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Natural titanium dioxide (TiO2) occurs in three distinct polymorphs (rutile, anatase, and brookite). Currently, TiO2 gained the attention of several researchers around the world. TiO2 is used in several applications because of its excellent properties (structural, optical, electrical, chemical, non toxic, etc.). Thus, the applications are influenced by its surface, size, morphology, and crystal phase. TiO2 as photocatalyst is widely used in energy and eco-friendly applications involving water purification, hydrogen production, phenol degradation, etc. The novelty of the present chapter lies in explaining the recently reported methods that are used to synthesize TiO2 nanoparticles, such as sol-gel, hydrothermal, precipitation, etc. The different properties of TiO2 are also provided in this chapter.
Laboratory of Useful Materials, National Institute of Research and Physicochemical Analysis, Ariana, Tunisia
Houyem Abderazzak
Laboratory of Useful Materials, National Institute of Research and Physicochemical Analysis, Ariana, Tunisia
Barış Avar
Department of Metallurgical and Materials Engineering, Zonguldak Bülent Ecevit University, Zonguldak, Turkey
Department of Nanotechnology Engineering, Zonguldak Bülent Ecevit University, Zonguldak, Turkey
*Address all correspondence to: mhadhbi_mohsen@yahoo.fr
1. Introduction
Titanium dioxide, with the chemical formula TiO2, is one of the most valuable raw material and has been used in several applications including photocatalysis, medicine, sensors, paints, environment, solar energy, and others. TiO2 has excellent corrosion resistance, good thermal and chemical stability, and low cost [1].
With the development of nanotechnology, TiO2 nanoparticles (NPs), with attractive properties, have been widely fabricated and developed. In the past decades, the demand of titanium dioxide NPs observed remarkable growth because of its specific properties. Moreover, titania is accepted as a pharmaceutical and food additive [2]. It is also used in destruction of viruses and bacteria, inactivation of cancerous cells, as well as clean-up of oil spills [3]. TiO2 NPs are employed for elimination of emerging contaminants [4]. Moreover, TiO2 NPs are one of the excellent semi-conducting materials applied in solar cells because of their good chemical stability, low toxicity, low cost, and high photocatalytic activity for the degradation of organic impurity [5, 6]. Furthermore, TiO2 NPs are widely used as photo-anode materials because of their powerful absorption of light particularly in UV range, good chemical solubility, excellent photo-corrosion resistance and low cost [7, 8]. TiO2 is widely used as photocatalyst material due to its suitable energy band gap, which is less than 3.5 eV [9].
The recent advances in TiO2 nanostructures and their applications have been summarized by Reghunath et al. [10]. Chen and Mao [11] have reported a review on the synthesis, properties, modifications, and applications of TiO2 NPs. Environmental and energy applications of titanium dioxide have been discussed by Ge et al. [12]. Mao et al. [13] have completed a review on the recent progress in TiO2 based catalysis for energy systems. In their work, Nur et al. [14] have investigated the development of TiO2 for improved dye degradation under UV-vis irradiation. In addition, the correlation between the improved in photocatalytic activity and various surface modifications have been reported [15]. Fujishima and Honda [16] prepared TiO2 used as photoelectrode for splitting water via photoelectrochemical water splitting.
This chapter provides recent advances in the synthesis of titanium dioxide NPs and their performance in different applications.
2. Synthesis methods of titanium dioxide nanoparticles
A number of methods have been used for the synthesis of TiO2 NPs, which are detailed below.
2.1 Polyol method
Recently, the polyol method has been found to be a very powerful route for the fabrication of nano-oxide and chalcogenide materials [17, 18]. In addition, polyol method is a simple and low cost route for fabricating metal oxide NPs.
Thus, a number of studies have been reported on the synthesis of TiO2 NPs by polyol method. For example, Shah and Rather [19] prepared TiO2 NPs by polyol method using titanium (IV) butoxide, ethylene glycol, and acetone. They concluded that the mean crystallite size increased from 9.3 to 66.9 nm when calcination temperature rises from 300 to 1000°C. In addition, the obtained products showed greater stability (zeta potential of −30.8 to −37.5 mV) in aqueous solutions. Also, Sasikala et al. [20] prepared a dispersed SnO2 on TiO2 NPs via polyol method at calcination temperature of 500°C. They concluded that the TiO2 containing SnO2 showed improved photocatalytic activity compared to pure TiO2 because of improved charge separation. Ultrafine anatase TiO2 nanocrystals, with size of 2–5 nm, have been prepared through polyol process [21]. Figure 1 shows the TEM images of TiO2 nanocrystals. The samples exhibited excellent photocatalytic activities.
