Particle size and entrapment efficiency of PLG‐rSAG microparticles.
\\n\\n
More than half of the publishers listed alongside IntechOpen (18 out of 30) are Social Science and Humanities publishers. IntechOpen is an exception to this as a leader in not only Open Access content but Open Access content across all scientific disciplines, including Physical Sciences, Engineering and Technology, Health Sciences, Life Science, and Social Sciences and Humanities.
\\n\\nOur breakdown of titles published demonstrates this with 47% PET, 31% HS, 18% LS, and 4% SSH books published.
\\n\\n“Even though ItechOpen has shown the potential of sci-tech books using an OA approach,” other publishers “have shown little interest in OA books.”
\\n\\nAdditionally, each book published by IntechOpen contains original content and research findings.
\\n\\nWe are honored to be among such prestigious publishers and we hope to continue to spearhead that growth in our quest to promote Open Access as a true pioneer in OA book publishing.
\\n\\n\\n\\n
\\n"}]',published:!0,mainMedia:null},components:[{type:"htmlEditorComponent",content:'
Simba Information has released its Open Access Book Publishing 2020 - 2024 report and has again identified IntechOpen as the world’s largest Open Access book publisher by title count.
\n\nSimba Information is a leading provider for market intelligence and forecasts in the media and publishing industry. The report, published every year, provides an overview and financial outlook for the global professional e-book publishing market.
\n\nIntechOpen, De Gruyter, and Frontiers are the largest OA book publishers by title count, with IntechOpen coming in at first place with 5,101 OA books published, a good 1,782 titles ahead of the nearest competitor.
\n\nSince the first Open Access Book Publishing report published in 2016, IntechOpen has held the top stop each year.
\n\n\n\nMore than half of the publishers listed alongside IntechOpen (18 out of 30) are Social Science and Humanities publishers. IntechOpen is an exception to this as a leader in not only Open Access content but Open Access content across all scientific disciplines, including Physical Sciences, Engineering and Technology, Health Sciences, Life Science, and Social Sciences and Humanities.
\n\nOur breakdown of titles published demonstrates this with 47% PET, 31% HS, 18% LS, and 4% SSH books published.
\n\n“Even though ItechOpen has shown the potential of sci-tech books using an OA approach,” other publishers “have shown little interest in OA books.”
\n\nAdditionally, each book published by IntechOpen contains original content and research findings.
\n\nWe are honored to be among such prestigious publishers and we hope to continue to spearhead that growth in our quest to promote Open Access as a true pioneer in OA book publishing.
\n\n\n\n
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\r\n\tIntegrated circuit (IC) forming from the integration of large numbers of very tiny electronic components into a small chip plays a key role in the nowadays circuit industries. Similarly, the circuit board (e.g., the printed circuit board) assembling with many electronic devices and IC components plays a significant role to enrich sciences, technologies and thus the daily applications in the world. A consumer electronic system usually needs a circuit board to integrate all the necessary components for performing the designed functions, such as a personal computer or a smartphone, for example. Consider the advanced developments and applications, the related challenges of manufacturing circuit boards may include materials, very high frequency, electromagnetic interference, energy strategy, flexible manufacture, bio/optic/electronic combination, 3D printing, standards, operating characteristics, recycling issues and so on. This book project intends to provide the reader with a comprehensive overview of the current state-of-the-art of circuit boards including materials and manufacturing technologies, developments and applications as well as the related issues.
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He received a Best Paper Award from the Chinese Institute of Engineers in 1989, and an Outstanding Teaching Award from the Yuan Ze University in 2005, respectively. He is a Senior Member of the IEEE. In 1991, he joined the Electrical Engineering Department of the Yuan-Ze Institute of Technology (currently Yuan Ze University), Taoyuan, Taiwan, ROC, where he is currently a Full Professor. Since 1998, his name has been listed in the Who\'s Who of the World. Currently, he serves as an Associate Editor of International Journal of Machine Learning and Cybernetics. He is the invited Editor of the book "Image Processing" published by InTech. 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Toxoplasmosis is of major clinical and veterinary importance. The infection in domestic animals such as sheep or pigs usually generates adverse economic impact due to the induction of severe abortion and neonatal loss [2]. In addition, toxoplasmosis in pregnant women may result in severe congenital fetal disorders, including hydrocephaly, blindness, and mental retardation [3]. Toxoplasmosis in immunocompromised individuals such as AIDS patients often develops lethal toxoplasmic encephalitis as an important opportunistic infection [4]. Although prophylactic anti‐Toxoplasma vaccines have been studied for a long time, only one commercial attenuated vaccine (Toxovax) has been licensed for use in sheep [5]. Most inactivated and recombinant vaccines developed in the past have produced only little to moderate protective efficacy against infections with a lethal challenge dose of the virulent strain of T. gondii [6].
Numerous earlier studies have demonstrated that cell‐mediated immunity is considered as the ‘appropriate’ immune response in the prevention of T. gondii infection [7]. Therefore, potent adjuvants that can improve cell‐mediated immunity have to include in Toxoplasma vaccine development in the future. In addition, gamma interferon (IFN‐γ), one of Th1‐type cytokines, mainly produced by CD4+ Th1 cells is able to subsequently stimulate CD8+ Tc cells to convert into cytotoxic effector cells for preventing acute and chronic T. gondii infection [6–8]. Thus, effective protection against T. gondii infection is critically dependent on the IFN‐γ‐associated Th1 cell‐mediated immunity. Therefore, effective vaccines formulated with potent adjuvants that are promised to induce an IFN‐γ‐associated Th1 cell‐mediated immune response seem more likely to be approved for use.
Most modern vaccines based on subunits of pathogens, such as purified proteins, are likely to be less immunogenic than traditional vaccine antigens and are often unable to initiate a strong immune response [9]. These subunit vaccines require effective adjuvants to aid them to elicit strong protective immune responses [10, 11]. Therefore, one of the current important issues in vaccinology is the urgent need for the development of new or improved adjuvants to enhance the immunogenicity or effectiveness of vaccines [9, 10, 12]. Different adjuvants capable of improving immunity and protection have been described in numerous studies [9, 10, 12]. However, the safety concern of an adjuvant is still a crucial issue to limit adjuvant development [13].
Adjuvants are special substances used in combination with an antigen to generate a more robust immune response than the antigen alone [11, 14, 15]. This broad definition encompasses a very wide range of materials for adjuvant development. Actually, adjuvants can be broadly separated into two classes, vaccine delivery systems and immunostimulatory agents, based on their main mechanisms of action [11]. Vaccine delivery systems are generally particulate, such as emulsions [16], micro/nano particles [17], iscoms, and liposomes [18], and their main function is to deliver antigens into antigen‐presenting cells (APCs) [11]. In contrast, immunostimulatory agents are predominantly derived from pathogens and often represent pathogen‐associated molecular patterns (PAMP), such as lipopolysaccharides (LPS) [19], monophosphoryl Lipid A (MPL-A) [20], and CpG oligodeoxynucleotides (CpG-ODN) [21], which activate cells of the innate immune system to induce the following acquired immune response [11].
