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Boron compounds are beneficial additives for industrial applications due to their superior physical, chemical, mechanical, and thermal features. The common use of boron compounds can be listed as ceramic, glass, glazes, metallurgy, lubricating agents, non-linear optical devices, and nuclear processes. Metal borates can be classified in accordance with the metal atom in the structure. According to the metal borate type, each compound exhibits different properties and is preferred for various applications. The other significant factor of a material that makes it preferable for the industry is its morphological characteristics. With the developing technology and novel synthesis procedures, metal borates can be fabricated at different morphologies. The characteristics of the metal borates can be improved by the modification of their surfaces. Capping agents are additive materials that are used to control particle growth and/or modify the morphological features of compounds. There is a recent increase in the number of studies based on metal borates prepared by using capping agents. In this chapter, the theoretical background on metal borates, synthesis procedures of metal borates, classification of the capping agent, the effect of capping agent on particle growth and examples of capping agent use on metal borates preparation were explained. Also, the characteristics of the same metal borates at different morphological features were compared.
*Address all correspondence to: fatma.senberber@nisantasi.edu.tr
1. Introduction
Boron is a rare portion element of earth’s crust, and it is generally found in nature as the complexes of oxygen (O), hydrogen (H) other metal atoms. More than 150 boron minerals have been identified until today [1, 2]. Since including similar composition of most of the natural boron reserves (B, O, H, and metal atoms), “boron minerals” and “metal borates” might be considered synonymous words.
The majority of the boron reserves are found in Turkey (72.8%), Russia (7.6%), and South America (6.1%). Also, the smaller reserves could be seen in China, Kazakhstan, Argentina, Italy, Mexico, and Germany. The most abundant examples of the boron minerals can be listed as Borax (Na2B4O7·10H2O), Tincalconite (Na2B4O7·5H2O), Colemanite (Ca2B6O11·5H2O), and Ulexite (NaCaB5O6(OH)6·5H2O). In the reserves of boron minerals, particles commonly form in microcrystalline [3, 4].
The unique properties of borates could be explained by the high constant elasticity, heat resistance, corrosion resistance, luminescence, and low softening and melting temperatures [5, 6]. Also, recent studies exhibit the biocompatible properties of boron minerals [7, 8]. In the uses of boron compounds, the chemical nature and structure of borates provide multifunctionality [9]. Traditional uses of boron minerals can be seen in ceramics and glazes, detergents, agriculture, metallurgy, and fire retarding materials. With the effect of developed technologies, these compounds can also be utilized in energy storage systems, laser systems, optoelectronics, band gap engineering, tissue engineering, wound healing, bone regeneration, bone formation, antibacterial compositions, adsorption of pollutants from wastewater, and design of biochemical sensors [3, 4, 5, 6, 7, 8, 9, 10, 11].
Considering the properties that boron provides to the materials in which it is added and/or doped, its strategic importance emerges. For this reason, studies on the modification of metal borates, synthesis of novel metal borates, and related developments continue around the world. To increase their characteristics, specific types of metal borate compounds such as lanthanum borates or other rare earth-doped borates could be synthesized, or capping agents could be employed to modify their properties.
In the synthesis of specific metal borates, the reserves can be transformed to compounds at higher with high added value by the reaction metal sources with the boron mineral or boric acid (H3BO3) [12, 13, 14]. Lithium borates, zinc borates, and aluminum borates can be given as examples.
Capping agents could especially be used in nanoparticle synthesis. In the use of the capping agents, the particle sizes were mostly decreased, and the morphology was homogenized without changing experimental procedures. Also, produced particles become stabilized in the solution and agglomeration can be eliminated [15, 16]. Because of the high surface area to volume ratio of the smaller particle sizes, especially on the nanoscale, the compounds exhibited novel and remarkable features different from their bulk and molecular counterparts [17, 18, 19].
The characteristics of the prepared sample are associated with the designed experimental setup. For the effective use of capping agents, their role of them in the particle growth mechanism should be clarified. A detailed understanding of the connection between characteristics and synthesis procedures of the novel borates obtained will increase the correct form of metal borate use in industrial applications.
