Hydrothermal Synthesis of Visible Light Photocatalytic SIO2 - TIO2 Nanocomposites

Hydrothermal Synthesis of Visible Light Photocatalytic SIO2 - TIO2 Nanocomposites | Research Square window.SnipcartSettings = { analytics: { enabled: false } }; (function() { var accessVector = localStorage.getItem('access_vector') || ''; window.dataLayer = window.dataLayer || []; if (accessVector) { window.dataLayer.push({ user: { profile: { profileInfo: { snid: accessVector } } } }); } })(); (function(w,d,s,l,i){w[l]=w[l]||[];w[l].push({'gtm.start':new Date().getTime(),event:'gtm.js'});var f=d.getElementsByTagName(s)[0],j=d.createElement(s),dl=l!='dataLayer'?'&l='+l:'';j.async=true;j.src='https://www.googletagmanager.com/gtm.js?id='+i+dl;f.parentNode.insertBefore(j,f);})(window,document,'script','dataLayer','GTM-K279D39R'); Browse Preprints In Review Journals COVID-19 Preprints AJE Video Bytes Research Tools Research Promotion AJE Professional Editing AJE Rubriq About Preprint Platform In Review Editorial Policies Our Team Advisory Board Help Center Sign In Submit a Preprint Cite Share Download PDF Research Article Hydrothermal Synthesis of Visible Light Photocatalytic SIO2 - TIO2 Nanocomposites Oguzhan Avciata, Mustafa Borucu, Semih Gorduk This is a preprint; it has not been peer reviewed by a journal. https://doi.org/ 10.21203/rs.3.rs-6095977/v1 This work is licensed under a CC BY 4.0 License Status: Posted Version 1 posted You are reading this latest preprint version Abstract In this study, Silicon Dioxide (SiO 2 ) doped nano Titanium Dioxide (TiO 2 ) nanocomposites were prepared by hydrothermal method and under different reaction conditions. The reason for doping with nano SiO 2 is to ensure that nano TiO 2 gains photocatalytic activity in the visible region instead of showing photocatalytic properties only under ultraviolet (UV) light. The synthesis process was carried out by changing the nano SiO 2 percentage in order to compare the nanocomposite materials formed in the synthesis part of these photocatalysts in terms of structure and to customize the content. A total of 3 different SiO 2 –TiO 2 nanocomposites and anatase form of TiO 2 were successfully synthesized using the hydrothermal method. Nano SiO 2 ratios were synthesized in the total nano TiO 2 material as 100%, 50% and 10%, respectively. The structure of the obtained nanocomposite was elucidated by X-ray diffraction (XRD), Scanning Electron Microscopy (SEM), Energy Dispersive Spectroscopy (EDS), Ultraviolet-Visible Diffuse Reflectance Spectroscopy (UV-DRS) and Fourier Transform Infrared Spectroscopy (FT-IR) techniques. Studies on the degradation of organic pollutants of nanocomposite under visible light showed that the obtained nanocomposite exhibits photocatalytic activity under visible light. Additionally, unlike the studies in the literature, SiO 2 and TiO 2 were synthesized from raw materials in the same environment, and synthesis was not performed separately. Due to this feature, it is seen as a method that has less effort and can make a difference compared to previous studies, and that can affect future studies. Hydrothermal Photocatalysis Nanocomposite TiO2 SiO2 Figures Figure 1 Figure 2 Figure 3 Figure 4 Figure 5 Figure 6 Figure 7 Introduction In recent years, the progress in creating advanced materials with enhanced photocatalytic activity has received considerable interest because of their potential roles in environmental remediation, energy generation, and sustainability [ 1 , 2 ]. Among these materials, nanocomposites that combine distinct properties of different components offer a promising avenue for optimizing photocatalytic performance [ 3 , 4 ]. The combination of Silica (SiO 2 ) and Titanium dioxide (TiO 2 ) in nanocomposites has demonstrated the ability to harness visible light for photocatalysis, opening new possibilities for efficient utilization of solar energy and pollutant degradation [ 5 , 6 ]. Photocatalysis, a process where light-activated catalysts promote chemical reactions, has become a crucial approach for tackling environmental issues. Titanium dioxide (TiO 2 ), a widely studied photocatalyst, exhibits exceptional properties such as chemical stability, non-toxicity, and photocatalytic activity under ultraviolet (UV) light [ 7 , 8 ]. However, its practical application is limited by its inability to utilize visible light effectively, which constitutes a major portion of the solar spectrum [ 9 ]. To overcome this limitation, researchers have explored innovative approaches, including the incorporation of other materials like silica (SiO 2 ), to advance photocatalytic properties performance of TiO 2 in the visible light region [ 10 , 11 ]. The hydrothermal synthesis method has emerged as a versatile technique for fabricating nanocomposites with tailored structures and properties. Through Accurate manipulation of reaction factors such as temperature, pressure, and precursor concentrations, it is possible to design nanocomposite structures that enhance photocatalytic activity [ 12 , 13 ]. The integration of SiO 2 and TiO 2 through the hydrothermal method offers a platform to design materials with synergistic effects, where the distinct properties of each component can be harnessed for improved photocatalysis [ 14 , 15 ]. The principal aim of this research this paper seeks to explore the synthesis of SiO 2 -TiO 2 nanocomposites via the hydrothermal method and to comprehensively evaluate their photocatalytic activity under visible light conditions [ 16 , 17 ]. Through a comprehensive evaluation of the nanocomposite's structural, morphological, and optical features, our goal is to elucidate the mechanisms involved in visible light-induced photocatalytic processes [ 18 , 19 ]. This study aims to add to the expanding field of knowledge on advanced nanomaterials for sustainable environmental applications and provide valuable information for the design and optimization of efficient photocatalytic systems [ 20 ]. The remaining sections of this paper will explore the methodology used for nanocomposite synthesis, the characterization techniques employed to evaluate structural and optical properties, and the experimental setup for assessing photocatalytic activity. Furthermore, the results obtained from this investigation will be analysed and discussed in the context of existing literature, with the aim of elucidating the potential of SiO 2 -TiO 2 nanocomposites as viable photocatalytic materials under visible light illumination. The synthesis and characterization of SiO 2 -TiO 2 nanocomposites, along with their evaluation for photocatalytic activity under visible light, have a significant impact on progressing the field of sustainable and efficient photocatalysis [ 22 ]. In this study, a nano TiO 2 photocatalyst doped with nano SiO 2 was synthesized via the hydrothermal method. Unlike previous literature studies [ 23 , 24 , 25 ], both SiO 2 and TiO 2 raw materials were synthesized in the same medium, without separate syntheses. Due to this feature, it is considered as a method that is less cumbersome compared to previous studies and could potentially make a difference, influencing future research endeavors. Materials and Methods Materials and equipments Titanium (IV) isopropoxide (Ti [OCH(CH 3 ) 2 ] 4 ), Tetraethyl orthosilicate (Si(OC 2 H 5 ) 4 ), ethanol (EtOH), isopropyl alcohol (2-Propanol), acetone were supplied by Merck company. The IR spectra were measured using a Thermo Fisher Scientific Nicolet iS10 spectrophotometer with an ATR sampling accessory. UV–Vis spectra were determined with a Shimadzu UV-2001 UV–Vis spectrophotometer. A high-pressure, high-temperature reactor (Berghof Pressure Digestion DAB-3, Germany) was used for the preparation of nanocomposites. XRD analysis was conducted using a Rigaku Miniflex X-ray diffractometer with Cu-Kα radiation (1.54 Å, 40 kV, 55 mA). Field-emission gun scanning electron microscopy (FEG-SEM) was performed on a Philips XL 30 SFEG. Finally, UV–Vis diffuse reflectance spectroscopy (UV-DRS) analyses were performed using a Shimadzu UV-3600 UV–Vis NIR spectrophotometer. Preperation of nanocomposites In this study, all nanocomposites were synthesized using the hydrothermal method, following the same process for the preperation of each nanocomposite. The synthesis of nanocomposite materials in the synthesis part of these photocatalysts was carried out by varying the nano SiO 2 percentage for the purpose of structural comparison and content customization. In this stage, three different nanocomposite materials were synthesized along with pure TiO 2 . Nano SiO 2 ratios were synthesized as %100, %50, and %10, respectively, in the total nano TiO 2 material. Their compositions and abbreviations are shown in Table 1 . Table 1 The synthesized nanomaterials and their nomenclatures. Nanomaterials Number Preperation Method Content of Photocatalyst Explanation Designations 1 Hydrothermal TiO 2 To enable a comparison with SiO 2 -doped nanocomposites, nano TiO 2 was synthesized in the anatase form. TiO 2 2 Hydrothermal SiO 2 / TiO 2 A nanocomposite with a 100% SiO 2 content relative to TiO 2 . S1 3 Hydrothermal SiO 2 / TiO 2 A nanocomposite with a 50% SiO 2 content relative to TiO 2 . S2 4 Hydrothermal SiO 2 / TiO 2 A nanocomposite with a 10% SiO 2 content relative to TiO 2 . S3 In a total of 150 mL of isopropanol (IPA), pure Titanium (IV) isopropoxide (50 mL) was slowly added with continuous stirring using a magnetic stirrer at room temperature for 15 minutes. A clear solution was obtained. After the dissolution process was