This chapter will focus predominantly on microparticle adjuvant, especially poly(lactide‐co‐glycolide) (PLG) polymer, to be used in tachyzoite surface antigen (SAG)‐based subunit vaccines against T. gondii, the etiological agent of toxoplasmosis. In our recent work, recombinant SAGs (rSAGs), including rSAG1, rSAG2, and rSAG1/2, have been, respectively, encapsulated with the PLG polymer for production of PLG‐encapsulated rSAG1 (PLG‐rSAG1) [22], PLG‐encapsulated rSAG2 (PLG‐rSAG2) [23], or PLG‐encapsulated rSAG1/2 (PLG‐rSAG1/2) microparticles [24]. This chapter describes adjuvant effect of PLG microparticles, controlled release of PLG microparticles, PLG microparticles‐immune system interaction, Toxoplasma SAG‐loaded PLG microparticles, protective immunity by Toxoplasma SAG‐loaded PLG microparticles, and future prospects. The capability of these PLG microparticle vaccines to control the stable release of antigenic rSAG1 and effectively induce and extend protective immunity would be advantageous for their application in the development of long‐lasting vaccines against T. gondii for future use in humans and animals.
Microparticles, one of the vaccine delivery systems, derived from different biodegradable and biocompatible polymers, including poly(lactide‐co‐glycolide), alginate, starch, and other carbohydrate polymers, can be designed as safe carriers for proteins or drugs to perform the main function of delivery systems [25]. Particularly, PLG polymers approved by the US Food and Drug Administration (FDA) have been extensively used as sutures [26] and drug carriers [27] for many years. Different forms of PLG polymers can be generated according to the ratio of lactide to glycolide used for the polymerization [28]. In the recent 10 years, PLG polymers have further become safe and potent adjuvants or delivery systems to encapsulate vaccine antigens for the development of controlled release microparticle vaccines [29]. The PLG microparticles are biodegradable through hydrolysis to break down into the biocompatible metabolites, lactic and glycolic acids, which produce little inflammatory activity and are excreted from the body via natural metabolic pathways [28]. PLG polymers provide a number of practical advantages in acting as vaccine adjuvants or delivery systems following PLG encapsulation. The PLG microencapsulation protects antigens from unfavorable degradation [30], allows the sustained and extended release of antigens for a long period [31], and enhances antigen uptake by APCs, such as macrophages and dendritic cells, in specific lymphoid regions [32]. These adjuvant effects strengthen antigen immunogenicity to favorably generate strong specific immunity, especially cell‐mediated immunity [29], which is urgently required for eliminating intracellular pathogens, such as T. gondii.
Earlier significant studies have shown that potent cell‐mediated immunity induced by PLG microparticles following vaccination is likely to be due to the uptake of PLG microparticles into APCs and the effective delivery of microparticle‐containing APCs to specific lymphoid compartments [25, 32, 33]. The size of PLG microparticles used for animal vaccination is a crucial parameter in facilitating the uptake of APCs [32]. Particles smaller than 10 μm in diameter are appropriate for direct uptake by APCs, such as macrophages and dendritic cells [25, 32]. The proper size range thus can stimulate APCs to facilitate the microparticle uptake. Following the uptake of microparticles, the APCs containing microparticles then migrate to other lymphoid compartments [25], such as the spleen and mesenteric lymph nodes, where they effectively present antigenic epitopes to T lymphocytes, especially Th1 and Tc, thereby inducing strong specific cell‐mediated immunity [32, 33]. In other words, facilitation of uptake and delivery of PLG microparticles by APCs can lead to more effective antigen processing and presentation to T lymphocytes capable of inducting cell‐mediated immune responses [25, 32–34]. Significant earlier studies have further demonstrated that the APCs containing microparticles can travel to specialized mucosal lymphoid compartments, including mucosal‐associated lymphoid tissues (MALTs), the inductive sites for stimulating potent immunity following intranasal or oral vaccination [35, 36]. Thus, PLG‐encapsulated antigens can be designed as effective mucosal vaccines that have potential to stimulate mucosal systems, such as intestinal and vaginal tracks via intranasal or oral administration [36].
The capability of PLG microparticles to regulate the extended release rate of PLG‐encapsulated antigens can lead to long‐term immunity in microparticle‐vaccinated animals [29, 37]. Various studies have demonstrated that PLG microparticles may perform pulsed and/or slow release of encapsulated antigens to promote effective immune responses [38]. The sustained and extended antigen release appears to substantially enhance and prolong antigen‐specific immunity for achieving long‐term protection [29, 31]. The antigen release from PLG microparticles is controlled by the degradation rate of PLG copolymer, which is largely due to the ratio of lactide to glycolide of PLG polymer, the molecular weight, and hydrophilicity of PLG polymer as well as the characteristics of PLG microparticles such as the morphology, size, and encapsulation efficiency [38]. The sustained antigen release of antigen‐loaded PLG microparticles have been applied in the development of various potent microparticle vaccines [29, 31]. In addition, antigen‐loaded PLG microparticles capable of sustaining release of an antigen also show potential for being designed as a single‐dose vaccine without the need for booster doses [37, 39]. However, as some sophisticated events, including enhancement of protein load in PLG microparticles as well as optimization and stabilization of protein release are involved in the design of a single‐dose vaccine [40], the feasibility needs to be assessed in future studies.
The microparticles based on biodegradable PLG polymers can be prepared by number of methods, such as spray drying, double emulsion, and phase separation‐coacervation [30]. However, the most widely used technique for preparation of protein‐loaded microparticles is the double emulsion method [30].
The protein is encapsulated in 50:50 poly(lactide‐co‐glycolide) microparticles using the double emulsion method as described previously [41, 42], with minor modifications [22–24]. In the process, PLG polymer is first dissolved in an organic solvent. The organic solvent dichloromethane is mainly used to dissolve PLG polymer. Protein in aqueous solvent is then emulsified with nonmiscible organic solution of PLG polymer by high speed homogenization or sonication to produce a water/oil emulsion. The resulting emulsion is further transferred to a solution of polyvinyl alcohol, which is used as a stabilizer. Again homogenization or intensive stirring is necessary to generate a double emulsion of water/oil/water. The water/oil/water emulsion is then stirred for 18 h at room temperature (RT) and pressurized to promote solvent evaporation and microparticle formation in a laboratory fume hood. Solvent extraction can also be undertaken yielding microparticles containing protein. The microparticles are collected by centrifugation and washed with distilled water to remove nonentrapped protein.
Based on previous studies, proteins used for PLG encapsulation can be scaled down by using the water/oil/water double emulsion method [30]. In addition, this method also results in high microparticle yields and encapsulation efficiencies [30]. However, there is still a potential concern of antigen denaturation due to organic solvent exposure during the encapsulation process [41, 42], although numerous proteins have been successfully entrapped in PLG microparticles without loss of structural integrity, immunogenicity, or bioactivity [25, 30]. Especially, antigenicity retention following the process of double emulsion method is a critical event to subsequently initiate effective immunity by vaccinating antigen‐loaded microparticles [30].
