgite
Mg4[B8O13(OH)2]2·7H2O
Monoclinic
Hungchaoite
MgB4O7·9H2O
Triclinic
Hydroxylborite
Mg3(BO3)(OH)3
Hexagonal
Inderite
MgB3O3(OH)5·5H2O
Monoclinic
Kurnakovite
MgB3O3(OH)5·5H2O
Triclinic
Mcallisterite
Mg2[B6O7(OH)6]2·9H2O
Trigonal
Pertsevite-(OH)
Mg2(BO3)(OH)
Orthorhombic
Pinnoite
Mg[B2O(OH)6]
Tetragonal
Preobrazhenskite
Mg3B11O15(OH)9
Orthorhombic
Szaibélyite
MgBO2(OH)
Monoclinic
Wightmanite
Mg5(BO3)O(OH)5·2H2O
Monoclinic
Dehydrated
Kotoite
Mg3[BO3]2
Orthorhombic
Suanite
Mg2[B2O5]
Monoclinic
Table 1.
Identified magnesium borates and their crystal systems [4].
Comparison of maximum adsorbent capacity values for magnesium borates.
In the studies of Zhang et al. [22] and Ma and Liu [37] magnesium borates were fabricated in hydrothermal conditions whereas Guo et al. [38] preferred thermal conditions [22, 37, 38]. As it is seen in Table 2, it has been observed that hydrated compounds have a larger BET surface area and maximum adsorbent capacity. The results indicated that both hydrated and dehydrated forms of magnesium borates can be a promising candidate for toxic dye adsorption.
2.1.5 Thermal behavior
Determination of thermal behavior for the magnesium borates could increase the evaluation probability as fire-retardant agents. Zhang et al. [39] studied the fire retardant effects of magnesium borate addition to the polyvinyl chloride (PVC) and lignin composite [39].
Thermal behavior of magnesium borates is related to hydrate groups in the structure. For the hydrated magnesium borates, thermal decomposition process begins with the dehydration reaction which means to split off the crystal water (·xH2O), and continues with the dehydroxylation reaction which means to split off hydroxyl anions (OH−) as a water molecule. With the increasing temperature, phase changes can also be seen.
As a typical example, thermal curves of TG and DTG for Admontite mineral between 25 and 750°C are presented in Figure 3. Admontite (MgB6O10·7H2O) mineral has lost its 7 moles of crystal water with a two-step reaction. In the first step, the reaction occurs in the range of 40–125°C, and the peak of DTG curve is seen at 116°C. The second step of decomposition emerges in the range of 125–570°C and the DTG peak is seen at 230°C. The mass losses of the first and second steps of decomposition are determined as 11% and 25%, respectively.
Figure 3.
TG and DTG curves of Admontite mineral (MgB6O10·7H2O).
For the dehydrated magnesium borate, only phase changes can be seen or the compound stays stable. This stability could be related with the reaction temperature of fabricated dehydrated magnesium borate.
The characteristic features of the samples associated with the composition, crystalline phases, and morphology are dependent on synthesis procedures. The magnesium borates can be fabricated in various morphologies of the rod, sphere, tube, whisker, belt, wire, porous, or multi-angular at both nanoscale and microscale [15, 40]. Examples of the different morphologies of magnesium borates were presented in Figure 4. Kumari et al. [15], synthesized the nano-scale whiskers of magnesium borates in hydrothermal conditions without a capping agent [15]. Liu et al. [40], prepared sub-micron rods of a dehydrated form of magnesium borates by calcination at higher temperatures than 600°C [40]. Guo et al. [38], designed a hybrid method to fabricate the 3D hierarchical flower-like particles of magnesium borates [38].
Figure 4.
Examples of the different morphologies of magnesium borates (a) nano-scale whisker by Kumari et al. [15], (b) sub-micron rod by Liu et al. [40], and (c) flower-like particle by Guo et al. [38].
The experimental design should be both low-cost and eliminate the risk of byproduct formation. The design can be shaped according to the required features of particles. Therefore, synthesis procedures can be classified as liquid-state, solid-state, and hybrid synthesis with the effect of development in production technologies.
3.1 Liquid-state (hydrothermal) synthesis
Liquid-state synthesis of magnesium borates principally includes the dissolution of raw materials in a suitable solvent medium and the reaction occurs with the impulsive effect of temperature increase. Commonly, the type of magnesium salts such as magnesium oxide (MgO), magnesium chloride (MgCl2), magnesium sulfate (MgSO4), and magnesium nitrate (Mg(NO3)2) is reacted with boric acid (H3BO3) or tincal (Na2B4O7·10H2O). At the end of the reaction, the solution is filtrated and dried. The growth mechanism could be explained by dissolution, nucleation, and recrystallization.
The growth mechanism according to the study of Ma and Liu is explained in Eqs. (1) and (2) [22]:
B5O6OH4−+H2O→2B2O4OH24−+H3BO3aq+7H+E1
2Mg2++B2O4OH24−→Mg2B2O4OH2E2
The particle shape and sizes can be controlled by optimizing the liquid-state reaction conditions. Derun et al. [6], fabricated the multi-angular particles of magnesium borate hydrates between the reaction temperatures of 80 and 100°C by using a traditional liquid-state method.