Figure 1.
TEM images of TiO2 NPs prepared by polyol method [21].
Furthermore, polyol method was used to synthesize TiO2 NPs by using different mole ratios of titanium tetrachloride and polyvinylpyrrolidone [22]. The photocatalytic performance of the prepared TiO2 NPs attained 97.83% with a power conversion efficiency of 4.6%. Kang and co-workers [23] synthesized TiO2 NPs, with average size of 25 nm, via polyol from titanium isopropoxide by refluxing at 270°C during 12 h. After that, the sample was heated at 600°C for 3 h. The final product showed an excellent electrochemical performance.
2.2 Hydrothermal method
Hydrothermal method is one of the most used route for nanomaterials synthesis. BiOI nanoflowers/TiO2 nanotubes were developed for the detection of atrazine [24]. The sensing platform showed good analytical performance for detecting atrazine.
Alev et al. [25] prepared TiO2 nanorods, with diameter of 100 nm, by hydrothermal using titanium butoxide, hydrochloric acid and deonised water. They concluded that the sensor response was 200% for 1000 ppm H2. Additionally, TiO2 NPs with size of 20 nm were prepared by hydrothermal method [26]. Figure 2 shows the TEM image of TiO2 NPs. The result obtained by UV-VIS analysis revealed that the decrease in size of TiO2 NPs is beneficial to the blue shift of their absorption peak.
Figure 2.
TEM image of TiO2 NPs [26].
Le et al. [27] synthesized TiO2/graphene by hydrothermal method using TiCl4 as a precursor. High performance was attained for the catalysts including well dispersed TiO2 NPs on the graphene surface with loadings ranging from 16.5% to 26%. Similarly, Yang et al. [28] prepared TiO2 NPs by hydrothermal. The results revealed that the peptization of the precipitate favored formation of the rutile phase and highly crystalline anatase. Europium (Er) doped TiO2 NPs were prepared by hydrothermal method for photonic application [29]. TEM analysis showed that the average particle size was about 50 nm. Indeed, the Er doping leads to a change in morphology of NPs from rodlike to triangular for Er ions increased from 1 to 3 mol%, respectively (as presented in Figure 3).
Figure 3.
TEM images of Er doped TiO2 NPs: (a) 1 Mol %, (b) 2 Mol%, and (c) 3 Mol% Er2+ [29].
Ag doped TiO2 NPs, with crystallite size of 10/13 nm, were prepared via hydrothermal at temperature of 180°C for 120 min [30]. It was revealed that the maximum photodegradation of indigo blue attained 75% after irradiation time of 150 min. Dadkhah et al. [31] prepared anatase TiO2 NPs by hydrothermal. They achieved conversion efficiency higher than 2.61% with the influence of amine ligands as a shape controller.
2.3 Sol-gel method
Sol-gel process is a powerful pathway for the synthesis of multi-component materials because of its mild synthesis conditions and low temperature. Thus, several researches have been reported on the fabrication of TiO2 NPs by sol-gel method. For example, Sabry et al. [32] synthesized TiO2 NPs by sol-gel process. The prepared material showed efficient photocatalytic activity of up to 68% after 180 min. Hsiung et al. [33] investigated the structure of photocatalytic active sites of TiO2 NPs prepared by sol-gel. They concluded that the material exhibited an excellent photocatalytic activity. Additionally, TiO2 NPs used as catalyst was prepared by sol-gel in acid at pH 3 [34]. The result showed that the material exhibited excellent reactivity for the photocatalytic reduction of nitric oxide.
Venkatachalam et al. [35] prepared alkaline earth metal (Mg2+ and Ba2+) doped TiO2 NPs by sol-gel method using titanium isopropoxide as precursor. Figure 4 illustrates the SEM image of the metal-doped TiO2 NPs, which are spherical in shape. Furthermore, the final product exhibited higher photocatalytic activity for the bisphenol.
Figure 4.
SEM image of metal-doped TiO2 NPs prepared by sol-gel [35].