Development efforts of subunit vaccines against T. gondii in our laboratory have been focused mainly on the major immunodominant SAGs of tachyzoites [22–24, 43, 44], the rapidly multiplying stage during the acute phase infection. Furthermore, SAG1 and SAG2 proteins have been identified as two major tachyzoite SAGs in the previous study [45]. These two proteins are involved in the process of host cell invasion [46] and can induce anti Toxoplasma immune responses [6]. Therefore, both SAG1 and SAG2 can be considered as potential candidate antigens for Toxoplasma vaccine development. SAG1 gene, SAG2 gene, and a hybrid gene consisting of SAG1 and SAG2 sequences had been, respectively, cloned in our previous work to produce recombinant SAG1 (rSAG1) protein [22, 43], recombinant SAG2 (rSAG2) protein [23, 43], and a recombinant chimeric protein, rSAG1/2 [24, 43]. Further animal studies in mice demonstrated that rSAG1, rSAG2, or rSAG1/2 emulsified with an oil adjuvant, Vet L‐10, induced partial protection against a lethal subcutaneous challenge of T. gondii tachyzoites [43]. If alternative effective adjuvants, such as the PLG polymer are used to make these recombinant proteins more immunogenic, more protective immunity against T. gondii may be achieved in animals.
In our recent work, rSAG1, rSAG2, or rSAG1/2 was then, respectively, encapsulated with the PLG polymer by using the double emulsion method for production of PLG‐encapsulated rSAG1 (PLG‐rSAG1) [22], PLG‐encapsulated rSAG2 (PLG‐rSAG2) [23], or PLG‐encapsulated rSAG1/2 (PLG‐rSAG1/2) microparticles [24]. Some microparticle characteristics, such as size (diameter), microparticle morphology, protein entrapment, and in vitro release were analyzed after PLG encapsulation (Tables 1 and 2). The morphological studies based on scanning electron microscopy showed that these microparticles are uniform population of spherical particles with a smooth surface. In addition, particle sizes of all three PLG microparticles in diameter were smaller than 10 μm (Table 1). Thus, the three PLG microparticles have an appropriate feature for direct uptake by APCs, such as macrophages and dendritic cells.
Microparticle | Mean particle size (μm) | Entrapment efficiency (%) | Reference |
---|---|---|---|
PLG‐rSAG1 | 4.25–6.58 | 69–81 | [22] |
PLG‐rSAG2 | 2.14–3.63 | 74–80 | [23] |
PLG‐rSAG1/2 | 1.27–1.65 | 72–83 | [24] |
Particle size and entrapment efficiency of PLG‐rSAG microparticles.
Microparticle | Release protein | Release period | Release profile | Reference |
---|---|---|---|---|
PLG‐rSAG1 | 87.8% rSAG1 | 35 days | Three phases | [22] |
PLG‐rSAG2 | 88.3% rSAG2 | 33 days | Three phases | [23] |
PLG‐rSAG1/2 | 88.5% rSAG1/2 | 56 days | Three phases | [24] |
Release of rSAG from PLG microparticles.
More importantly, the release of rSAG1, rSAG2, or rSAG1/2 from PLG microparticles was also analyzed (Table 2). We found that the in vitro cumulative release of rSAG1, rSAG2, and rSAG1/2 from PLG microparticles suspended in phosphate buffered saline (PBS) could be, respectively, sustained for 35, 33, and 56 days with three distinct phases consisting of an initial burst release, a very slow release, and a final rapid release (Table 2). Actually, based on previous critical investigations, such three‐phase fluctuation in antigen release from PLG microparticles is due to the initial rapid diffusion of coated antigen on the PLG microparticle surface, the very slow and gradual diffusion of encapsulated antigen, and the final rapid diffusion of antigen because of the PLG microparticle degradation [47–49]. Furthermore, in the triphasic antigen release profile, both initial and final rapid release of entrapped antigen, respectively, look like priming and boosting doses usually employed in a conventional immunization procedure [49]. Thus, vaccination with a single dose of PLG‐rSAG microparticles that are able to fulfill the triphasic rSAG release may be thought of as treating with two doses of rSAG protein. However, further improvements such as enhancement of protein load in PLG microparticles, as well as, optimization and stabilization of protein release are needed to evaluate the feasibility [40]. On the other hand, Western blotting assay with use of mouse monoclonal antibodies specific to tachyzoite SAGs demonstrated that released rSAG proteins from PLG microparticles still retained the original SAG antigenicity during the release from PLG microparticles [22–24]. These data indicate that both the encapsulation procedure and release from microparticles in our previous work are not detrimental to the antigenicity of rSAG. Thus, rSAG proteins have been successfully encapsulated with PLG polymers by the double emulsion method and the resulting PLG‐rSAG microparticles not only properly preserved the SAG’s antigenicity, but also sustained the controlled, stable release of the antigenic rSAG proteins from PLG microparticles. Based on these data, therefore, released rSAG proteins from PLG microparticles have the potential to induce anti SAG immune responses.
Although different adjuvants capable of improving immune responses and protection against T. gondii have been studied [6, 50], the biodegradable and biocompatible PLG polymers are so far seldom used as potent adjuvants for Toxoplasma vaccine development. Stanley and his coauthors first employed the double emulsion method to produce PLG‐encapsulated microparticle vaccine against T. gondii [51]. In the same study, the PLG microparticle vaccine containing a tachyzoite extract plus a mucosal adjuvant, cholera toxin, failed to provide protection in sheep [51]. The unexpected protection in sheep indicates that more effort is therefore needed to improve not only the stability of encapsulated Toxoplasma antigens but also the immune responses and protection they induce in animals.
On the other hand, the adjuvant effects of the PLG encapsulation had been exercised to, respectively, prepare PLG‐rSAG1, PLG‐rSAG2, and PLG‐rSAG1/2 microparticles in our three previous studies [22–24]. The ability of these PLG‐rSAG microparticles to trigger protective immunity against T. gondii was subsequently evaluated in BALB/c mice by vaccination through the intraperitoneal route. Results showed that both PLG‐rSAG1 and PLG‐rSAG1/2 microparticles effectively induced not only significant long‐lasting (10 weeks) specific humoral and cell‐mediated immune responses, accompanied by secretion of a large amount of IFN‐γ, but also high protection (80% for PLG‐rSAG1 microparticles and 83% for PLG‐rSAG1/2 microparticles) against T. gondii tachyzoite infection [22, 24]. However, PLG‐rSAG2 microparticles could induce sustained (10 weeks) lymphocyte proliferation and IFN‐γ production [23]. Furthermore, after a lethal subcutaneous challenge of 1 × 104T. gondii tachyzoites (RH strain), PLG‐rSAG2 microparticles also improved anti Toxoplasma protection (87%) [23], which is higher, though not statistically significant, than either 80% of PLG‐rSAG1 microparticles [22] or 83% of PLG‐rSAG1/2 microparticles [24].