Capping agents are important additive materials to modify particle shape and size. The uses of the capping agents and modifiers have gradually increased both liquid-state and solid-state conditions. Several types of surfactants, polymers, extracts, ligands, cyclodextrins, dendrimers, and polysaccharides could be utilized with this aim. These organic compounds exhibit the ability to modify the metal surface, provide sufficient dispersion, and prevent the agglomeration of nanoparticle [20, 21].
2.1 Mechanism
The relationship between the capping agent and the metal surface is related to the electrical forces between the steric features of the surface, interfaces, composition, and chemical features of the ligand [20]. For a typically liquid-state synthesis procedure, the stages of particle formation include nucleation and growth. The modifying additives of capping agents are effective in both stages. Based on its characteristics, controlling the shape and size of the synthesized particles could be possible. With the addition of the capping agents, a draft could be prepared for the formation of the nucleus. The assumed draft also would be affected by the length of the molecules of the capping compound.
The growth mechanism of the particle can be explained with the steps of diffusion from cluster to particle surface and the bonding and/or reaction between ion and solid particles. Controlling the reaction and/or diffusion rate is also possible with the use of the reaction parameters [22].
Amphiphilic molecules of the capping agents include an apolar hydrocarbon group and a polar head group. The functionality of the capping agent is related to these apolar-polar groups. The apolar group reacts with the liquid medium, whereas the polar group bonded to the metal ion to contribute to the nanostructure [23]. The role of the capping agents on nanoparticle formation is schematized in Figure 1.
Figure 1.
The role of the capping agents on nanoparticle formation.
The capping molecule acts as a barrier for the transferring of ions on the produced particle surface. However, the partial transfer of the ions could be possible in the solution medium [22]. The selectivity of the capping agent is effective on the particle size of the prepared sample. The increasing selectivity will lead to lower mass transfer and limited particle growth. Two essential factors that affect the mass transfer between solution and particle are (i) the adsorption/desorption in the bulk and surfactant system; and (ii) the connection between the surfactant and the surface of the solid particle.
2.2 Classification
The functional groups of the capping agents are effective in the formation of solid particle–ligand interface, and ligand-solution interface. These groups are commonly found in polyatomic structures such as carboxylate, amino, and other coordinating groups including heteroatoms. According to the obtained interface between solid particle–ligand and ligand- solution, the fabricated sample could exhibit different properties such as hydrophilicity [24]. Anions or neutral molecules bound to the organic ligand centre are called donor atoms. The most common examples of the capping agent with the different donor atoms are presented in Figure 2.
Figure 2.
Common examples of the capping agent with the different donor atoms.
The classification of the capping agents is based on the donor atom of capping agents [23, 25]:
N-terminated capping agents are the organic ligands that include the donor atom of N such as cetyl trimethyl ammonium bromide (CTAB), octadecyl amine, (ODA), oleyamine, (oAm), hexadecyl amine, (HDA), polyvinyl pyrrolidone (PVP), and pyridine. These organic compounds are favorable to use in the preparation of metal oxide nanoparticles for being liquid state at room conditions, low cost, and stable in colloidal solutions.
O-terminated capping agents are the ligands that include the donor atom of O such as polyethylene glycol, linolenic acid, and oleic acid. These compounds could react with the double bond or are absorbed by the carboxylate group of the nanoparticle.
P-terminated capping agents are the organic structures that include the donor atom of P such as tri-n-octyl phosphine (TOP) and tri-n-octyl phosphene oxide (TOPO). Especially, they are preferable in the hot injection preparation methods with the starting materials of organometallic compounds.
S-terminated capping agents are the organic ligands that include the donor atom of S such as 1-thioglycerol. Mostly, they exhibit hydrophilic features.