Saravanan and Duby [36] investigated the optical and morphological properties of TiO2 NPs synthesized via sol-gel method using titanium butoxide as a precursor. UV-Visible analyses revealed the absorbance peak in the UV region (about 380 nm) and FTIR spectrum confirmed the existence of anatase TiO2 in the range of 400–1000 cm−1. The average particle size of the TiO2 NPs determined by dynamic light scattering (DLS) was found 131 nm. Govindaraj et al. [37] synthesized TiO2 NPs to be used as a photo-anode by the sol-gel method. UV-Visible spectrum revealed the light absorption in the UV region with optical bandgap of 3.2 eV (see Figure 5).
Figure 5.
Schematic diagram of the sol-gel route used for preparing TiO2 NPs [37].
Sinha et al. [38] studied the structural, optical, and antibacterial performance of the Mg doped TiO2 NPs prepared by the sol-gel method. They reported that optical transmittance increases from 3 to 3.07 eV. In addition, the photoluminescence emission shows inner UV to blue resign from pure and doped TiO2 NPs. Furthermore, Mugundan et al. [39] synthesized barium doped TiO2 NPs by the sol-gel method. They concluded that the pure TiO2 NPs revealed higher second harmonic generation efficiency compared to barium doped TiO2 NPs. Nachit et al. [40] investigated the photocatalytic activity of TiO2 NPs prepared by sol-gel process at low temperature. The mean crystallite size of TiO2 NPs reached 30 nm at 500°C using an acid. In addition, the photocatalytic activity of TiO2 NPs revealed that the degradation of Rhodamine B under UV light have a removal efficiency of 95% during 60 min.
2.4 Chemical vapor deposition method
Chemical vapor deposition (CVD) is a powerful method for the synthesis of nanomaterials with enhanced performances.
Several works have been reported on the fabrication of TiO2 NPs by CVD. For example, Liu et al. [41] prepared TiO2 NPs by CVD method. They revealed that the gas phase hydrolysis reaction may be decomposed into two processes: (i) hydrolysis of TiCl4 into TiO(OH)2 and (ii) decomposition of TiO(OH)2 to TiO2. The influence of various concentrations of TiO2 NPs on CVD grown graphene was investigated by electrical charge transport measurements and Raman spectroscopy [42]. The schematic diagram of TiO2 doped CVD grown single layer graphene devices is presented in Figure 6. The obtained results showed that TiO2 change the electronic properties besides the structure of the CVD grown graphene.
Figure 6.
Schematic diagram of TiO2 doped CVD grown single layer graphene devices [42].
Similarly, Li et al. [43] synthesized TiO2 NPs, with mean particle size of 22 nm, by CVD method. The TEM image of TiO2 NPs is presented in Figure 7. They concluded that the TiO2 NPs with the metal ion dopants possess elevated photocatalytic activities compared to un-doped TiO2 NPS.
Figure 7.
TEM image of TiO2 NPs prepared by CVD [43].
Ding et al. [44] synthesized TiO2 NPs via CVD process. The results obtained by XPS and nitrogen ads/desorption revealed that most of TiO2 NPs were distributed on the external surface of the support and the coating was stable. V2O5-TiO2 NPs were prepared from two precursors by CVD [45]. They revealed that the CVD process was a suitable method for the single step synthesis of nanocomposite coatings. Lee et al. [46] prepared TiO2 NPs by CVD method. The results revealed that a 60 min sample coating time gave the most highly photocatalytic activity.
2.5 3D printing method
In the last few years, several works have been developed to fabricate 3D porous materials; principally 3D porous TiO2 based materials.
Arango et al. [47] prepared a porous TiO2 by 3D printing. They suggested that a large surface area could be realized for the TiO2 via 3D printing technology.
Liu et al. [48] used 3D printing to prepare the porous Pb/TiO2 composites applied to remove the organic contamination in the wastewater. The obtained materials exhibited high catalytic activity, good stability, and reusability against the treatment of high concentration 4-NP wastewater. The optical images of the Pb/TiO2 scaffolds with 4, 8, 12, and 16 layers are presented in Figure 8.
Figure 8.
Optical images of the Pb/TiO2 scaffolds with (a): 4, (b): 8, (c): 12, and (d): 16 layers.
Additionally, Aleni et al. [49] used 3D printing to fabricate a 3D dense and porous TiO2 structure. The final products exhibited similar mechanical properties to those of porous ceramics prepared via conventional methods.