With the developing technology, liquid-state synthesis techniques can also be modified by the use of sonochemistry and capping agents.
3.1.1 Advantages of sonochemistry in liquid-state conditions
As being new and fast-growing technology, ultrasonic treatment has become a significant step in several industrial applications. It is seen that acoustic waves usage shortens the reaction time and increases the reaction yield in comparison with the traditional methods. Due to these effects of cavitation, energy saving can be obtained according to the experimental setup. For this reason, the use of an ultrasonic beam is preferred to obtain proper particle formation.
In many synthesis procedures, the ultrasonic treatment is accepted as a vital step. The employment of ultrasound in the synthesis procedure accelerates the reaction rate and yield. The effects of ultrasound can be operated by factors of power level, cycle, ultrasonic treatment time, and type of ultrasonic reactor. The common types of power sources for ultrasonic treatment in laboratory scale are presented in Figure 5.
Figure 5.
The examples of ultrasound sources in laboratory scale; (a) ultrasonic prob, and (b) ultrasonic bath.
The reaction mechanism of sonochemistry has not been defined in a detailed way. However, the beneficial contributions of ultrasound make it frequently employable in applications. The studies on the use of sonochemistry are generally based on the prevention of by-product formation, efficient use of raw materials, eco-friendly solvent usage, better waste management (selectivity), and energy savings [41].
Yildirim et al. [42] synthesized the mixtures of Admontite (MgB6O10·7H2O) and Mcallisterite (Mg2[B6O7(OH)6]2·9H2O) at higher reaction yields than 84% by using acoustic cavitation [42]. Kipcak et al. [43], produced the magnesium borate hydrates at higher crystallinity in a sub-micron scale with the effect of ultrasound energy [43]. The comparison of the Admontite morphologies synthesized by the ultrasonic liquid-state method and the traditional liquid-state method was presented in Figure 6. As is seen in Figure 5. In comparison with the traditional liquid-state methods, smaller particle sizes were observed in the use of ultrasonic-assisted synthesis techniques [6, 42].
Figure 6.
The comparison of the Admontite morphologies synthesized (a) by ultrasonic liquid-state method [42], and (b) by traditional liquid-state method [6].
3.1.2 Effect of capping agent in liquid-state conditions
The capping agents can be employed to overcome the drawbacks of the synthesis procedures and to produce particles with homogenous and novel morphologies. The selected surfactant can be cationic, anionic, or non-ionic. In the use of capping agent, the type of capping agent is not able to highlight the relationship between the agent and the core particle. Some type of capping agents use could decrease the particle size; however, the crystallinity of samples could be affected adversely [15]. This situation might require a more detailed examination of the relationship between the capping agent and the magnesium borate particle.
In the modified liquid-state synthesis of magnesium borates, the examples of the preferred capping agent are polyvinyl pyrrolidone (PVP), sodium dodecyl sulfate (SDS), nickel nitrate (Ni(NO3)2), cetyltrimethylammonium bromide (CTAB) and triton (T) [15, 37, 44, 45]. The examples of the effects of different capping agents on the synthesized magnesium borates were presented in Figure 7. Kumari et al. [15] reported the characteristic effects of surfactant addition to the liquid-state synthesis of magnesium borate particles and indicated the notable changes in morphology to obtain nano-whiskers [15]. In the synthesis of inorganic ceramic compounds, PVP is utilized to decrease particle size and/or to sustain homogeneous morphology. However, hierarchic porous structures were obtained in the PVP-based synthesis of magnesium borates [44].
Figure 7.
The effects of different capping agents on the synthesized magnesium borates (a) CTAB, (b) SDS, (c) T at low magnification, and (d) T at high magnification [15].
3.2 Solid-state (thermal) synthesis
Solid-state synthesis of magnesium borates fundamentally involves the mixture of the powders of raw materials without any liquid component and the reaction of solid powders occurs with the impulsive effect of temperature increase in high-temperature furnaces. The common magnesium sources preferred in this synthesis method are MgO and magnesium hydroxide (Mg(OH)2). Mostly, the raw materials are reacted in air atmosphere. The prepared sample is commonly in micron-scale at heterogeneous morphology. Mg2B2O7, MgB4O7, and Mg3B4O6 are notable combinations of dehydrated magnesium borates [45, 46].
In the phase diagram of Liu et al. [40] for the solid-state synthesis of magnesium borates, the reaction commonly occurs at higher reaction temperatures than 800°C [40]. In this synthesis procedure, the main drawback of solid-state is the requirement of grinding and sieving processes after the solid-state reaction. Chen et al. [47] used capping agent addition of Ni(NO3)2 to eliminate these extra processes of the solid-state synthesis procedure [47].