Green capping agents are the ligands such as citric acid, enzymes, polyphenols, and biodegradable polymers. There is a remarkable increase in the use of green capping agents especially in nanoparticle synthesis with the development of green technologies, and the increasing importance of sustainability. The green ligands can be easily obtained from the extraction of aromatic plants, fruits, roots, leaves, and their peels. In the preparation of green ligands, the most common solvent used in the extraction process is water. The biochemical composition amount and quality may be affected by the operation parameters of the extraction process. However, there is no research was seen on the use of green capping agents in the modification of metal borates. This may be due to the effect of the capping agent on the particle growth mechanism that has not been adequately studied for the metal borate modification.
Metal borates are well-known materials due to their superior properties such as their resistance to physical, chemical, and thermal conditions, the activities of magnetic and electrical, and antibacterial behavior [12]. Metal atom links to the borate groups at the positions of tetragonal and trigonal, and the compounds exhibit symmetrical and asymmetrical stretching. These symmetric and asymmetric stretchings are typical for a molecule and could be examined by using the Fourier-transform infrared spectroscopy (FT-IR) and/or Raman spectroscopy. The characteristic band values of borates groups for metal borates for the FT-IR and Raman spectrums are summarized in Table 1.
Stretching type
FT-IR (cm−1)
Raman (cm−1)
B(3)-O
Asymmetrical
1600–1400
1500–1300
Symmetrical
1400–1200
1300–1200
B(4)-O
Asymmetrical
1200–950
1200–1050
Symmetrical
950–700
1050–750
Polyanions of (B6O7(OH)6)−2 and (B3O3(OH)4)−2
700–600
750–620
Table 1.
The characteristic band values of borates groups for metal borates for the FT-IR and Raman spectrums [26, 27, 28].
Some properties of the metal borate could be intrinsic to the metal atom bonded in structure, the designed experimental procedure, and the crystallinity of the sample. This would lead to specific uses of the metal borates according to their types. The synthesis of modified boron minerals can be beneficial for the special uses of metal borates. The common uses of metal borates according to the metal atom bonded to the borate structure can be seen in Table 2.
Examples, chemical formulas, and uses of some metal borates [2, 12, 13, 29, 30, 31, 32, 33, 34, 35, 36].
The modification of the metal borates would also lead to novel applications. Although the traditional uses of magnesium borates are thermoluminescence and neutron shielding, the studies on their novel uses showed that magnesium borates modified by capping agents exhibited the hierarchical porous microspheres in morphology and could be an alternative for the Congo Red adsorption from wastewater [37, 38, 39].
3.2 Synthesis procedures
Metal borates could be produced by using both liquid-state (hydrothermal) and solid-state (thermal) methods. The synthesis procedure of metal borate could also be adapted to novel technologies such as ultrasound and microwave methods [40, 41]. Although these technologies provide a minor or major decrease in particle size distribution, there is still a requirement for the homogenization in surface morphology of the obtained samples.
Liquid-state synthesis of metal borates involves the stages of (i) dissolution of metal and boron sources in liquid mediums, (ii) mixing the prepared solutions at the suitable ratio, reaction temperature, and time, and (iii) filtration and drying if it is necessary. Water is selected as the solution medium in liquid-state conditions; however, other types of fuels could also be used in metal borate preparation. The liquid-state synthesis procedure could also be entitled as hydrothermal, combustion, and co-precipitation methods [42, 43, 44]. The capping agent is usually added to the mixture of the dissolved sources. The main point of the liquid-state synthesis procedure is that the selected capping agent should be soluble in the solution for better interaction between the core particle and the capping agent molecules.
Solid-state synthesis of metal borates includes the stages of (i) mixing of metal and boron sources at the suitable mole ratios at powder state, (ii) calcination of prepared mixtures at the suitable reaction temperature and time, (iii) grinding, if it is necessary. The described method can be entitled as the solid-state, calcination or thermal method [45, 46, 47]. The capping agent should be added to the powder mixture. The main point of the solid-state synthesis procedure is to obtain a homogeneous mixture of powder at the initial state.
To improve the characteristics of the metal borates, some experimental procedures could also be defined as the combination of both methods. Most of the combinations include the preparations of metal and boron complexes in hydrothermal conditions and the calcination of the prepared complexes [44].