completed, deionized water (5 mL) was added drop by drop to this solution using a burette, and the suspension was vigorously mixed with a magnetic stirrer for 2 hours. The suspension was then moved into a 250 mL Teflon container of a high-temperature and high-pressure hydrothermal reactor. Afterward, the reactor lids were securely closed using a torque wrench. The heating eye of the reactor was used to raise the temperature inside to 210°C, and the sample was kept in the hydrothermal reactor for 24 hours. After this period, the reactor's heater was turned off, allowing the reactor vessel to return to room temperature. The lids of the reactors, now at room temperature, were opened under a fume hood to prevent the release of trapped gases. The reaction contents were removed from the Teflon containers, and a white precipitate was observed. To remove other liquids present in the reaction vessel from the precipitate, it was rotated at 9000 rpm for 5 minutes. The liquid part was dissected by decantation. The remaining solid white part was washed twice with water and then with ethanol and exposed to centrifugation at 9000 rpm for 5 minutes each time. The obtained precipitate was left to dry in a clean environment at room temperature for one day, followed by further drying in an 80°C vacuum oven. After the drying process, the synthesized materials were ground in a mortar until homogenized. The resulting powdered materials were stored in sealed containers. The nanocatalyst obtained because of the synthesis will be referred to as TiO 2 , following the abbreviation used in other studies for characterization and applications of these materials. Without altering the synthesis methods described above, the addition of Tetraethyl orthosilicate (TEOS) was carried out to introduce SiO 2 into the nanocomposite. Specifically, 50 mL of TEOS was added to 150 mL of IPA and 50 mL of Titanium (IV) Isopropoxide for %100 SiO 2 /TiO 2 , 25 mL of TEOS for %50 SiO 2 /TiO 2 , and 5 mL of TEOS for %10 SiO 2 /TiO 2 . The remaining processes followed the same synthesis steps. In the subsequent stages, the designations S1 for %100 SiO 2 /TiO 2 , S2 for %50 SiO 2 /TiO 2 , and S3 for %10 SiO 2 /TiO 2 will be used. The photocatalytic experiment of synthesized nanomaterials For photocatalytic degradation experiments, methylene blue (MB), a commonly used organic dye was employed [ 26 , 27 ]. The identical experimental procedures were applied to investigate the photocatalytic activities of all synthesized photocatalysts. 3 ppm aqueous solution of methylene blue dye was prepared for use in the photocatalytic studies. A volume of 100 mL of the dye solution was taken for each experiment. To this, 0.1 g of each photocatalyst was added to achieve adsorption/desorption equilibrium and suspension. The mixture was first sonicated for 10 minutes and then kept in the dark for 30 minutes. Before the start of the photocatalytic process, 2 mL of the dye solution was sampled, and the initial absorbance spectrum was recorded using a UV-Visible spectrometer. The ambient temperature in the photoreactor was continuously monitored and maintained at 22–25°C. Magnetic stirring was employed for mixing. For subsequent measurements during the photocatalytic process, 2 mL aliquots were taken at specified time intervals. These processes were continued until the absorbances of the dye in the environment reached their minimum values, indicating the degradation of dyes by the synthesized photocatalysts under visible light. These procedures were carried out for all photocatalysts. The interior of the photoreactor specially designed for conducting photocatalytic studies is entirely coated with aluminium sheet. At the top section of the reactor's interior, there are two lamps: one is a 250 W lamp emitting only visible light (without UV), and the other, a 400 W UVC lamp, is used for comparative purposes. To prevent overheating in the environment due to the power of these lamps, small holes are in parallel on one side of the reactor. On the opposite side of these holes, a powerful fan is mounted to draw in cool air from the outside. At the bottom of the reactor, a magnetic stirrer is placed to ensure continuous stirring throughout the photocatalytic degradation process, ensuring the homogeneous distribution of photocatalysts. For safety reasons, and due to the potential harmful effects on the eyes and skin, the photoreactor lid should always remain closed during operation, and direct eye contact with the lights inside the photoreactor should be avoided. Result and discussion Characterization of nanocomposites The investigation of the properties and characteristics of TiO 2 and SiO 2 –TiO 2 nanocomposites were examined through FT-IR, XRD, FEG-SEM, EDS, and UV-DRS. FT-IR spectroscopy was employed to elucidate the characteristics of the synthesized nanocomposites and identify distinctions. Figure 1 illustrates the FT-IR spectra of the prepared nanocomposites. We observed subtle distinctions in the FT-IR spectra between the TiO 2 and SiO 2 -TiO 2 nanocomposites. These variances can be attributed to the attachment of SiO 2 molecules onto the TiO 2 surface. Notably, the spectra of all nanocomposites exhibited Ti-O-Ti and Ti-O stretching vibrations within the 650 − 500 cm − 1 range, affirming the formation of the TiO 2 structure [ 28 ]. Furthermore, we detected peaks corresponding to stretching vibrations of Ti-OH and H-OH bonds in adsorbed water molecules at approximately 1631 cm − 1 and 3400 cm − 1 , respectively [ 29 ]. Comparatively, when examining the SiO 2 -TiO 2 nanocomposites' FT-IR spectra against that of TiO 2 , we observed additional peaks. Additionally, a broad Si-O-Si band has emerged around 1000 cm − 1 . The presence of this band indicates the existence of SiO 2 in the structure [ 30 , 31 ]. This situation is valid for all materials obtained. Investigating the crystal structure of TiO 2 involves the widely utilized technique of X-ray diffraction (XRD). Figure 2 displays the XRD patterns for TiO 2 and SiO 2 –TiO 2 nanocomposites. As depicted in Fig. 2 , the primary distinct diffraction peaks of TiO 2 were identified at 2θ angles of 25.35°, 37.86°, 48.03°, 53.91°, 55.06°, 62.67°, 68.75°, 70.25°, and 75.07°, corresponding to the lattice planes of (101), (004), (200), (105), (211), (204), (116), (220), and (215), respectively. The most prominent peak was observed at 2θ = 25.35°, corresponding to the (101) plane. These observed peaks align well with the standard spectrum of the anatase phase of TiO 2 (JCPDS card no: 21-2172) [ 32 , 33 , 34 ]. This outcome confirms the successful formation of the anatase form of TiO 2 . Notably, no discernible peaks were observed in the pattern, and there were no indications of rutile phase identification in the XRD spectrum. This result signifies that the anatase phase, known for its superior photocatalytic activity, has been effectively prepared. Furthermore, the XRD diffraction patterns of the prepared nanocomposites showed no significant deviations, except for minor fluctuations in peak intensity. Specifically, it is evident that the presence of SiO 2 does not exert an influence on the crystal structure of TiO 2 and does not introduce any additional distinctive peaks in the XRD patterns. This can be attributed to the low concentration of SiO 2 applied to the TiO 2 surface [ 35 , 36 ]. It is affirmed that all SiO 2 –TiO 2 nanocomposites were successfully synthesized based on their XRD patterns. The Debye–Scherrer equation was used to determine the average crystal sizes, with the crystal sizes of TiO 2 , S1, S2, and S3 measuring 14.76, 13.35, 13.50, and 13.60 nm, respectively. These findings reveal that the crystal sizes of the prepared nanocomposites are closely comparable. The slight discrepancies in crystal sizes between the nanocomposites may be attributed to the interactions' strength between the SiO 2 and TiO 2 particles. It's worth noting that the tiny crystal size of the photocatalyst plays an important role in its photocatalytic activity [ 37 ]. The nanostructure of the synthesized nanocomposites was analysed using Field Emission Gun Scanning electron microscopy to examine surface modifications on TiO 2 . Figure 3 displays the FEG-SEM images of the nanocomposites at various amplification levels. A careful examination of these FEG-SEM images reveals that the surfaces exhibit a uniform, spherical-like TiO 2 structure with clustered groups. In the case of SiO 2 –TiO 2 nanocomposites, Si, Ti and O molecules are present on the surface, resulting in the uniform spherical particles on the SiO 2 -TiO 2 surface. This observation indicates a moderate level of physical adsorption of SiO 2 molecules onto the TiO 2 surface. To identify the elemental components of all the prepared nanocomposites, Energy-Dispersive X-ray (EDX) analysis was conducted. The EDX spectrum of TiO 2 exhibits peaks corresponding to Ti and O atoms. However, upon examining the EDX data of SiO 2 –TiO 2 nanocomposites, peaks for Si elements within the SiO 2 structure, as well as the signals for Ti and O elements, are evident. Based on these results, it is evident that the TiO 2 nanocomposites indeed contain SiO 2 compounds. In summary, the FEG-SEM analysis confirmed the presence of a uniform spherical-like structure on the TiO 2 surface, with clustered groups. The EDX analysis revealed the elemental composition, providing unmistakable evidence that the TiO 2 nanocomposites include SiO 2 compounds. The EDX analysis and elemental identification can be found in Fig. 4 and Table 2 . Table 2 EDX