As T. gondii is an obligate intracellular parasite, protective immunity to T. gondii is largely mediated by Th1 cell‐mediated immunity [6, 7]. Previous studies have shown that induction of both lymphocyte proliferation and IFN‐γ production (one of Th1‐type cytokines) positively correlates with protective Th1 cell‐mediated immunity against T. gondii [43, 44, 51]. In addition, IFN‐γ has been demonstrated to be a critical mediator that has to be secreted for as long as possible in order to maintain anti Toxoplasma immunity [52, 53]. We found that sustained lymphocyte proliferation and significant IFN‐γ production readily detected in mice immunized with PLG‐rSAG microparticles in our previous studies [22–24]. These findings indicate that immunization with PLG‐rSAG microparticles really elicits the IFN‐γ‐associated Th1 cell‐mediated immunity, which is the expected response that we aimed to induce in mice.
Based on previous studies, PLG microparticles appear to favorably facilitate a size‐dependent interaction with APCs, such as macrophages and dendritic cells [32–34]. The particles, like PLG‐rSAG microparticles prepared in our previous studies (Table 1), smaller than 10 μm in diameter are directly taken by APCs [32]. Based on our previous results, the proper size range thus could stimulate peritoneal macrophages to facilitate the uptake of these PLG‐rSAG microparticles administered in the mouse peritoneal cavity [22–24]. Therefore, the microparticle‐containing macrophages in the peritoneal cavity then traveled to other lymphoid compartments, including the spleen, and effectively presented SAG epitopes to Th1 and Tc; thereby, inducing strong SAG‐specific Th1 cell‐mediated immunity to protect mice from the tachyzoite challenge. Our previous studies [22–24] and those recorded by others [32–34] have shown that facilitation of uptake and delivery of PLG‐rSAG microparticles by macrophages can lead to more effective antigen processing and presentation to T lymphocytes capable of inducting cell‐mediated immunity. Thus, the high survival rates in mice have demonstrated that PLG‐rSAG microparticles effectively elicit protective Th1 cell‐mediated immunity to remove tachyzoite‐infected cells for limiting parasite dissemination during the experimental tachyzoite challenge [7].
In addition to Th1‐dependent cell‐mediated immunity, in our previous studies, high titers of anti Toxoplasma IgG in mouse sera elicited by PLG‐rSAG microparticles have indicated that systemic humoral immunity mediated by Th2 may participate in the prevention of T. gondii infection [54, 55]. However, further measurements by the dye test are still needed to assay these antibodies to elucidate their functional lytic activities. Therefore, peritoneal vaccination of mice with PLG‐rSAG microparticles may generate mixed Th1/Th2 immunity against T. gondii.
PLG polymers are the primary candidates for the development of microparticle vaccines [25]. The rSAG proteins (rSAG1, rSAG2, and rSAG1/2) prepared in our laboratory have been successfully encapsulated with PLG polymers to generate PLG‐rSAG microparticles capable of sustaining long‐term stable release of antigenic rSAG proteins. Moreover, following peritoneal immunization in mice, PLG‐rSAG microparticles induce not only long‐term (10 weeks) SAG‐specific humoral and cell‐mediated immune responses, but also high protection against a lethal challenge of T. gondii tachyzoites [22–24]. Our studies provide a valuable basis for developing long‐lasting vaccines against T. gondii for future use in humans and animals. Our experimental data indicate that the encapsulation procedure we used for production of PLG‐rSAG microparticles is feasible at the laboratory level. However, this procedure have never been used to try mass production of PLG‐rSAG microparticles. More effort is therefore needed to evaluate the optimized encapsulation conditions used to fulfill the need for mass production [40].
The PLG‐rSAG microparticles we prepared previously could allow the sustained and extended release of rSAG proteins over a long period. Such long‐term release of rSAG proteins could repeatedly stimulate the immune effector cells to maintain enhanced immunity following immunization with PLG‐rSAG microparticles [29, 37]. However, the triphasic rSAG release detected in the cumulative release assay we carried out in the previous studies was done in vitro in PBS and; therefore, may not completely reflect in vivo release in mice [22–24]. Further studies are therefore needed to confirm the critical effect of triphasic rSAG release on in vivo anti Toxoplasma immune responses.
One adjuvant effect acted by PLG microparticle vaccines is to facilitate antigen uptake via APCs [25, 32, 33]. Different APCs populated in various administrating routes are able to perform the uptake of antigen‐loaded PLG microparticles and then process and present the epitopes of PLG‐encapsulated antigen on the major histocompatibility (MHC) molecules [32]. Therefore, different routes of delivery of antigen‐loaded PLG microparticles give rise to different vaccine efficacy in animals [32]. The mouse protective immunity induced by intraperitoneally administered PLG‐rSAG microparticles protected mice from a lethal subcutaneous challenge of T. gondii tachyzoites. However, such intraperitoneal administration of the microparticle vaccine appears to be inappropriate for use in large animals such as sheep or swine. In order to corroborate the conclusions drawn from the mouse model, more studies are needed to evaluate the proper route for administration of PLG‐rSAG microparticles in target animals. In addition, due to the natural infection initiated by ingesting oocysts released in cat feces or consuming meat from infected animals containing the long‐lived tissue cysts, future experiments will also be necessary to assess whether mucosal administration (oral or nasal route) of PLG‐rSAG microparticles protects these animals from an oral challenge of oocysts or tissue cysts of T. gondii.
The rapid growth of global population as well as industrialization has led to a concomitant increase in environmental pollution. This has very negative effects on natural elements that are vital for life on earth such as air and water. It becomes very crucial therefore to find sustainable ways to mitigate pollution in order to provide a clean and safe environment for humans. Photocatalysis has attracted worldwide interest due to its potential to use solar energy not only to solve environmental problems but also provide a renewable and sustainable energy source. An efficient photocatalyst converts solar energy into chemical energy which can be used for environmental and energy applications such as water treatment, air purification, self-cleaning surfaces, hydrogen production by water cleavage and CO2 conversion to hydrocarbon fuels.
\nResearch in the development of efficient photocatalytic materials has seen significant progress in the last 2 decades with a large number of research papers published every year. Improvements in the performance of photocatalytic materials have been largely correlated with advances in nanotechnology. Of many materials that have been studied for photocatalysis, titanium dioxide (TiO2; titania) has been extensively researched because it possesses may merits such as high photocatalytic activity, excellent physical and chemical stability, low cost, non-corrosive, nontoxicity and high availability [1, 2, 3, 4]. The photocatalytic activity of titania depends on its phase. It exists in three crystalline phases; the anatase, rutile and brookite. The anatase phase is metastable and has a higher photocatalytic activity, while the rutile phase is more chemically stable but less active. Some titania with a mixture of both anatase and rutile phases exhibit higher activities compared to pure anatase and rutile phases [5, 6, 7]. When titania is irradiated with light of sufficient energy, electrons from the valence band are promoted to the conduction band, leaving an electron deficiency or hole, h+, in the valence band and an excess of negative charge in the conduction band. The free electrons in the conduction band are good reducing agents while the resultant holes in the valence band are strong oxidizing agents and can both participate in redox reactions.