3.2.1 Advantages of microwaves in solid-state conditions
Microwave energy can be defined as non-ionizing electromagnetic radiation with frequencies between 300 MHz and 300 GHz [48]. Similar to the effects of sonochemistry in liquid-state conditions, microwaves can be beneficial to solid-state synthesis procedures to increase the interaction between the powders of raw materials. Unlike traditional calcination techniques, the heating direction is from the inside to the outside of the heated sample in microwave conditions. This situation could assist both to increase reaction yield in solid-state conditions and to decrease the by-product formation. The temperature increase is supplied with the microwave effects. The reaction costs can be reduced effectively with the optimization of reaction conditions. In the reaction procedure, microwave power level and microwave treatment time are notable operating parameters. However, the relationship between the microwave parameters and supplied temperature increase has not been comprehensively studied. In that case, more detailed experimental setups should be designed for the determination of the reaction mechanisms.
Very few studies indicated the possible use of microwave energy in magnesium borate synthesis. Kipcak et al. [49, 50], proved the beneficial effects of microwave to decrease the reaction time in magnesium borate synthesis in comparison with traditional calcination techniques [49, 50].
3.3 Hybrid synthesis
Hybrid synthesis procedure can be defined as the combination of liquid and solid-state conditions. The experimental procedure generally begins in hydrothermal conditions and continues with a solid-state step. Pechini, combustion, and sol-gel synthesis techniques can be assumed as examples of hybrid synthesis [51]. The steps of the hybrid procedure could be more complex than the traditional techniques; however, high purity and homogeneous morphology can be obtained. To strengthen the properties of magnesium borates, hybrid methods should be supported with novel technologies.
Gonzalez et al. [27], synthesized the Tm and Ag-doped MgB4O7 with the reaction of Mg(NO3)2 and H3BO3 in urea medium, at the calcination temperature range of 750–950°C by using the combustion method [27]. Zhang et al. [37]; preferred the capping agent of N, N, − dimethylformamide nitrate to fabricate the hierarchic porous particles of magnesium borates. The liquid-state reaction occurred at 150°C for 12 hours whereas the solid-state reaction continued at 600°C for 12 hours [37]. Chen et al. [44], fabricated the mesoporous structure of Mg2B2O7 in microsphere morphology by adding the SDS to the reaction medium of Mg(NO3)2 and borax. The two-step process began with the 80°C for 2 hours and continued with 500°C for 4 hours [44]. Wang et al. [52], prepared the fibers of magnesium borates with a two-step reaction. The mixture of MgCl2 and borax is reacted at 80°C for 12 hours and then sintered at 800°C for 6 hours [52]. In the hybrid synthesis of Zhu et al., the high purity of Mg2B2O5 was synthesized with the reaction of MgCl2, H3BO3, and NaOH [53].
The comparison of the obtained morphological features of hybrid and traditional procedures can be seen in Figure 8. The uniform particle formation was obtained in the hybrid synthesis of Chen et al. [44] whereas the heterogeneous morphology can be seen in the traditional hydrothermal synthesis of Derun et al. [6].
Figure 8.
The comparison of the obtained particle morphologies (a) hybrid [44], and (b) traditional [6] synthesis.
Magnesium borates are beneficial for many industrial-scale applications. The ease of their synthesis increases the interest in the studies in this field. The properties of synthesized samples are related with their characteristics. This situation requires the modification of the traditional synthesis method with novel technologies. In this chapter, the relationship between the characteristics, properties, and novel technologies was interpreted. The comparative table of traditional and advanced synthesis methods can be seen in Table 3. The common points of the advanced syntheses techniques are the increase in contact interfaces between the molecules of starting materials. Decreasing the reaction time and temperature can be obtained at higher reaction yields with the help of effective contact of molecules. The other important advantage is the modification of particle surfaces.
Method
Advantages
Disadvantages
Liquid-state
Ultrasonic-Assisted
Decreasing the reaction time
Uniform morphology
Increasing reaction temperature with increasing ultrasonic-treatment
Traditional
Increasing crystallinity
Longer reaction times
Non-uniform morphology
Solid-state
Microwave
Decreasing the reaction time
Uniform morphology
Complex experimental setup requires
Traditional
Increasing crystallinity
Higher reaction temperatures and times
Decreasing reaction yield
Non-uniform morphology
Hybrid
Modify the morphology
Decreasing the reaction time and temperature
Decreasing crystallinity
Table 3.
Comparison of traditional and advanced synthesis techniques.
The improved characteristics showed their effects in the applications. The common applications of magnesium borates are limited by mechanical and radiation permeation. However, the use of magnesium borates with the contribution of their redesigned morphologies was begun in adsorption, ion-battery agent, and hydrogen release agent in chemotherapy.
It is expected that the significance of magnesium borates in industrial applications would be expanded with the increase of advanced technologies in magnesium borate synthesis. In this case, the development of modified synthesis techniques with a novel experimental setup is suggested.
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Written By
Fatma Tugce Senberber Dumanli
Submitted: 11 February 2022Reviewed: 14 March 2022Published: 17 April 2022
Open access peer-reviewed chapter