results for the synthesized nanocomposites Nanocomposite Elements wt % at% TiO 2 O 17.42 38.7 Ti 82.58 61.3 S1 O 39.34 61 Si 20.78 18.35 Ti 39.88 20.65 S2 O 47.14 66.81 Si 15.74 13.09 Ti 37.13 18.1 S3 O 40.45 65.78 Si 4.86 4.5 Ti 54.7 29.72 The spectroscopic analysis of the nanocomposites was conducted using Ultraviolet-Visible Diffuse Reflectance Spectroscopy (UV-DRS) to investigate their light absorption characteristics in detail [ 38 ]. The resulting spectra are presented in Fig. 5 , showcasing the distinct optical behaviors of the materials. Titanium dioxide (TiO 2 ), in particular, demonstrates a sharp and well-defined absorption peak at 387 nanometers (nm) within the ultraviolet (UV) region, while no absorption is observed in the visible spectrum. This lack of visible light absorption is attributed to the intrinsic electronic structure of TiO 2 , which features a significantly large band gap energy of 3.2 electron volts (eV). This high band gap energy restricts the excitation of electrons under visible light, thus confining TiO 2 ’s photoactivity predominantly to the UV range. In contrast, the UV-DRS spectra of Silicon dioxide-Titanium dioxide (SiO 2 -TiO 2 ) nanocomposites reveal the emergence of absorption bands spanning the 400 to 600 nm range, which are characteristic of Silicon dioxide (SiO 2 ) [ 39 ]. These features represent a marked deviation from the behavior of pure TiO 2 and indicate a shift in the absorption spectrum toward the visible region. This shift is particularly significant, as it highlights the potential modification of the electronic and optical properties of TiO 2 due to its interaction with SiO 2 . Such changes can be attributed to alterations in the local electronic environment or the formation of new energy states at the interface of the composite material. The expanded light absorption range observed in the SiO 2 -TiO 2 nanocomposites is a notable advancement, as it addresses the limitation of TiO 2 's high band gap energy, which hinders effective absorption of visible light. By extending the absorption into the visible spectrum, the SiO 2 -TiO 2 composites demonstrate enhanced light sensitivity, making them promising candidates for applications where visible light activation is desirable. This enhanced optical behavior underscores the synergistic interaction between SiO 2 and TiO 2 within the composite, enabling the tailoring of material properties to suit specific functional requirements. Examination of photocatalytic performance The photocatalytic performance of the synthesized TiO 2 and SiO 2 –TiO 2 photocatalysts were systematically investigated with respect to the degradation process of methylene blue (MB), a widely used cationic organic dye, under UV-filtered visible light irradiation. MB was selected as a model pollutant due to its cationic nature and its high affinity for adsorption on TiO 2 surfaces, which is facilitated by negatively charged oxygen atoms within its molecular structure [ 40 ]. The distinct absorption peak of MB at 664 nm allows for precise and convenient monitoring of its degradation via UV-Visible spectroscopy, where the concentration of the dye can be quantitatively tracked through changes in absorption intensity [ 41 ]. Photocatalytic efficiency is recognized to be affected by several parameters, including catalyst loading, particle size, surface area, reaction temperature, pH, and the beginning concentration of the dye [ 42 ]. In this study, to ensure the reliability and comparability of results across different photocatalysts, all experimental conditions—such as photocatalyst dosage, initial concentration, pH value, ambient temperature of MB, and light intensity—were kept constant. The only variable in these experiments was the type of photocatalyst utilized. It is noteworthy that the pH of the MB solution was consistently maintained at around 6–7, with no significant fluctuations observed throughout the photocatalytic tests, thereby eliminating pH as a potential factor influencing the degradation process. 3 ppm aqueous solution of methylene blue in deionized water was prepared as the substrate for photocatalytic degradation experiments. From this stock solution, 100 ml aliquots were extracted for each experimental run. To these aliquots, 0.1 g of the respective photocatalyst was added. In order to ensure both sufficient dispersion and adsorption/desorption equilibrium, the dye-catalyst suspensions were first subjected to ultrasonic treatment for 10 minutes. This was followed by a 30-minute incubation period in the dark to account for any non-photocatalytic adsorption effects prior to light exposure. After this pre-treatment phase, an initial 2 ml sample was withdrawn from each solution, and the absorbance spectrum was recorded using a UV-Visible spectrometer to determine the baseline concentration of MB. The photocatalytic degradation experiments were conducted in a photoreactor controlled at a controlled temperature of 22–25°C, and continuous stirring was provided by a magnetic stirrer to ensure homogeneity within the reaction mixture. At predetermined time intervals during the photocatalytic process, 2 ml aliquots were collected for further absorbance measurements. These measurements were taken periodically until the absorbance values reached a minimum, indicating near-complete degradation of the dye. The experimental protocol was repeated for all photocatalysts synthesized in this study to comprehensively assess their photocatalytic efficiency under visible light conditions. Absorbance spectra were recorded across the 400–700 nm wavelength range using a UV-Visible spectrometer. The photocatalytic efficiency was evaluated by monitoring the reduction in absorbance at the characteristic peak of MB (664 nm), and the changes in the spectra were analyzed to quantify the degradation performance. The degradation profiles of all photocatalysts are presented below, highlighting the comparative efficiency of each material in promoting the photocatalytic breakdown of MB under visible light irradiation. As represented in Fig. 6 and Fig. 7 , it was observed that the aqueous solution of methylene blue was approximately 100% degraded after 2 minutes under the influence of visible light with the S1-coded nanocatalyst. Similarly, the aqueous solution of methylene blue exhibited approximately 100% degradation after 6 minutes under visible light with the S2-coded nanocatalyst, and after 10 minutes with the S3-coded nanocatalyst. This observation provides evidence that an increase in the SiO 2 ratio within the nanocomposite enhances the activity of the photocatalytic material under visible light. In addition to their photocatalytic properties, the nanocomposites were further characterized by SEM and EDS analyses, which confirmed their nanoscale structure and homogeneity. The observed nanoscale morphology is critical for maximizing surface area and enhancing photocatalytic interactions with pollutants. A key novelty of this thesis lies in the synthesis approach and its contribution to the literature. Unlike most previous studies where the nanostructures are synthesized separately and later combined through doping processes, this research utilized a hydrothermal method to co-synthesize the SiO 2 and TiO 2 nanocomposite in a single step under identical conditions. This methodological approach is relatively underexplored in the field, offering a more integrated synthesis route that potentially enhances the interaction between the two components, leading to improved photocatalytic performance. Conclusion In this study, nano SiO 2 -doped nano TiO 2 nanocomposites were synthesized using the hydrothermal method under varying reaction conditions. The primary motivation for incorporating nano SiO 2 was to improve the photocatalytic efficiency of nano TiO 2 from being limited to UV light to include the visible light spectrum, thereby enhancing its potential applications in broader environmental conditions. The investigation of the structure of the synthesized nanocomposites was carried out through a combination of advanced analytical techniques, including XRD, SEM-EDS, FT-IR, and UV-DRS Spectrophotometry. These techniques confirmed the successful formation of the nanocomposite materials and provided detailed insights into their morphological and compositional features. The photocatalytic behavior of the nanocomposites under visible light was studied by studying the degradation of organic dye pollutants, specifically methylene blue. The results demonstrated that the nanocomposites presented significant photocatalytic activity in the visible light region. Among the synthesized samples, the nanocomposite with a 100% SiO 2 /TiO 2 ratio, designated as S1, was found to be the most effective in degrading the organic pollutant, achieving complete degradation of the methylene blue solution within an exceptionally short time of approximately two minutes under visible light irradiation. This rapid degradation rate is a rare phenomenon in the existing literature and highlights the superior efficiency of the S1 nanocomposite, positioning it as a promising material for future photocatalytic applications and further studies. Furthermore, the study revealed that the photocatalytic efficiency of the nanocomposites varied proportionally with the SiO 2 content. The nanocomposite labeled S2, containing a 50% SiO 2 /TiO 2 ratio, while not as effective as S1, still exhibited noteworthy photocatalytic activity under visible light, demonstrating a significant degradation rate in a relatively short time. The nanocomposite designated as S3, with a 10% SiO 2 /TiO 2 ratio, although less efficient compared to S1 and S2, still outperformed pure anatase TiO 2 in terms of visible light-induced photocatalytic activity. These findings collectively suggest that the incorporation of SiO 2 into the TiO 2 matrix enhances the visible light responsiveness of the nanocomposite, with the photocatalytic activity being closely tied to the SiO 2 content. Declarations Funding: No fund is received for this work. Conflict of interest : The authors declare no competing interests. Ethics and consent to participate: Not Applicable. Consent for publication: No Applicable. Author Contributions Statement Oğuzhan Avcıata and Mustafa Borucu conceptualized and designed the study. Mustafa Borucu conducted the experiments and performed the data analysis. Semih Gördük contributed to the interpretation of the data. Mustafa Borucu and Oğuzhan Avcıata drafted the manuscript. Semih Gördük critically revised the manuscript for important intellectual content. All authors have reviewed and approved the final version of the manuscript and agree to be accountable for all aspects of the work. References J. Yi, G. Zhang, Y. Wang, W. 