\nTitania however suffers from a number of drawbacks that limit its practical applications in photocatalysis. Firstly, the photogenerated electrons and holes coexist in the titania particle and the probability of their recombination is high. This leads to low rates of the desired chemical transformations with respect to the absorbed light energy [8, 9]. The relatively large band gap energy (~ 3.2 eV) requires ultraviolet light for photoactivation, resulting in a very low efficiency in utilizing solar light. UV light accounts for only about 5% of the solar spectrum compared to visible light (45%) [1, 10]. In addition to these, because titania is non-porous and has a polar surface, it exhibits low absorption ability for non-polar organic pollutants [10, 11, 12, 13]. There is also the challenge to recover nano-sized titania particles from treated water in regards to both economic and safety concern [14]. The TiO2 nanoparticles also suffer from aggregation and agglomeration which affect the photoactivity as well as light absorption [15, 16, 17, 18]. Several strategies have been employed in the open literature to overcome these drawbacks. These strategies aim at extending the wavelength of photoactivation of TiO2 into the visible region of the spectrum thereby increasing the utilization of solar energy; preventing the electron/hole pair recombination and thus allowing more charge carriers to successfully diffuse to the surface; increasing the absorption affinity of TiO2 towards organic pollutants as well as preventing the aggregation and agglomeration of the nano-titania particles while easing their recovery from treated water. Several reviews have been published in recent years on the development of strategies to eliminate the limitations of titania photocatalysis [1, 19, 20, 21, 22, 23, 24, 25]. Most of these however focus on pollutant removal from wastewater, water splitting for hydrogen production, CO2 conversion and reaction mechanisms [1, 21, 25, 26, 27, 28, 29, 30, 31]. In this chapter, we review some of the latest publications mainly covering the last 5 years, on strategies that have been researched to overcome the limitations of TiO2 for general photocatalytic applications and the level of success that these strategies have been able to achieve. Based on the current level of research in this field, we also present some perspectives on the future of modified TiO2 photocatalysis.
\nA large number of research works have been published on TiO2 modification to enhance its photocatalytic properties. These modifications have been done in many different ways which include metal and non-metal doping, dye sensitization, surface modification, fabrication of composites with other materials and immobilization and stabilization on support structures. The properties of modified TiO2 are always intrinsically different from the pure TiO2 with regards to light absorption, charge separation, adsorption of organic pollutants, stabilization of the TiO2 particles and ease of separation of TiO2 particles.
\nMetal doping has been extensively used to advance efforts at developing modified TiO2 photocatalysts to operate efficiently under visible light. The photoactivity of metal-doped TiO2 photocatalysts depends to a large extent on the nature of the dopant ion and its nature, its level, the method used in the doping, the type of TiO2 used as well as the reaction for which the catalyst is used and the reaction conditions [32]. The mechanism of the lowering of the band gap energy of TiO2 with metal doping is shown in Figure 1. It is believed that doping TiO2 with metals results in an overlap of the Ti 3d orbitals with the d levels of the metals causing a shift in the absorption spectrum to longer wavelengths which in turn favours the use of visible light to photoactivate the TiO2.
\nBand-gap lowering mechanism of metal-doped TiO2.
Doping of TiO2 nanoparticles with Li, Na, Mg, Fe and Co by high energy ball milling with the metal nitrates was found to widen the TiO2 visible light response range. In the Na-doped sample, Ti existed as both Ti4+ and Ti3+ and the conversion between Ti4+ and Ti3+ was found to prevent the recombination of electrons and (e−) and holes (h+). The metal ion doping promoted crystal phase transformations that generated electrons (e−) and holes (h+) [33]. Mesoporous TiO2 prepared by sol gel technique and doped with different levels of Pt (1–5 wt% nominal loading) resulted in a high surface area TiO2 with an enhanced catalytic performance in photocatalytic water splitting for the Pt-doped samples. The 2.5 wt%Pt-TiO2 had showed the optimum catalytic performance and a reduction in the TiO2 band gap energy from 3.00 to 2.34 eV with an enhanced electron storage capacity, leading to a minimization of the electron-hole recombination rate [34]. Noble metal nanoparticles such as Ag [35], Pt [34], Pd [36], Rh [37] and Au [38] have also been used to modify TiO2 for photocatalysis and have been reported to efficiently hinder electron-hole recombination due to the resulting Schottky barrier at the metal-TiO2 interface. The noble metal nanoparticles act as a mediator in storing and transporting photogenerated electrons from the surface of TiO2 to an acceptor. The photocatalytic activity increases as the charge carriers recombination rate is decreased.
\nIn a recent review by Low et al. [21] the deposition of Au onto TiO2 surface is reported to result in electron transfer from photo-excited Au particles (> 420 nm) to the conduction band of TiO2, which showed a decrease in their absorption band (∼550 nm) and the band was recovered by the addition of electron donors such as Fe2+ and alcohols. Zhang et al. [39] reported that the visible light activity of coupled Au/TiO2 can be ascribed to the electric field enhancement near the metal nanoparticles. Moreover, numerous researchers coupled Au and Ag nanoparticles onto TiO2 surface to use their properties of localized surface plasmonic resonance (LSPR) in photocatalysis [40]. Wang et al. [41] and Hu et al. [42] reported an improved photocatalytic performance due to the Pt nanoparticle which increased the electron transfer rate to the oxidant. It was observed that photocatalytic sacrificial hydrogen generation was influenced by several parameters such as platinum loading (wt%) on TiO2, solution pH, and light (UV, visible and solar) intensities [43]. Moreover, complete discoloration and dye mineralization were achieved using Pt/TiO2 as catalyst; the results were attributed to the higher Pt content of the photocatalyst prepared with the highest deposition time. For Pt-TiO2 catalysts the best discoloration and dye mineralization were obtained over the catalyst prepared by photochemical deposition method and using 120 min of deposition time in the synthesis. These results may be due to the higher Pt content of the photocatalyst prepared with the highest deposition time.
\nHaung et al. [44] prepared Pt/TiO2 nanoparticles from TiO2 prepared at various hydrolysis pH values and found that the phase of TiO2 obtained depended largely on the hydrolysis pH. The anatase/rutile intersection of a Pt/TiO2 sample had a lower recombination rate compared to the anatase phase of Pt/TiO2 due to the longer recombination pathway. Though, the Pt/TiO2 anatase phase showed better degradation efficiency than the Pt/TiO2 anatase/rutile intersection. The decrease in the anatase composition of TiO2, and the decrease in the composition of TiO2 resulted in the degradation rate decrease, suggesting that anatase composition in the Pt/TiO2 system played a crucial role of increasing the photocatalytic degradation of Acid Red 1 dye.
\nLiu et al. [45] prepared the palladium doped TiO2 (Pd-TiO2) photocatalyst using chemical reduction method and tested it the photocatalytic degradation of organic pollutant. It was found that the TiO2 grain size was reduced while the specific surface area increased and the absorption of ultraviolet light also enhanced after using chemical reduction method, however, all these changes had no effect on degradation of organic pollutant. But the degradation was significantly improved due to the deposition of Pd nanoparticles; the Pd/TiO2 organic pollutant degradation was 7.3 times higher compared to TiO2 (P25).