Xu et al. [50] developed 3D printing to assembly TiO2 powders into hierarchical porous structures at macro and microscale. The schematic illustration of 3D printing process is presented in Figure 9. The obtained results showed that the TiO2 structures with abundant light absorption sites and high surface area could enhance the conversion efficiency of N2 and NH3.
Figure 9.
Schematic illustration of 3D printing of a hierarchical porous TiO2 [50].
Furthermore, Wang et al. [51] synthesized TiO2 NPs containing macrostructures by 3D printing for Arsenic (III) removal in water. They showed that 3D printing could fabricate and design macrostructures with special functions.
2.6 Mechanical alloying
Mechanical alloying (MA) is a low cost and simple route for preparing nanostructured materials among them TiO2 NPs. The schematic illustration of the MA is presented in Figure 10.
Figure 10.
Schematic illustration of the MA process.
Yao et al. [52] prepared nanostructured TiO2 coating by mechanical alloying process. The results showed that the obtained material exhibited an excellent photocatalytic activity. Vilchez et al. [53] synthesized TiO2 NPs by MA during 5 min. The TEM images of TiO2 NPs are presented in Figure 11. The obtained material, with size in the range of 2–4 nm and specific surface area of 298 m2 g−1, exhibiting a good photocatalytic activity.
Figure 11.
TEM images of TiO2 NPs prepared by MA [53].
Kim et al. [54] prepared TiO2 NPs by MA and heat treatment. The mean crystallite size was less than 6 nm. The UV-Visible spectrum showed that the obtained TiO2 NPs had an elevated wavelength rage (in the range of 650 and 700 nm) compared to Ni doped TiO2 (480–500 nm) and rutile (380–400 nm). In addition, PL spectrum exhibited a new emission peak confirming the decrease in the band gap. Furthermore, Fe (III) doped TiO2 NPs have been synthesized via MA [55]. The final product showed excellent selectivity, stability, sensitivity, and fast response. Additionally, Eadi et al. [56] developed new Fe doped TiO2 NPs by MA from FeCl3 and TiO2 powder. The results showed that the mean particle size was about 28 nm and the prepared material could be applied for gas sensing and photocatalytic degradation. Carniero et al. [57] investigated the effect of process parameters on the structural, optical, magnetic, and photocatalytic properties of iron doped TiO2 NPs prepared by MA. The results showed that the incorporation of iron in the TiO2 NPs has improved their photocatalytic activity.
2.7 Green synthesis
Green synthesis is a simple and ecofriendly method used for the preparation of nanomaterials. Abisharani et al. [58] synthesized TiO2 NPs from titanium trychloride using Cucurbita pepo seeds extract. FTIR results showed that the existence of different functional biomolecules acted as a reducing factor for conversion of TiO4 into TiO2 NPs.
Isnaeni et al. [59] prepared TiO2 NPs by green method including TiCl3 hydrolysis with mango-peel extract. They revealed that the used method could be employed as an alternative to prepare phase pure anatase and rutile. Helmy et al. [60] synthesized S doped TiO2 NPs by a novel green synthesis using Malva parviflora plant extract. They also studied their photocatalytic, antimicrobial, and antioxidant activities. The results showed that the samples exhibited good antibacterial and photocatalytic activities.
In addition, Samhitha et al. [61] studied the TiO2 NPs prepared by various green synthesis methods for anticancer applications. Shen et al. [62] prepared Ce doped TiO2 NPs supported on porous glass. Figure 12 shows TEM image of TiO2 NPs. The mean diameter was about 5 nm. This study concludes that the green method makes Ce doped TiO2 NPs immobilized on porous glass.
Figure 12.
TEM image of TiO2 NPs prepared by green method [62].
Additionally, TiO2 NPs were synthesized through green method from Demostachaya bipinnata extract [63]. It has been shown that the prepared TiO2 NPs are a good candidate for controlling mosquito vectors and agricultural pest management. Nabi et al. [64] prepared TiO2 NPs, with mean crystallite size in the range of 80–100 nm, by green method using citrus limetta extract (as presented in Figure 13). The results showed that the degradation activity was more than 90% within 80 min. This excellent photocatalytic activity confirms that TiO2 NPs are ecofriendly and have powerful applications in purification of water.
Figure 13.
Schematic diagram of the synthesis of TiO2 NPs by green method [64].