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Also discoverable on Platform About Our Team In Review Editorial Policies Advisory Board Help Center Resources Author Services Accessibility API Access RSS feed Manage Cookie Preferences © Research Square 2026 | ISSN 2693-5015 (online) Privacy Policy Terms of Service Do Not Sell My Personal Information {"props":{"pageProps":{"initialData":{"identity":"rs-6095977","acceptedTermsAndConditions":true,"allowDirectSubmit":true,"archivedVersions":[],"articleType":"Research Article","associatedPublications":[],"authors":[{"id":422147010,"identity":"1cefaafe-ca42-43f8-8af8-7f3ef18fcb04","order_by":0,"name":"Oguzhan Avciata","email":"data:image/png;base64,iVBORw0KGgoAAAANSUhEUgAAAZAAAAAyAQMAAABI0h/eAAAABlBMVEX///8AAABVwtN+AAAACXBIWXMAAA7EAAAOxAGVKw4bAAAA8UlEQVRIiWNgGAWjYLCCBCDmZ2BsPMBjAOMS1mLAINnA2IDQcoCwJgMGA6CqAzwwS/Fp4Wc/Y/jhQc0feeMbyQ0H3hTUAUVyDJg/7sGtRbInx1gi4ZiB4bYbiQ0H5xiwAUXeGDAceIbHRQfS0hgS2AwYQVoO8xjwMBjcyAFqweMyg/PPgFr+GdhvngHWIsFgT1DLjeRjDIltBokbJMBagOEgQUCL5IzHhyUS+4yTZ5x5CPJLAo/EmWcFB87g0cLPn9j48cc3Odv+9vSHD978qZPjb0/e+KACjxYEEEgAU+CoIUoD0D4i1Y2CUTAKRsHIAwB+rFg1sefkswAAAABJRU5ErkJggg==","orcid":"","institution":"Yıldız Technical University","correspondingAuthor":true,"prefix":"","firstName":"Oguzhan","middleName":"","lastName":"Avciata","suffix":""},{"id":422147011,"identity":"6fc3f04e-cc56-43f2-8e8c-8303d58bb431","order_by":1,"name":"Mustafa Borucu","email":"","orcid":"","institution":"Yıldız Technical University","correspondingAuthor":false,"prefix":"","firstName":"Mustafa","middleName":"","lastName":"Borucu","suffix":""},{"id":422147012,"identity":"5d4b778c-226c-4e17-9d59-8e4247711d1b","order_by":2,"name":"Semih Gorduk","email":"","orcid":"","institution":"Yıldız Technical University","correspondingAuthor":false,"prefix":"","firstName":"Semih","middleName":"","lastName":"Gorduk","suffix":""}],"badges":[],"createdAt":"2025-02-24 10:38:35","currentVersionCode":1,"declarations":"","doi":"10.21203/rs.3.rs-6095977/v1","doiUrl":"https://doi.org/10.21203/rs.3.rs-6095977/v1","draftVersion":[],"editorialEvents":[],"editorialNote":"","failedWorkflow":false,"files":[{"id":77629372,"identity":"e52b7668-3314-4055-8c9c-90ab6a931ee7","added_by":"auto","created_at":"2025-03-03 17:08:53","extension":"png","order_by":1,"title":"Figure 1","display":"","copyAsset":false,"role":"figure","size":27771,"visible":true,"origin":"","legend":"\u003cp\u003eFT-IR spectra of the synthesized nanocomposites\u003c/p\u003e\n\u003cp\u003eFourier Transform Infrared (FTIR) spectra of SiO₂-TiO₂ nanocomposites synthesized under different conditions (S1, S2, and S3). The individual spectra for each sample are presented separately (top left: S1, top right: S2, bottom left: S3), and the comparative overlay of all three spectra is displayed in the bottom right panel. The transmittance (%) is plotted against the wavenumber (cm⁻¹) to identify the characteristic functional groups and bonding interactions present in the nanocomposites. The spectra exhibit absorption bands corresponding to Si-O-Si, Ti-O-Ti, and Si-O-Ti bonds, with notable peaks in the fingerprint region (400–1200 cm⁻¹), indicating the successful incorporation of SiO₂ and TiO₂ phases.\u003c/p\u003e","description":"","filename":"Onlinefloatimage1.png","url":"https://assets-eu.researchsquare.com/files/rs-6095977/v1/3f842ad13df4054a2a157468.png"},{"id":77629768,"identity":"2825d4c5-7fe6-4583-886e-fa70a2df3d11","added_by":"auto","created_at":"2025-03-03 17:16:53","extension":"png","order_by":2,"title":"Figure 2","display":"","copyAsset":false,"role":"figure","size":15113,"visible":true,"origin":"","legend":"\u003cp\u003eX-ray diffraction (XRD) patterns of the synthesized nanocomposites\u003c/p\u003e\n\u003cp\u003eX-ray diffraction (XRD) patterns of TiO₂ and SiO₂-TiO₂ nanocomposites synthesized under different conditions (S1, S2, and S3). The diffraction intensity (counts) is plotted as a function of 2θ (degrees) to identify the crystalline phases present in the samples. The top-left panel represents the reference TiO₂ diffraction pattern, while the remaining panels (top-right: S1, bottom-left: S2, bottom-right: S3) illustrate the diffraction patterns of nanocomposites. The observed peaks correspond to the anatase TiO₂ and crystalline SiO₂ phases, confirming the structural characteristics of the synthesized nanomaterials. The presence of characteristic diffraction peaks suggests the successful formation of the SiO₂-TiO₂ composite structure.\u003c/p\u003e","description":"","filename":"Onlinefloatimage2.png","url":"https://assets-eu.researchsquare.com/files/rs-6095977/v1/47224fb0439425195a667d8b.png"},{"id":77629377,"identity":"7ace4ed9-c346-48c0-bfc9-97318903f479","added_by":"auto","created_at":"2025-03-03 17:08:53","extension":"png","order_by":3,"title":"Figure 3","display":"","copyAsset":false,"role":"figure","size":106392,"visible":true,"origin":"","legend":"\u003cp\u003eSEM images of the prepared nanocomposites\u003c/p\u003e\n\u003cp\u003eScanning Electron Microscopy (SEM) images of TiO₂ and SiO₂-TiO₂ nanocomposites synthesized under different conditions (S1, S2, and S3). The images are arranged in pairs, with the left column showing lower magnification (10 µm scale) and the right column showing higher magnification (1 µm scale). The top row represents pure TiO₂, while the subsequent rows correspond to samples S1, S2, and S3. The micrographs illustrate the morphological differences between the synthesized nanocomposites, highlighting variations in particle size, agglomeration behavior, and surface texture. The spherical and aggregated structures observed in the composites indicate the successful formation of SiO₂-TiO₂ hybrid structures.\u003c/p\u003e","description":"","filename":"Onlinefloatimage3.png","url":"https://assets-eu.researchsquare.com/files/rs-6095977/v1/2162aae47c36e1d2321806f3.png"},{"id":77629770,"identity":"7f449683-c133-4e7c-af55-9a2b01786abc","added_by":"auto","created_at":"2025-03-03 17:16:53","extension":"png","order_by":4,"title":"Figure 4","display":"","copyAsset":false,"role":"figure","size":823148,"visible":true,"origin":"","legend":"\u003cp\u003eEDX results for the synthesized nanocomposites\u003c/p\u003e\n\u003cp\u003eSEM-EDS (Scanning Electron Microscopy - Energy Dispersive X-ray Spectroscopy) analysis of TiO₂ and SiO₂-TiO₂ nanocomposites synthesized under different conditions (S1, S2, and S3). The left column presents SEM images of the samples, highlighting the selected regions for elemental analysis. The right column displays the corresponding EDS spectra, indicating the elemental composition of each sample. The EDS spectra confirm the presence of titanium (Ti), oxygen (O), and silicon (Si) elements, validating the incorporation of SiO₂ within the TiO₂ matrix in the nanocomposites. The variations in silicon intensity among S1, S2, and S3 samples suggest differences in SiO₂ distribution and content across the synthesized material.\u003c/p\u003e","description":"","filename":"floatimage4.png","url":"https://assets-eu.researchsquare.com/files/rs-6095977/v1/202f00aba148fb20c5ecdac7.png"},{"id":77629376,"identity":"ef1e1714-7c9b-4a4f-b8e5-8b789de181cc","added_by":"auto","created_at":"2025-03-03 17:08:53","extension":"png","order_by":5,"title":"Figure 5","display":"","copyAsset":false,"role":"figure","size":23125,"visible":true,"origin":"","legend":"\u003cp\u003eUV- DRS spectra of the prepared nanocomposites\u003c/p\u003e\n\u003cp\u003eUV-Vis diffuse reflectance spectra of SiO₂-TiO₂ nanocomposites synthesized under different conditions (S1, S2, and S3). The reflectance percentage is plotted as a function of wavelength (nm) to analyze the optical properties and bandgap characteristics of the samples. The individual spectra for each sample are shown separately (top left: S1, top right: S2, bottom left: S3), while the comparative overlay of all three spectra is presented in the bottom right panel. The sharp increase in reflectance at specific wavelengths indicates the optical bandgap of the nanocomposites, revealing variations in light absorption behavior depending on synthesis conditions.