\nRepouse et al. [46] prepared a series of noble metal promoted TiO2 (P25) by wet impregnation and found that the dispersion of the small metal crystallites on TiO2 did not affect the optical band gap of TiO2. The Pt-promoted catalyst exhibited the highest photocatalytic efficiency in the degradation of bisphenol A under solar irradiation. They also found the presence of humic acid to considerably improve the reaction rate of Rh/TiO2 but had a clearly adverse effect with P25 TiO2 photocatalyst. Fluorescence data revealed that humic acid is capable of photosensitizing the Rh/TiO2 catalyst.
\nIndium-doped TiO2 have recently been used for photocatalytic reduction of CO2 [47]. Indium doping resulted in an increase in surface area because of suppression of TiO2 particle growth during the TiO2 synthesis. The light absorption ability of the In-TiO2 was enhanced due to the introduction of the impurity level below the conduction band level of the TiO2. The photocatalytic CO2 reduction activity of the In-TiO2 was about 8 time that of pure TiO2 as a consequence of the high surface area and extended light absorption range.
\nThe doping of TiO2 with transition metals such as Cr [48], Co [48], Fe [48, 49, 50], Ni [48, 51], Mn [48, 52], V [53], Cu [54], Ni [51] and Zn [55], has been studied by different research groups. Numerous studies reported that doping of TiO2 with transition metals improve the photocatalytic activity, attributable to a change in the electronic structure resulting in the absorption region being shifted from UV to visible light. The shift results from charge-transfer transition between the d electrons of the transition metals and the conduct or valence band of TiO2 nanoparticles. Inturi et al. [48] compared the doping of TiO2 nanoparticles with Cr, Fe, V, Mn, Mo, Ce, Co, Cu, Ni, Y and Zr and it was found that Cr, Fe and V showed improved conversions in the visible region while, the incorporation of the other transition metals (Mn, Mo, Ce, Co, Cu, Ni, Y and Zr) exhibited an inhibition effect on the photocatalytic activity. The Cr-doped TiO2 demonstrated a superior catalytic performance and the rate constant was found to be approximately 8–19 times higher than the rest of the metal doped catalysts. It was reported that the reduction peaks in Cr-doped TiO2 shifted to much lower temperatures, due to the increase in the reduction potential of titania and chromium. Therefore, the higher photocatalytic efficiency of Cr/TiO2 in the visible light can be attributed to strong interaction (formation of Cr-O-Ti bonds). Fe-doped TiO2 nanoparticles were used in the visible light degradation of para-nitrophenol and it was found that the Fe-dopant concentration was crucially important in determining the activity of the catalyst. The maximum degradation rate of para-nitrophenol observed was 92% in 5 h when the Fe(3+) molar concentration was 0.05 mol%, without addition of any oxidizing reagents. The excellent photocatalytic activity was as a result of an increase in the threshold wavelength response as well as maximum separation of photogenerated charge carriers [49]. On the other hand, Fe-doped TiO2 evaluated for solar photocatalytic activity for the degradation of humic acid showed a retardation effect for the doped catalysts compared to the bare TiO2 specimens, which could be attributed to surface complexation reactions rather than the reactions taking place in aqueous medium. The faster removal rates attained by using bare TiO2 could be regarded as substrate specific rather than being related to the inefficient visible light activated catalytic performance [50]. Ola et al. [56] reported that the properties of V doped TiO2 were tuned towards visible light because of the substitution of the Ti4+ by V4+ or V5+ ions since the V4+ is centred at 770 nm while the absorption band of V5+ is lower than 570 nm. Moradi et al. [57] obtained high photocatalytic activity of Fe doped TiO2 and studied the effects of Fe3+ doping content on the band gap and size of the nanoparticles. It was found that the increase in the doping content decreased the band gap energy and particle size from 3.3 eV and 13 nm for bare TiO2 to 2.9 eV and 5 nm for Fe10-TiO2, respectively.
\nThe rare earth metals doped TiO2 catalyst also have good electron trapping properties which can result in a stronger absorption edge shift towards longer wavelength, obtaining narrow band gap. Bethanabotla et al. [58] carried out a comprehensive study on the rare earth doping into a TiO2 and found that the rare earth dopants improved the aqueous-phase photodegradation of phenol at low loadings under simulated solar irradiation, with improvements varying by catalyst composition. Differences in defect chemistry on key kinetic steps were given as the explanation for the enhanced performance of the rare earth doped samples compared to pure titania. Reszczyńska et al. [59] prepared a series of Y3+, Pr3+, Er3+ and Eu3+ modified TiO2 nanoparticles photocatalysts and results demonstrate that the incorporation of RE3+ ions into TiO2 nanoparticles resulted in blue shift of absorption edges of TiO2 nanoparticles and could be ascribed to movement of conduction band edge above the first excited state of RE3+. Moreover, incorporated RE3+ ions at the first excited state interact with the electrons of the conduction band of TiO2, resulting in a higher energy transfer from the TiO2 to RE3+ ions. But observed blue shift could be also attributed to decrease in crystallite size of RE3+–TiO2 in comparison to TiO2. The Y3+, Pr3+, Er3+ and Eu3+ modified TiO2 nanoparticles exhibited higher activity under visible light irradiation compared to pure P25 TiO2 and can be excited under visible light in the range from 420 to 450 nm. In a similar work on rare earths (Er, Yb, Ho, Tb, Gd and Pr) titania nanotubes (RE-NTs), [60] the RE3+ species were found to be located at the crystal boundaries rather than inside the TiO2 unit cell and an observed excitation into the TiO2 absorption band with resulting RE3+ emission confirmed energy migration between the TiO2 matrix and RE3+. The presence of the rare earth component was found to reduce recombination of the electrons and holes successfully by catching them and also by promoting their rapid development along the surface of TiO2 nanoparticles. Lanthanide ions doping did not impact the energy gap of TiO2 nanoparticles, however this enhanced the light absorption of catalyst. The surface range of TiO2 nanoparticles generally increases by La3+ particle doping by diminishing the crystallite size and accordingly, the doped TiO2 nanoparticle displayed higher adsorption capacity. Based on theoretical calculations, it was proposed that during the electrochemical process, new Ho-f states and surface vacancies were formed and may reduce the photon excitation energy from the valence to the conduction band under visible light irradiation. The photocatalytic activity under visible light irradiation was attributed not to ·OH but to other forms of reactive oxygen species (O2·−, HO2, H2O2).
\nTiO2 nanoparticles have been comprehensively doped at the O sites with non-metals such as C [61], B [62], I [63], F [64], S [65], and N [66]. Non-metal dopants are reported to be more appropriate for the extension of the photocatalytic activity of TiO2 into visible region compared to metal dopant [67, 68]. This can be ascribed to the impurity states which are near the valence band edge, however, they do not act as charge carriers, and their role as recombination centres might be minimized [53]. As shown in Figure 2, the mixing of the p states of the doped non-metal with the O2p states shifts the valence band edge upward and narrows the band-gap energy of the doped TiO2 photocatalyst. The nitrogen and carbon doped TiO2 nanoparticles has been reported to exhibit greater photocatalytic activity under visible light irradiation compared to other non-metal dopants.