Figure 14 shows the different crystal structures of TiO2 [65]. As it can be seen in this figure, there are three forms (polymorphs) namely anatase, rutile, and brookite, which are classified according to their crystalline arrangements. Thus, rutile is the most stable at higher temperature, whereas anatase is the most stable at lower temperature. Furthermore, at high temperature, anatase and brookite could be transformed into rutile. Brookite in the powder or thin film forms reveals excellent stability and superior photocatalytic activity to that of anatase [66]. In addition, anatase is favored in photocatalysis because of its high photocatalytic activity between all the three polymorphs [19].
Figure 14.
Different crystal structures of TiO2 [65].
Table 1 illustrates the different properties of titanium dioxide NPs. As it can be concluded from these values, TiO2 NPs possess interesting physicochemical properties, which are influenced by different factors such as exposed crystal faces, morphology, and size of particles. Chen and Mao have published a review on the synthesis, properties, and applications of TiO2 NPs [11].
Figure 15 shows the different hierarchical nanostructures of TiO2. Four morphologies, involving 0D (quantum dots), 1D (nanotubes, nanorods, nanofibers,…), 2D (nanflakes nanosheets,…), and 3D (nanospheres, nanoflowers,…), can be obtained.
In this chapter, we summarized some advances in the synthesis and properties of titanium dioxide nanoparticles. TiO2 is basically found in three crystalline forms: brookite, anatase and rutile. Its important potential application including its use as a food additive, in cosmetics, as a pigment, semiconductor, as well as in catalysis and photocatalysis, for UV adsorption and hydrogen storage has contributed to its massive elaboration by different methods and processes. On the other hand, materials with a nanometric structure display structural, mechanical, physical, chemical, optical and electrical properties that are distinctly improved in comparison to the materials with a micrometric structure. However, each synthesis method allows favoring one or more of the above mentioned properties, allowing to promote the application of the obtained material in a specific field.
Several researches have been made on the preparation and characterization of TiO2 NPs for various applications. Different synthesis methods have been presented to prepare titanium dioxide nanoparticles. For instance polyol process, which combines simplicity and low cost, allows to obtain TiO2 NPs with different shapes and sizes depending on the starting reagents and operating conditions for photocatalytic activities applications. Hydrothermal is the most used method for nanomaterials synthesis and titanium dioxide can be successfully synthesized with different nanoscale shapes as sensors including dispersed TiO2 NPs on the graphene surface. Nevertheless, the sol-gel method remains a powerful alternative for the synthesis of multi-component materials at mild and low temperature conditions leading to efficient photocatalytic activity of TiO2. However, the Chemical vapor deposition process is suitable for the single step synthesis of nanocomposite coatings with enhanced properties. In this context, single layer graphene devices doped with TiO2 have been obtained by CVD. This doping has shown that TiO2 modifies the electronic properties as well as the structure of the CVD grown graphene. On the other hand, 3D porous TiO2 based materials with high catalytic activity and good stability can be obtained through 3D printing technology. Among the simplest and most cost-effective processes for nanostructured materials synthesis, mechanical alloying is a very powerful technique for rapid elaboration of TiO2 NPs with excellent photocatalytic activity Nevertheless, compared to conventional methods, green method has been proven to be far more efficient; low cost, and eco-friendly route to the synthesis of TiO2 NPs.
The results obtained in this work enable a better understanding of the synthesis methods as well as the different related properties of titanium dioxide nanoparticles. However, the selection of the synthesis method is conditioned by the required properties of the titanium dioxide NPs and the cost of the final material to be obtained. This is all the more sought after for a value-added and large-scale TiO2 elaboration, which promotes the development of more innovative applications.
XRD, SEM, and TEM are the most used techniques for the nanostructured titanium dioxide characterization. The structural, morphological, and intrinsic properties of TiO2 NPs were also discussed and related to its performance in various applications. Titanium dioxide was a prime candidate material because of its low-cost, high-abundance, and ease of synthesis.
The authors would like to thank Ms. Maja Bozicevic, Author Service Manager, for her remarkable efforts. This work was supported by Scientific Research Projects Coordination Unit of Zonguldak Bülent Ecevit University, project no 2022-73338635-01.
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Written By
Mohsen Mhadhbi, Houyem Abderazzak and Barış Avar
Submitted: 05 December 2022Reviewed: 11 April 2023Published: 02 May 2023
Open access peer-reviewed chapter