\u003c/p\u003e","description":"","filename":"Onlinefloatimage5.png","url":"https://assets-eu.researchsquare.com/files/rs-6095977/v1/9dd938b4ec4ae997f7a8f785.png"},{"id":77629382,"identity":"04810d49-f1fc-4c7e-bf46-f87a0b95a7b7","added_by":"auto","created_at":"2025-03-03 17:08:53","extension":"png","order_by":6,"title":"Figure 6","display":"","copyAsset":false,"role":"figure","size":34469,"visible":true,"origin":"","legend":"\u003cp\u003eThe degradation of Methylene Blue by photocatalysis was followed through UV-Vis absorption spectra under illumination, using the synthesized nanocomposites\u003c/p\u003e\n\u003cp\u003eTime-dependent UV-Vis absorption spectra of TiO₂ and SiO₂-TiO₂ nanocomposites (S1, S2, and S3) during photocatalytic degradation of an organic dye under visible light irradiation. The absorbance is plotted as a function of wavelength (nm) for different time intervals (0, 2, 4, 6, 8, 10, and 12 minutes), demonstrating the degradation efficiency of each sample. The TiO₂ reference sample (top-left) exhibits significant absorption at around 600-700 nm, while the nanocomposites (top-right: S1, bottom-left: S2, bottom-right: S3) show a gradual decrease in absorbance over time, indicating enhanced photocatalytic activity. The variations in degradation rates among the samples highlight the influence of SiO₂ incorporation on the photocatalytic performance.\u003c/p\u003e","description":"","filename":"Onlinefloatimage6.png","url":"https://assets-eu.researchsquare.com/files/rs-6095977/v1/7ac2b8c256cd63dd8d8e9088.png"},{"id":77629378,"identity":"a47d8cff-7606-491e-b1f6-5076aa46adf1","added_by":"auto","created_at":"2025-03-03 17:08:53","extension":"png","order_by":7,"title":"Figure 7","display":"","copyAsset":false,"role":"figure","size":16597,"visible":true,"origin":"","legend":"\u003cp\u003ea) Full degradation times of Methylene Blue the prepared photocatalysts, b) The activation capability of the synthesized nanocomposites in the visible region within a 2-minute timeframe.\u003c/p\u003e\n\u003cp\u003e(a) Comparison of photocatalytic degradation efficiency of SiO₂-TiO₂ nanocomposites (S1, S2, and S3) based on degradation time. The 3D bar chart illustrates the variation in degradation times for different samples, highlighting S3 as the most efficient photocatalyst. (b) UV-Vis absorbance spectra of TiO₂ and SiO₂-TiO₂ nanocomposites after 2 minutes of photocatalytic reaction. The absorbance is plotted against wavelength (nm), showing a significant reduction in dye concentration for S1, S2, and S3, compared to TiO₂. The results indicate that SiO₂ incorporation enhances photocatalytic activity, with S3 exhibiting the highest degradation efficiency.\u003c/p\u003e","description":"","filename":"Onlinefloatimage7.png","url":"https://assets-eu.researchsquare.com/files/rs-6095977/v1/8479a84219279207683cd3b6.png"},{"id":78515598,"identity":"8b70568e-8c5b-4cd5-9142-a0fa6ee9ce9a","added_by":"auto","created_at":"2025-03-14 10:47:05","extension":"pdf","order_by":0,"title":"","display":"","copyAsset":false,"role":"manuscript-pdf","size":1733076,"visible":true,"origin":"","legend":"","description":"","filename":"manuscript.pdf","url":"https://assets-eu.researchsquare.com/files/rs-6095977/v1/c3f9d835-b172-48b2-82f8-d00b745993c5.pdf"}],"financialInterests":"No competing interests reported.","formattedTitle":"\u003cp\u003eHydrothermal Synthesis of Visible Light Photocatalytic SIO2 - TIO2 Nanocomposites\u003c/p\u003e","fulltext":[{"header":"Introduction","content":"\u003cp\u003eIn recent years, the progress in creating advanced materials with enhanced photocatalytic activity has received considerable interest because of their potential roles in environmental remediation, energy generation, and sustainability [\u003cspan citationid=\"CR1\" class=\"CitationRef\"\u003e1\u003c/span\u003e, \u003cspan citationid=\"CR2\" class=\"CitationRef\"\u003e2\u003c/span\u003e]. Among these materials, nanocomposites that combine distinct properties of different components offer a promising avenue for optimizing photocatalytic performance [\u003cspan citationid=\"CR3\" class=\"CitationRef\"\u003e3\u003c/span\u003e, \u003cspan citationid=\"CR4\" class=\"CitationRef\"\u003e4\u003c/span\u003e]. The combination of Silica (SiO\u003csub\u003e2\u003c/sub\u003e) and Titanium dioxide (TiO\u003csub\u003e2\u003c/sub\u003e) in nanocomposites has demonstrated the ability to harness visible light for photocatalysis, opening new possibilities for efficient utilization of solar energy and pollutant degradation [\u003cspan citationid=\"CR5\" class=\"CitationRef\"\u003e5\u003c/span\u003e, \u003cspan citationid=\"CR6\" class=\"CitationRef\"\u003e6\u003c/span\u003e].\u003c/p\u003e \u003cp\u003ePhotocatalysis, a process where light-activated catalysts promote chemical reactions, has become a crucial approach for tackling environmental issues. Titanium dioxide (TiO\u003csub\u003e2\u003c/sub\u003e), a widely studied photocatalyst, exhibits exceptional properties such as chemical stability, non-toxicity, and photocatalytic activity under ultraviolet (UV) light [\u003cspan citationid=\"CR7\" class=\"CitationRef\"\u003e7\u003c/span\u003e, \u003cspan citationid=\"CR8\" class=\"CitationRef\"\u003e8\u003c/span\u003e]. However, its practical application is limited by its inability to utilize visible light effectively, which constitutes a major portion of the solar spectrum [\u003cspan citationid=\"CR9\" class=\"CitationRef\"\u003e9\u003c/span\u003e]. To overcome this limitation, researchers have explored innovative approaches, including the incorporation of other materials like silica (SiO\u003csub\u003e2\u003c/sub\u003e), to advance photocatalytic properties performance of TiO\u003csub\u003e2\u003c/sub\u003e in the visible light region [\u003cspan citationid=\"CR10\" class=\"CitationRef\"\u003e10\u003c/span\u003e, \u003cspan citationid=\"CR11\" class=\"CitationRef\"\u003e11\u003c/span\u003e].\u003c/p\u003e \u003cp\u003eThe hydrothermal synthesis method has emerged as a versatile technique for fabricating nanocomposites with tailored structures and properties. Through Accurate manipulation of reaction factors such as temperature, pressure, and precursor concentrations, it is possible to design nanocomposite structures that enhance photocatalytic activity [\u003cspan citationid=\"CR12\" class=\"CitationRef\"\u003e12\u003c/span\u003e, \u003cspan citationid=\"CR13\" class=\"CitationRef\"\u003e13\u003c/span\u003e]. The integration of SiO\u003csub\u003e2\u003c/sub\u003e and TiO\u003csub\u003e2\u003c/sub\u003e through the hydrothermal method offers a platform to design materials with synergistic effects, where the distinct properties of each component can be harnessed for improved photocatalysis [\u003cspan citationid=\"CR14\" class=\"CitationRef\"\u003e14\u003c/span\u003e, \u003cspan citationid=\"CR15\" class=\"CitationRef\"\u003e15\u003c/span\u003e].\u003c/p\u003e \u003cp\u003eThe principal aim of this research this paper seeks to explore the synthesis of SiO\u003csub\u003e2\u003c/sub\u003e-TiO\u003csub\u003e2\u003c/sub\u003e nanocomposites via the hydrothermal method and to comprehensively evaluate their photocatalytic activity under visible light conditions [\u003cspan citationid=\"CR16\" class=\"CitationRef\"\u003e16\u003c/span\u003e, \u003cspan citationid=\"CR17\" class=\"CitationRef\"\u003e17\u003c/span\u003e]. Through a comprehensive evaluation of the nanocomposite's structural, morphological, and optical features, our goal is to elucidate the mechanisms involved in visible light-induced photocatalytic processes [\u003cspan citationid=\"CR18\" class=\"CitationRef\"\u003e18\u003c/span\u003e, \u003cspan citationid=\"CR19\" class=\"CitationRef\"\u003e19\u003c/span\u003e]. This study aims to add to the expanding field of knowledge on advanced nanomaterials for sustainable environmental applications and provide valuable information for the design and optimization of efficient photocatalytic systems [\u003cspan citationid=\"CR20\" class=\"CitationRef\"\u003e20\u003c/span\u003e].\u003c/p\u003e \u003cp\u003eThe remaining sections of this paper will explore the methodology used for nanocomposite synthesis, the characterization techniques employed to evaluate structural and optical properties, and the experimental setup for assessing photocatalytic activity. Furthermore, the results obtained from this investigation will be analysed and discussed in the context of existing literature, with the aim of elucidating the potential of SiO\u003csub\u003e2\u003c/sub\u003e-TiO\u003csub\u003e2\u003c/sub\u003e nanocomposites as viable photocatalytic materials under visible light illumination.\u003c/p\u003e \u003cp\u003eThe synthesis and characterization of SiO\u003csub\u003e2\u003c/sub\u003e-TiO\u003csub\u003e2\u003c/sub\u003e nanocomposites, along with their evaluation for photocatalytic activity under visible light, have a significant impact on progressing the field of sustainable and efficient photocatalysis [\u003cspan citationid=\"CR22\" class=\"CitationRef\"\u003e22\u003c/span\u003e]. In this study, a nano TiO\u003csub\u003e2\u003c/sub\u003e photocatalyst doped with nano SiO\u003csub\u003e2\u003c/sub\u003e was synthesized via the hydrothermal method. Unlike previous literature studies [\u003cspan citationid=\"CR23\" class=\"CitationRef\"\u003e23\u003c/span\u003e, \u003cspan citationid=\"CR24\" class=\"CitationRef\"\u003e24\u003c/span\u003e, \u003cspan citationid=\"CR25\" class=\"CitationRef\"\u003e25\u003c/span\u003e], both SiO\u003csub\u003e2\u003c/sub\u003e and TiO\u003csub\u003e2\u003c/sub\u003e raw materials were synthesized in the same medium, without separate syntheses. Due to this feature, it is considered as a method that is less cumbersome compared to previous studies and could potentially make a difference, influencing future research endeavors.