3.2.1 Effects of capping agents on the produced metal borates
In the heterogeneous form of processes of adsorption, desorption, surface reaction, and adsorbate lateral diffusion, each process includes bond-breaking and bond-making facts, which are related to the electronic properties of the reactants and surfactant material [20]. The growth-limiting role of the capping agent on particles is also based on the relationship between the particle and the capping agent. The efficiency of the capping agent is mainly based on the suitable matching of material and reaction conditions and the interaction of the capping agent with the core particle. Commonly, the proper amount of capping agent in the reaction medium is assumed as 1% or lower.
The advantages of the capping agent in metal borate synthesis can be listed as the homogenization of the sample surface, modification of particle shape, and obtaining smaller particle size. By using the cationic surface-active agent of CTAB, nonionic surface-active agent of Triton-114, and anionic surface-active agent of oleic acid, the modification of the surfaces of the hydrothermally synthesized zinc borates was presented in Figure 3. As could be seen in the SEM analysis results, in Figure 3, the capping agent uses of the CTAB and oleic acid decreased the length of the prepared samples whereas the use of T as a capping agent reshaped the particle appearance. Ipek (2020) also indicated the improvement of the fire-retardant properties of zinc borate by decreasing the particle sizes with the use of capping agents [36]. To overcome the problem of incompatibility of zinc borate in polymer matrixes, Li et al. (2010) produced hydrophobic zinc borate by the modification with oleic acid [47].
Figure 3.
The modification of hydrothermally synthesized zinc borates by using (A) without capping agent, (B) CTAB added, (C) triton 114 added, and (D) oleic acid added [36].
Erfani et al. (2012) synthesized ultra fine particles of calcium tetraborate by using the capping agent of PVP to control the particle size and to reduce the agglomeration in a co-precipitation method [17]. Khalilzadeh et al. (2016) experimented that increasing PVP addition up to a certain value in the production of lithium tetraborate narrowed the particle size range, reduced the average particle diameter, decreased agglomeration, and increased the band gap value [33]. Xing et al. (2019) studied the modifying effect of folic acid on the yttrium borate to strengthen its photoluminescence emission intensity features in hydrothermal conditions [48]. Liu et al. (2010) synthesized the nanoscale europium-doped barium borate (Ba–B–O: Eu3+) with the addition of oleic acid as a capping agent and enhanced the emission intensities of products by adjusting the correct ratio of the modifying agent [13].
The only drawback of the capping agent usage in metal borate synthesis can be explained by the decrease in crystallinity. A few studies indicated that the use of a capping agent could adversely affect the prepared sample and a decrease in the crystallinity of the product could be seen in some cases. In the fabrication of magnesium borate hydroxide powders, Kumari et al. studied the effects of different capping agents CTAB, SDS, and Triton on the products. The results indicated the well-modified morphology of the sample at lower crystallinity [49]. The XRD results of Kumari et al. were presented in Figure 4. As it was given in Figure 4, the adverse effect of capping agents on the Triton, SDS and CTAB added magnesium borate hydrates can be seen with the decreasing peaks of the (h k l) values of (0 2 0), (3 2 0), (2 1 1), (2 2 1), (5 1 0), (3 4 0) and (0 5 1). The decrease in crystallinity could be explained by the limited growth of the core particles due to the capping agent effect.
Figure 4.
XRD results of the synthesized magnesium borate hydroxides with different capping agents [49].
With the help of the nanoscale metal borate productions with the usage of the capping agents, samples with high added value have been obtained compared to the microcrystalline structures. In the use of a capping agent, the type of the capping agent, the amount, being soluble in the selected solvent and the interaction between the capping agent and particle are the key points. For the correct determination of the capping agent, the particle growth mechanism, and effects of the capping agent on it were detailed studied. Also, the advantages and disadvantages of the capping agent usage in metal borate preparation were discussed. The novel uses and changes in characteristics of modified nanoscale metal borates were presented.
It is expected that the significance of metal borates in industrial applications would be expanded with the increase of advanced technologies in their 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: 29 April 2023Reviewed: 04 May 2023Published: 25 May 2023
Open access peer-reviewed chapter