\nBand-gap energy narrowing mechanism for non-metal-doped TiO2.
N-doped TiO2 (N-TiO2) appears to be the most efficient and extensively investigated photocatalyst for non-metal doping. Zeng et al. [69] reported the preparation of a highly active modified N-TiO2 nanoparticle via a novel modular calcination method. The excellent photocatalytic performance of the photocatalyst was ascribed to excellent crystallinity, strong light harvesting and fast separation of photogenerated carriers. Moreover, the enhancement of charge separation was attributed to the formation of paramagnetic [O-Ti4+-N2−-Ti4+-VO] cluster. The surface oxygen vacancy induced by vacuum treatment trapped electron and promoted to generate super oxygen anion radical which was a necessary active species in photocatalytic process. Phongamwong et al. [70] investigated the photocatalytic activity of CO2 reduction under visible light over modified N-TiO2 photocatalyst and they have found that the band gap of N-TiO2 photocatalyst slightly decreases with increasing N content. In addition, the sub-band energies related to the impurity energy level were observed in the N-TiO2 photocatalyst because of the interstitial N species and the sub-band gap energies were found to have decreased from 2.18 eV with 10 wt% N-TiO2 photocatalyst. In contrast, the replacement of O by N is difficult because of the radius of N (17.1 nm) being higher compared to O (14 nm) and the electroneutrality can be maintained by oxygen vacancies, that are provided by replacement of three oxygen vacancies by two nitrogen atom [71]. N-TiO2 photocatalyst reduces the oxygen energy vacancies from 4.2 to 0.6 eV, suggesting that N favors the formation of oxygen vacancies [72].
\nIn contrast, O atoms (14 nm) could be substituted easily by F atoms (13.3 nm) because of their similar ionic radius [73]. Yu et al. [64] reported that the F-doped TiO2 (F-TiO2) is able to absorb visible light due to the high-density states that were evaluated to be below the maxima valence band, although there was no shift in the band edge of TiO2. Samsudin et al. found a synergistic effect between fluorine and hydrogen in hydrogenated F-doped TiO2 which enabled light absorption in UV, visible and infrared light illumination with enhanced electrons and holes separation. Surface vacancies and Ti3+ centres of the hydrogenated F-doped catalyst coupled with enhanced surface hydrophilicity facilitated the production of surface-bound and free hydroxyl radicals. Species present on the surface of the catalyst triggered the formation of new Ti3+ occupied states under the conduction band of the hydrogenated F-doped TiO2, thus narrowing the band gap energy [73]. Enhanced photocatalytic performance of N-doped TiO2 over pure TiO2 has also been ascribed to efficient separation of electron-hole pairs as well as an increased creation of surface radicals such as hydroxyl The band gap can also be narrowed by doping TiO2 with S, since replacement of S into TiO2 can be performed easily due to larger radius of S atoms (18 nm) compared to O atoms (14 nm). S incorporation in TiO2 has been reported to change the lattice spacing of the TiO2 with a reduction in the band gap width from 3.2 to 1.7 eV allowing for higher photocatalytic activity [74]. N, S and C co-doped TiO2 samples photocatalytic reduction of Cr(IV) showed that the co-doping and calcination played an important role in the microstructure and photocatalytic activity of the catalysts. The co-doped samples calcined at 500°C showed the highest activities ascribed to the synergistic effect in enhancing crystallization of anatase and (N, S and C) co-doping. The carbon doped TiO2 (C-TiO2) is reported to be more active than N-TiO2, therefore, C-TiO2 has received special attention [75]. Noorimotlagh et al. [76] investigated the photocatalytic removal of nonylphenol (NP) compound using visible light active C-TiO2 with anatase/rutile. It was found that the doping of C into TiO2 lattice may enhance the visible light utilization and affect the structural properties of the as-synthesized photocatalysts. Moreover, it was reported that after C doping and changing the calcination temperature, the band gap was narrowed from 3.17 to 2.72 eV and from 2.72 to 2.66 eV, respectively. Ji et al. [61] reported the preparation of C-TiO2 with a diameter of around 200 nm and the tube wall was composed of anatase TiO2, amorphous carbon, crystalline carbon and carbon element doping into the lattice of TiO2. The C-TiO2 nanotubes exhibited much better performance in photocatalytic activity than bare TiO2 under UV and visible light. The obtained results were ascribed to the C doping, which narrowed the band gap energy of TiO2, extended the visible light adsorption toward longer wavelength and hindered charge recombination.
\nAlthough single metal doped and non-metal doped TiO2 have exhibited excellent performance in decreasing the electrons and holes recombination, but they suffer from thermal stability and losing a number of dopants during catalyst preparation process [77]. Therefore, co-doping of two kinds of atoms into TiO2 has recently attracted much interest [78]. The electronic structure of TiO2 can be altered by co-doping on TiO2 by formation of new doping levels inside its band gap. Abdullah et al. [77] reported that the doping levels situated within the band gap of TiO2 can either accept photogenerated electrons from TiO2 valence band or absorb photons with longer wavelengths. Therefore, suggesting that the TiO2 absorption range can be expanded.
\nZang et al. [79] evaluated the photocatalytic degradation of atrazine under UV and visible light irradiation by N,F-codoped TiO2 nanowires and nanoparticles in aqueous phase. It was found that photocatalytic degradation of atrazine was higher in the presence of N,F-codoped TiO2 nanowires than that of N,F-codoped TiO2 nanoparticles. The higher photocatalytic performance in the presence of N,F-codoped TiO2 nanowires was attributed to the higher charge carrier mobility and lower carrier recombination rate. Moreover, the speed of electron diffusion across nanoparticle intersections is several orders of magnitude smaller compared to that of nanowire because of frequent electron trapping at the intersections of nanoparticles and increasing the recombination of separated charges before they reach the TiO2 nanoparticles surface. Park et al. [80] showed the best performance for novel Cu/N-doped TiO2 photoelectrodes for dye-sensitized solar cells. It was found that the Cu/N-doped TiO2 nanoparticles provided higher surface area, active charge transfer and decreased charge recombination. Moreover, the addition of suitable content of Cu- to N-doped TiO2 electrode effectively inhibited the growth of TiO2 nanoparticles and improved the optical response of the photoelectrode under visible light irradiation. Chatzitakis et al. [81] studied the photoelectrochemical properties of C, N, F codoped TiO2 nanotubes. It was found that increasing surface area is not followed by increase in the photoconversion efficiency, but rather that an optimal balance between electroactive surface area and charge carrier concentration occurs.