\u003c/p\u003e"},{"header":"Materials and Methods","content":"\u003cdiv id=\"Sec3\" class=\"Section2\"\u003e \u003ch2\u003eMaterials and equipments\u003c/h2\u003e \u003cp\u003eTitanium (IV) isopropoxide (Ti [OCH(CH\u003csub\u003e3\u003c/sub\u003e)\u003csub\u003e2\u003c/sub\u003e]\u003csub\u003e4\u003c/sub\u003e), Tetraethyl orthosilicate (Si(OC\u003csub\u003e2\u003c/sub\u003eH\u003csub\u003e5\u003c/sub\u003e)\u003csub\u003e4\u003c/sub\u003e), ethanol (EtOH), isopropyl alcohol (2-Propanol), acetone were supplied by Merck company. The IR spectra were measured using a Thermo Fisher Scientific Nicolet iS10 spectrophotometer with an ATR sampling accessory. UV\u0026ndash;Vis spectra were determined with a Shimadzu UV-2001 UV\u0026ndash;Vis spectrophotometer. A high-pressure, high-temperature reactor (Berghof Pressure Digestion DAB-3, Germany) was used for the preparation of nanocomposites. XRD analysis was conducted using a Rigaku Miniflex X-ray diffractometer with Cu-Kα radiation (1.54 \u0026Aring;, 40 kV, 55 mA). Field-emission gun scanning electron microscopy (FEG-SEM) was performed on a Philips XL 30 SFEG. Finally, UV\u0026ndash;Vis diffuse reflectance spectroscopy (UV-DRS) analyses were performed using a Shimadzu UV-3600 UV\u0026ndash;Vis NIR spectrophotometer.\u003c/p\u003e \u003c/div\u003e\n\u003ch3\u003ePreperation of nanocomposites\u003c/h3\u003e\n\u003cp\u003eIn this study, all nanocomposites were synthesized using the hydrothermal method, following the same process for the preperation of each nanocomposite. The synthesis of nanocomposite materials in the synthesis part of these photocatalysts was carried out by varying the nano SiO\u003csub\u003e2\u003c/sub\u003e percentage for the purpose of structural comparison and content customization. In this stage, three different nanocomposite materials were synthesized along with pure TiO\u003csub\u003e2\u003c/sub\u003e. Nano SiO\u003csub\u003e2\u003c/sub\u003e ratios were synthesized as %100, %50, and %10, respectively, in the total nano TiO\u003csub\u003e2\u003c/sub\u003e material. Their compositions and abbreviations are shown in Table\u0026nbsp;\u003cspan refid=\"Tab1\" class=\"InternalRef\"\u003e1\u003c/span\u003e.\u003c/p\u003e \u003cp\u003e \u003cdiv class=\"gridtable\"\u003e\u003ctable float=\"Yes\" id=\"Tab1\" border=\"1\"\u003e \u003ccaption language=\"En\"\u003e \u003cdiv class=\"CaptionNumber\"\u003eTable 1\u003c/div\u003e \u003cdiv class=\"CaptionContent\"\u003e \u003cp\u003eThe synthesized nanomaterials and their nomenclatures.\u003c/p\u003e \u003c/div\u003e \u003c/caption\u003e \u003ccolgroup cols=\"5\"\u003e \u003cdiv align=\"left\" class=\"colspec\" colname=\"c1\" colnum=\"1\"\u003e\u003c/div\u003e \u003cdiv align=\"left\" class=\"colspec\" colname=\"c2\" colnum=\"2\"\u003e\u003c/div\u003e \u003cdiv align=\"left\" class=\"colspec\" colname=\"c3\" colnum=\"3\"\u003e\u003c/div\u003e \u003cdiv align=\"left\" class=\"colspec\" colname=\"c4\" colnum=\"4\"\u003e\u003c/div\u003e \u003cdiv align=\"left\" class=\"colspec\" colname=\"c5\" colnum=\"5\"\u003e\u003c/div\u003e \u003cthead\u003e \u003ctr\u003e \u003cth align=\"left\" colname=\"c1\"\u003e \u003cp\u003eNanomaterials Number\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colname=\"c2\"\u003e \u003cp\u003ePreperation Method\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colname=\"c3\"\u003e \u003cp\u003eContent of Photocatalyst\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colname=\"c4\"\u003e \u003cp\u003eExplanation\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colname=\"c5\"\u003e \u003cp\u003eDesignations\u003c/p\u003e \u003c/th\u003e \u003c/tr\u003e \u003c/thead\u003e \u003ctbody\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003e1\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003eHydrothermal\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c3\"\u003e \u003cp\u003eTiO\u003csub\u003e2\u003c/sub\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c4\"\u003e \u003cp\u003eTo enable a comparison with SiO\u003csub\u003e2\u003c/sub\u003e-doped nanocomposites, nano TiO\u003csub\u003e2\u003c/sub\u003e was synthesized in the anatase form.\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c5\"\u003e \u003cp\u003eTiO\u003csub\u003e2\u003c/sub\u003e\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003e2\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003eHydrothermal\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c3\"\u003e \u003cp\u003eSiO\u003csub\u003e2\u003c/sub\u003e / TiO\u003csub\u003e2\u003c/sub\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c4\"\u003e \u003cp\u003eA nanocomposite with a 100% SiO\u003csub\u003e2\u003c/sub\u003e content relative to TiO\u003csub\u003e2\u003c/sub\u003e.\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c5\"\u003e \u003cp\u003eS1\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003e3\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003eHydrothermal\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c3\"\u003e \u003cp\u003eSiO\u003csub\u003e2\u003c/sub\u003e / TiO\u003csub\u003e2\u003c/sub\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c4\"\u003e \u003cp\u003eA nanocomposite with a 50% SiO\u003csub\u003e2\u003c/sub\u003e content relative to TiO\u003csub\u003e2\u003c/sub\u003e.\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c5\"\u003e \u003cp\u003eS2\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003e4\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003eHydrothermal\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c3\"\u003e \u003cp\u003eSiO\u003csub\u003e2\u003c/sub\u003e / TiO\u003csub\u003e2\u003c/sub\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c4\"\u003e \u003cp\u003eA nanocomposite with a 10% SiO\u003csub\u003e2\u003c/sub\u003e content relative to TiO\u003csub\u003e2\u003c/sub\u003e.\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c5\"\u003e \u003cp\u003eS3\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003c/tbody\u003e \u003c/colgroup\u003e \u003c/table\u003e\u003c/div\u003e \u003c/p\u003e \u003cp\u003eIn a total of 150 mL of isopropanol (IPA), pure Titanium (IV) isopropoxide (50 mL) was slowly added with continuous stirring using a magnetic stirrer at room temperature for 15 minutes. A clear solution was obtained. After the dissolution process was completed, deionized water (5 mL) was added drop by drop to this solution using a burette, and the suspension was vigorously mixed with a magnetic stirrer for 2 hours. The suspension was then moved into a 250 mL Teflon container of a high-temperature and high-pressure hydrothermal reactor. Afterward, the reactor lids were securely closed using a torque wrench. The heating eye of the reactor was used to raise the temperature inside to 210\u0026deg;C, and the sample was kept in the hydrothermal reactor for 24 hours. After this period, the reactor's heater was turned off, allowing the reactor vessel to return to room temperature. The lids of the reactors, now at room temperature, were opened under a fume hood to prevent the release of trapped gases. The reaction contents were removed from the Teflon containers, and a white precipitate was observed. To remove other liquids present in the reaction vessel from the precipitate, it was rotated at 9000 rpm for 5 minutes. The liquid part was dissected by decantation. The remaining solid white part was washed twice with water and then with ethanol and exposed to centrifugation at 9000 rpm for 5 minutes each time. The obtained precipitate was left to dry in a clean environment at room temperature for one day, followed by further drying in an 80\u0026deg;C vacuum oven. After the drying process, the synthesized materials were ground in a mortar until homogenized. The resulting powdered materials were stored in sealed containers. The nanocatalyst obtained because of the synthesis will be referred to as TiO\u003csub\u003e2\u003c/sub\u003e, following the abbreviation used in other studies for characterization and applications of these materials.\u003c/p\u003e \u003cp\u003eWithout altering the synthesis methods described above, the addition of Tetraethyl orthosilicate (TEOS) was carried out to introduce SiO\u003csub\u003e2\u003c/sub\u003e into the nanocomposite. Specifically, 50 mL of TEOS was added to 150 mL of IPA and 50 mL of Titanium (IV) Isopropoxide for %100 SiO\u003csub\u003e2\u003c/sub\u003e/TiO\u003csub\u003e2\u003c/sub\u003e, 25 mL of TEOS for %50 SiO\u003csub\u003e2\u003c/sub\u003e/TiO\u003csub\u003e2\u003c/sub\u003e, and 5 mL of TEOS for %10 SiO\u003csub\u003e2\u003c/sub\u003e/TiO\u003csub\u003e2\u003c/sub\u003e. The remaining processes followed the same synthesis steps. In the subsequent stages, the designations S1 for %100 SiO\u003csub\u003e2\u003c/sub\u003e/TiO\u003csub\u003e2\u003c/sub\u003e, S2 for %50 SiO\u003csub\u003e2\u003c/sub\u003e/TiO\u003csub\u003e2\u003c/sub\u003e, and S3 for %10 SiO\u003csub\u003e2\u003c/sub\u003e/TiO\u003csub\u003e2\u003c/sub\u003e will be used.\u003c/p\u003e\n\u003ch3\u003eThe photocatalytic experiment of synthesized nanomaterials\u003c/h3\u003e\n\u003cp\u003eFor photocatalytic degradation experiments, methylene blue (MB), a commonly used organic dye was employed [\u003cspan citationid=\"CR26\" class=\"CitationRef\"\u003e26\u003c/span\u003e, \u003cspan citationid=\"CR27\" class=\"CitationRef\"\u003e27\u003c/span\u003e]. The identical experimental procedures were applied to investigate the photocatalytic activities of all synthesized photocatalysts. 3 ppm aqueous solution of methylene blue dye was prepared for use in the photocatalytic studies. A volume of 100 mL of the dye solution was taken for each experiment. To this, 0.1 g of each photocatalyst was added to achieve adsorption/desorption equilibrium and suspension. The mixture was first sonicated for 10 minutes and then kept in the dark for 30 minutes. Before the start of the photocatalytic process, 2 mL of the dye solution was sampled, and the initial absorbance spectrum was recorded using a UV-Visible spectrometer. The ambient temperature in the photoreactor was continuously monitored and maintained at 22\u0026ndash;25\u0026deg;C. Magnetic stirring was employed for mixing. For subsequent measurements during the photocatalytic process, 2 mL aliquots were taken at specified time intervals. These processes were continued until the absorbances of the dye in the environment reached their minimum values, indicating the degradation of dyes by the synthesized photocatalysts under visible light. These procedures were carried out for all photocatalysts. The interior of the photoreactor specially designed for conducting photocatalytic studies is entirely coated with aluminium sheet. At the top section of the reactor's interior, there are two lamps: one is a 250 W lamp emitting only visible light (without UV), and the other, a 400 W UVC lamp, is used for comparative purposes. To prevent overheating in the environment due to the power of these lamps, small holes are in parallel on one side of the reactor. On the opposite side of these holes, a powerful fan is mounted to draw in cool air from the outside. At the bottom of the reactor, a magnetic stirrer is placed to ensure continuous stirring throughout the photocatalytic degradation process, ensuring the homogeneous distribution of photocatalysts. For safety reasons, and due to the potential harmful effects on the eyes and skin, the photoreactor lid should always remain closed during operation, and direct eye contact with the lights inside the photoreactor should be avoided.\u003c/p\u003e"},{"header":"Result and discussion","content":"\u003cdiv id=\"Sec7\" class=\"Section2\"\u003e \u003ch2\u003eCharacterization of nanocomposites\u003c/h2\u003e \u003cp\u003eThe investigation of the properties and characteristics of TiO\u003csub\u003e2\u003c/sub\u003e and SiO\u003csub\u003e2\u003c/sub\u003e\u0026ndash;TiO\u003csub\u003e2\u003c/sub\u003e nanocomposites were examined through FT-IR, XRD, FEG-SEM, EDS, and UV-DRS.\u003c/p\u003e \u003cp\u003eFT-IR spectroscopy was employed to elucidate the characteristics of the synthesized nanocomposites and identify distinctions. Figure\u0026nbsp;\u003cspan refid=\"Fig2\" class=\"InternalRef\"\u003e1\u003c/span\u003e illustrates the FT-IR spectra of the prepared nanocomposites. We observed subtle distinctions in the FT-IR spectra between the TiO\u003csub\u003e2\u003c/sub\u003e and SiO\u003csub\u003e2\u003c/sub\u003e-TiO\u003csub\u003e2\u003c/sub\u003e nanocomposites. These variances can be attributed to the attachment of SiO\u003csub\u003e2\u003c/sub\u003e molecules onto the TiO\u003csub\u003e2\u003c/sub\u003e surface. Notably, the spectra of all nanocomposites exhibited Ti-O-Ti and Ti-O stretching vibrations within the 650\u0026thinsp;\u0026minus;\u0026thinsp;500 cm\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e range, affirming the formation of the TiO\u003csub\u003e2\u003c/sub\u003e structure [\u003cspan citationid=\"CR28\" class=\"CitationRef\"\u003e28\u003c/span\u003e]. Furthermore, we detected peaks corresponding to stretching vibrations of Ti-OH and H-OH bonds in adsorbed water molecules at approximately 1631 cm\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e and 3400 cm\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e, respectively [\u003cspan citationid=\"CR29\" class=\"CitationRef\"\u003e29\u003c/span\u003e]. Comparatively, when examining the SiO\u003csub\u003e2\u003c/sub\u003e-TiO\u003csub\u003e2\u003c/sub\u003e nanocomposites' FT-IR spectra against that of TiO\u003csub\u003e2\u003c/sub\u003e, we observed additional peaks. Additionally, a broad Si-O-Si band has emerged around 1000 cm\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e. The presence of this band indicates the existence of SiO\u003csub\u003e2\u003c/sub\u003e in the structure [\u003cspan citationid=\"CR30\" class=\"CitationRef\"\u003e30\u003c/span\u003e, \u003cspan citationid=\"CR31\" class=\"CitationRef\"\u003e31\u003c/span\u003e]. This situation is valid for all materials obtained.\u003c/p\u003e\u003cp\u003eInvestigating the crystal structure of TiO\u003csub\u003e2\u003c/sub\u003e involves the widely utilized technique of X-ray diffraction (XRD). Figure\u0026nbsp;\u003cspan refid=\"Fig4\" class=\"InternalRef\"\u003e2\u003c/span\u003e displays the XRD patterns for TiO\u003csub\u003e2\u003c/sub\u003e and SiO\u003csub\u003e2\u003c/sub\u003e\u0026ndash;TiO\u003csub\u003e2\u003c/sub\u003e nanocomposites. As depicted in Fig.\u0026nbsp;\u003cspan refid=\"Fig4\" class=\"InternalRef\"\u003e2\u003c/span\u003e, the primary distinct diffraction peaks of TiO\u003csub\u003e2\u003c/sub\u003e were identified at 2θ angles of 25.35\u0026deg;, 37.86\u0026deg;, 48.03\u0026deg;, 53.91\u0026deg;, 55.06\u0026deg;, 62.67\u0026deg;, 68.75\u0026deg;, 70.25\u0026deg;, and 75.07\u0026deg;, corresponding to the lattice planes of (101), (004), (200), (105), (211), (204), (116), (220), and (215), respectively. The most prominent peak was observed at 2θ\u0026thinsp;=\u0026thinsp;25.35\u0026deg;, corresponding to the (101) plane. These observed peaks align well with the standard spectrum of the anatase phase of TiO\u003csub\u003e2\u003c/sub\u003e (JCPDS card no: 21-2172) [\u003cspan citationid=\"CR32\" class=\"CitationRef\"\u003e32\u003c/span\u003e, \u003cspan citationid=\"CR33\" class=\"CitationRef\"\u003e33\u003c/span\u003e, \u003cspan citationid=\"CR34\" class=\"CitationRef\"\u003e34\u003c/span\u003e]. This outcome confirms the successful formation of the anatase form of TiO\u003csub\u003e2\u003c/sub\u003e. Notably, no discernible peaks were observed in the pattern, and there were no indications of rutile phase identification in the XRD spectrum. This result signifies that the anatase phase, known for its superior photocatalytic activity, has been effectively prepared.\u003c/p\u003e \u003cp\u003eFurthermore, the XRD diffraction patterns of the prepared nanocomposites showed no significant deviations, except for minor fluctuations in peak intensity. Specifically, it is evident that the presence of SiO\u003csub\u003e2\u003c/sub\u003e does not exert an influence on the crystal structure of TiO\u003csub\u003e2\u003c/sub\u003e and does not introduce any additional distinctive peaks in the XRD patterns. This can be attributed to the low concentration of SiO\u003csub\u003e2\u003c/sub\u003e applied to the TiO\u003csub\u003e2\u003c/sub\u003e surface [\u003cspan citationid=\"CR35\" class=\"CitationRef\"\u003e35\u003c/span\u003e, \u003cspan citationid=\"CR36\" class=\"CitationRef\"\u003e36\u003c/span\u003e]. It is affirmed that all SiO\u003csub\u003e2\u003c/sub\u003e\u0026ndash;TiO\u003csub\u003e2\u003c/sub\u003e nanocomposites were successfully synthesized based on their XRD patterns. The Debye\u0026ndash;Scherrer equation was used to determine the average crystal sizes, with the crystal sizes of TiO\u003csub\u003e2\u003c/sub\u003e, S1, S2, and S3 measuring 14.76, 13.35, 13.50, and 13.60 nm, respectively. These findings reveal that the crystal sizes of the prepared nanocomposites are closely comparable. The slight discrepancies in crystal sizes between the nanocomposites may be attributed to the interactions' strength between the SiO\u003csub\u003e2\u003c/sub\u003e and TiO\u003csub\u003e2\u003c/sub\u003e particles. It's worth noting that the tiny crystal size of the photocatalyst plays an important role in its photocatalytic activity [\u003cspan citationid=\"CR37\" class=\"CitationRef\"\u003e37\u003c/span\u003e].\u003c/p\u003e \u003cp\u003eThe nanostructure of the synthesized nanocomposites was analysed using Field Emission Gun Scanning electron microscopy to examine surface modifications on TiO\u003csub\u003e2\u003c/sub\u003e. Figure\u0026nbsp;\u003cspan refid=\"Fig6\" class=\"InternalRef\"\u003e3\u003c/span\u003e displays the FEG-SEM images of the nanocomposites at various amplification levels. A careful examination of these FEG-SEM images reveals that the surfaces exhibit a uniform, spherical-like TiO\u003csub\u003e2\u003c/sub\u003e structure with clustered groups. In the case of SiO\u003csub\u003e2\u003c/sub\u003e\u0026ndash;TiO\u003csub\u003e2\u003c/sub\u003e nanocomposites, Si, Ti and O molecules are present on the surface, resulting in the uniform spherical particles on the SiO\u003csub\u003e2\u003c/sub\u003e-TiO\u003csub\u003e2\u003c/sub\u003e surface. This observation indicates a moderate level of physical adsorption of SiO\u003csub\u003e2\u003c/sub\u003e molecules onto the TiO\u003csub\u003e2\u003c/sub\u003e surface.\u003c/p\u003e \u003cp\u003eTo identify the elemental components of all the prepared nanocomposites, Energy-Dispersive X-ray (EDX) analysis was conducted. The EDX spectrum of TiO\u003csub\u003e2\u003c/sub\u003e exhibits peaks corresponding to Ti and O atoms. However, upon examining the EDX data of SiO\u003csub\u003e2\u003c/sub\u003e\u0026ndash;TiO\u003csub\u003e2\u003c/sub\u003e nanocomposites, peaks for Si elements within the SiO\u003csub\u003e2\u003c/sub\u003e structure, as well as the signals for Ti and O elements, are evident. Based on these results, it is evident that the TiO\u003csub\u003e2\u003c/sub\u003e nanocomposites indeed contain SiO\u003csub\u003e2\u003c/sub\u003e compounds. In summary, the FEG-SEM analysis confirmed the presence of a uniform spherical-like structure on the TiO\u003csub\u003e2\u003c/sub\u003e surface, with clustered groups. The EDX analysis revealed the elemental composition, providing unmistakable evidence that the TiO\u003csub\u003e2\u003c/sub\u003e nanocomposites include SiO\u003csub\u003e2\u003c/sub\u003e compounds. The EDX analysis and elemental identification can be found in Fig.