\nZhao et al. [82] investigated the photocatalytic H2 evolution performance of Ir-C-N tridoped TiO2 under UV-visible light irradiation. The photocatalytic activity of TiO2 nanoparticles was reported to be improved by Ir-C-N tridoped TiO2 under UV-visible light, due the synergistic effect between Ir, C and N on the electron structure of TiO2. It was found that Ir existed as Ir4+ by substituting Ti in the lattice of TiO2 nanoparticles, whereas the C and N were also incorporated into the surface of TiO2 nanoparticles in interstitial mode. The absorption of TiO2 nanoparticles was expanded into the visible light region and the band gap was narrowed to ~3.0 eV, resulting in improved photocatalytic H2 evolution under UV-visible light irradiation. Tan et al. [83] investigated the photocatalytic degradation of methylene blue by W–Bi–S-tridoped TiO2 nanoparticles. It was found that the absorption edge of TiO2 was expanded into visible-light region after doping with W, Bi and S and the catalytst showed the best photocatalytic activity, than that of TiO2, S-TiO2, W–S–TiO2 and Bi–S–TiO2. This might be attributed to the synergistic effect of W, Bi and S.
\nAmongst the various strategies that have been used to enhance TiO2 photocatalytic activity, improvement of morphology, crystal structure and surface area have also been considered important and widely investigated approach to achieve better photocatalytic performance. The nanotitania crystallinity can simply be enhanced by optimizing the annealing temperature. However, the stability of the structure and geometries have to be considered when annealing [84]. For the nanotitania morphology and surface area, various ordered structures have been studied. TiO2 nanotubes [85, 86], nanowires [79], nanospheres [87], etc. Tang et al. fabricated monodisperse mesoporous anatase TiO2 nanospheres using a template material and found the resulting catalysts to show high photocatalytic degradation efficiency and selectivity towards different target dye molecules and could be readily separated from a slurry system after photocatalytic reaction [87]. Anodic TiO2 nanotubes have been reported to allow a high control over the separation of photogenerated charge carriers in photocatalytic reactions. The nanotube array has as key advantage the fact that nanotube modifications can be embedded site specifically into the tube wall or at defined locations along the tube wall. This allows for engineering of reaction sites giving rise to enhanced photocatalytic efficiencies and selectivities [88].
\nThe design and preparation of graphene-based composites containing metal oxides and metal nanoparticles have attracted attention for photocatalytic performances. For example, Tan et al. [89] prepared a novel graphene oxide-doped-oxygen-rich TiO2 (GO–OTiO2) hybrid heterostructure and evaluated its activity for photoreduction of CO2 under the irradiation of low-power energy-saving daylight bulbs. It was found that the photostability of O2–TiO2 was significantly improved by the addition of GO, at which the resulting hybrid composite retained a high reactivity. The photoactivity attained was about 1.6 and 14.0 folds higher than that of bare O2–TiO2 and the commercial Degussa P25, respectively. This high photocatalytic performance of GO–OTiO2 was attributed to the synergistic effect of the visible-light-responsiveness of O2–TiO2 and an enhanced separation and transfer of photogenerated charge carriers at the intimate interface of GO–OTiO2 heterojunctions. This study is reported to have opened up new possibilities in the development of novel, next generation heterojunction photocatalysts for energy and environmental related applications. Lin et al. [90] also investigated photoreduction of CO2 with H2O vapor in the gas-phase under the irradiation of a Xe lamp using TiO2/nitrogen (N) doped reduced graphene oxide (TiO2/NrGO) nanocomposites. They found that the quantity and configuration of N dopant in the TiO2/NrGO nanocomposites strongly influenced the photocatalytic efficiency, and the highest catalytic activity was observed for TiO2/NrGO nanocomposites with the highest N doping content. Moreover, modified TiO2/rGO demonstrated a synergistic effect, enhancing CO2 adsorption on the catalyst surface and promoting photogenerated electron transfer that resulted in a higher CO2 photoreduction rate of TiO2/NrGO. Qu et al. [91] prepared the graphene quantum dots (GQDs) with high quantum yield (about 23.6% at an excitation wavelength of 320 nm) and GQDs/TiO2 nanotubes (GQDs/TiO2 nanoparticles) nanocomposites and the photocatalytic activity was tested towards the degradation of methyl orange. It was found that the GQDs deposited on TiO2 nanoparticles can expand the visible light absorption of TiO2 nanoparticles and enhance the activity on photocatalytic degradation of methyl orange under UV-vis light irradiation (ʎ = 380–780 nm). Furthermore, the photocatalytic activity of GQDs/TiO2 nanoparticles was approximately 2.7 times as higher than that of bare TiO2 nanoparticles. Tian et al. [92] reported the preparation of N, S co-doped graphene quantum dots (N, S-GQDs)-reduced graphene oxide- (rGO)-TiO2 nanotubes (TiO2NT) nanocomposites for photodegradation of methyl orange under visible light irradiation. It was found that the S-GQDs+rGO + TiO2 nanocomposites simultaneously showed an extended photoresponse range, improved charge separation and transportation properties. Moreover, the apparent rate constant of N, S-GQDs+rGO + TiO2NT is 1.8 and 16.3 times higher compared to rGO + TiO2NT and pure TiO2NT, respectively. Suggesting that GQDs can improve the utilization of solar light for energy conversion and environmental therapy.
\nAnother drawback of TiO2 nanoparticles mentioned above is the formation of uniform suspension in water which makes its recovery difficult, therefore hindering the application of photocatalytic in an industrial scale. As a result, many studies have attempted the modification of TiO2 nanoparticles on support materials such as clays [93, 94] quartz [95], stainless steel [96], etc. Clays have been reported to be a significant support material for TiO2 nanoparticles because of their layered morphology, chemical as well as mechanical stability, cation exchange capacity, non-toxic nature, low cost and availability. Therefore, TiO2/clay nanocomposites have attracted much attention for application in both water and air purification and have been prepared by numerous researchers. Belver et al. [97] investigated the removal of atrazine under solar light using a novel W-TiO2/clay photocatalysts. It was found that the photocatalytic activity of W-TiO2/clay catalyst exhibited higher photocatalytic performance than that of an un-doped TiO2/clay, which was explained by the presence of W ions in the TiO2 nanostructure. The substitution of Ti ions with W resulted in the increase of its crystal size and the distortion of its lattice and moderately narrower band gap of photocatalysts. Mishra et al. [98] reported the preparation of TiO2/clay nanocomposites for photocatalytic degradation of VOC and dye. They found that the photocatalytic performance of TiO2/clay nanocomposites is highly dependent on the clay texture (as 2:1 clays show highest activity than 1:1) apart from their surface area and porosity. Moreover, the reactions involving TiO2/Clay photocatalyst were fast with rate constant of 0.02886 and 0.04600 min−1 for dye and VOC respectively than the other nanocomposites.
\nIn this chapter, we have given an overview of the development of modified TiO2 catalysts and its future prospects from a scientific point of view. We note that the field has experienced major advances in the last 5 years especially in the area of modifying TiO2 with carbon nanomaterials. Based on the literature we have covered here, we believe that there is still quite a lot that can be achieved in improving the performance of TiO2 catalysts for photocatalytic applications.
\nThere are no conflicts of interest to declare.
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