\u0026nbsp;\u003cspan refid=\"Fig8\" class=\"InternalRef\"\u003e4\u003c/span\u003e and Table\u0026nbsp;\u003cspan refid=\"Tab2\" class=\"InternalRef\"\u003e2\u003c/span\u003e.\u003c/p\u003e \u003cp\u003e \u003cdiv class=\"gridtable\"\u003e\u003ctable float=\"Yes\" id=\"Tab2\" border=\"1\"\u003e \u003ccaption language=\"En\"\u003e \u003cdiv class=\"CaptionNumber\"\u003eTable 2\u003c/div\u003e \u003cdiv class=\"CaptionContent\"\u003e \u003cp\u003eEDX results for the synthesized nanocomposites\u003c/p\u003e \u003c/div\u003e \u003c/caption\u003e \u003ccolgroup cols=\"4\"\u003e \u003cdiv align=\"left\" class=\"colspec\" colname=\"c1\" colnum=\"1\"\u003e\u003c/div\u003e \u003cdiv align=\"left\" class=\"colspec\" colname=\"c2\" colnum=\"2\"\u003e\u003c/div\u003e \u003cdiv align=\"char\" char=\".\" class=\"colspec\" colname=\"c3\" colnum=\"3\"\u003e\u003c/div\u003e \u003cdiv align=\"left\" class=\"colspec\" colname=\"c4\" colnum=\"4\"\u003e\u003c/div\u003e \u003cthead\u003e \u003ctr\u003e \u003cth align=\"left\" colname=\"c1\"\u003e \u003cp\u003eNanocomposite\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colname=\"c2\"\u003e \u003cp\u003eElements\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colname=\"c3\"\u003e \u003cp\u003ewt %\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colname=\"c4\"\u003e \u003cp\u003eat%\u003c/p\u003e \u003c/th\u003e \u003c/tr\u003e \u003c/thead\u003e \u003ctbody\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003eTiO\u003csub\u003e2\u003c/sub\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003eO\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c3\"\u003e \u003cp\u003e17.42\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c4\"\u003e \u003cp\u003e38.7\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e\u0026nbsp;\u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003eTi\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c3\"\u003e \u003cp\u003e82.58\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c4\"\u003e \u003cp\u003e61.3\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003eS1\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003eO\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c3\"\u003e \u003cp\u003e39.34\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c4\"\u003e \u003cp\u003e61\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e\u0026nbsp;\u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003eSi\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c3\"\u003e \u003cp\u003e20.78\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c4\"\u003e \u003cp\u003e18.35\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e\u0026nbsp;\u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003eTi\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c3\"\u003e \u003cp\u003e39.88\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c4\"\u003e \u003cp\u003e20.65\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003eS2\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003eO\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c3\"\u003e \u003cp\u003e47.14\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c4\"\u003e \u003cp\u003e66.81\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e\u0026nbsp;\u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003eSi\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c3\"\u003e \u003cp\u003e15.74\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c4\"\u003e \u003cp\u003e13.09\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e\u0026nbsp;\u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003eTi\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c3\"\u003e \u003cp\u003e37.13\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c4\"\u003e \u003cp\u003e18.1\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003eS3\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003eO\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c3\"\u003e \u003cp\u003e40.45\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c4\"\u003e \u003cp\u003e65.78\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e\u0026nbsp;\u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003eSi\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c3\"\u003e \u003cp\u003e4.86\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c4\"\u003e \u003cp\u003e4.5\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e\u0026nbsp;\u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003eTi\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c3\"\u003e \u003cp\u003e54.7\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c4\"\u003e \u003cp\u003e29.72\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003c/tbody\u003e \u003c/colgroup\u003e \u003c/table\u003e\u003c/div\u003e \u003c/p\u003e \u003cp\u003eThe spectroscopic analysis of the nanocomposites was conducted using Ultraviolet-Visible Diffuse Reflectance Spectroscopy (UV-DRS) to investigate their light absorption characteristics in detail [\u003cspan citationid=\"CR38\" class=\"CitationRef\"\u003e38\u003c/span\u003e]. The resulting spectra are presented in Fig.\u0026nbsp;\u003cspan refid=\"Fig10\" class=\"InternalRef\"\u003e5\u003c/span\u003e, showcasing the distinct optical behaviors of the materials. Titanium dioxide (TiO\u003csub\u003e2\u003c/sub\u003e), in particular, demonstrates a sharp and well-defined absorption peak at 387 nanometers (nm) within the ultraviolet (UV) region, while no absorption is observed in the visible spectrum. This lack of visible light absorption is attributed to the intrinsic electronic structure of TiO\u003csub\u003e2\u003c/sub\u003e, which features a significantly large band gap energy of 3.2 electron volts (eV). This high band gap energy restricts the excitation of electrons under visible light, thus confining TiO\u003csub\u003e2\u003c/sub\u003e\u0026rsquo;s photoactivity predominantly to the UV range.\u003c/p\u003e \u003cp\u003eIn contrast, the UV-DRS spectra of Silicon dioxide-Titanium dioxide (SiO\u003csub\u003e2\u003c/sub\u003e-TiO\u003csub\u003e2\u003c/sub\u003e) nanocomposites reveal the emergence of absorption bands spanning the 400 to 600 nm range, which are characteristic of Silicon dioxide (SiO\u003csub\u003e2\u003c/sub\u003e) [\u003cspan citationid=\"CR39\" class=\"CitationRef\"\u003e39\u003c/span\u003e]. These features represent a marked deviation from the behavior of pure TiO\u003csub\u003e2\u003c/sub\u003e and indicate a shift in the absorption spectrum toward the visible region. This shift is particularly significant, as it highlights the potential modification of the electronic and optical properties of TiO\u003csub\u003e2\u003c/sub\u003e due to its interaction with SiO\u003csub\u003e2\u003c/sub\u003e. Such changes can be attributed to alterations in the local electronic environment or the formation of new energy states at the interface of the composite material.\u003c/p\u003e \u003cp\u003eThe expanded light absorption range observed in the SiO\u003csub\u003e2\u003c/sub\u003e-TiO\u003csub\u003e2\u003c/sub\u003e nanocomposites is a notable advancement, as it addresses the limitation of TiO\u003csub\u003e2\u003c/sub\u003e's high band gap energy, which hinders effective absorption of visible light. By extending the absorption into the visible spectrum, the SiO\u003csub\u003e2\u003c/sub\u003e-TiO\u003csub\u003e2\u003c/sub\u003e composites demonstrate enhanced light sensitivity, making them promising candidates for applications where visible light activation is desirable. This enhanced optical behavior underscores the synergistic interaction between SiO\u003csub\u003e2\u003c/sub\u003e and TiO\u003csub\u003e2\u003c/sub\u003e within the composite, enabling the tailoring of material properties to suit specific functional requirements.\u003c/p\u003e \u003c/div\u003e \u003cdiv id=\"Sec8\" class=\"Section2\"\u003e \u003ch2\u003eExamination of photocatalytic performance\u003c/h2\u003e \u003cp\u003eThe photocatalytic performance of the synthesized TiO\u003csub\u003e2\u003c/sub\u003e and SiO\u003csub\u003e2\u003c/sub\u003e\u0026ndash;TiO\u003csub\u003e2\u003c/sub\u003e photocatalysts were systematically investigated with respect to the degradation process of methylene blue (MB), a widely used cationic organic dye, under UV-filtered visible light irradiation. MB was selected as a model pollutant due to its cationic nature and its high affinity for adsorption on TiO\u003csub\u003e2\u003c/sub\u003e surfaces, which is facilitated by negatively charged oxygen atoms within its molecular structure [\u003cspan citationid=\"CR40\" class=\"CitationRef\"\u003e40\u003c/span\u003e]. The distinct absorption peak of MB at 664 nm allows for precise and convenient monitoring of its degradation via UV-Visible spectroscopy, where the concentration of the dye can be quantitatively tracked through changes in absorption intensity [\u003cspan citationid=\"CR41\" class=\"CitationRef\"\u003e41\u003c/span\u003e]. Photocatalytic efficiency is recognized to be affected by several parameters, including catalyst loading, particle size, surface area, reaction temperature, pH, and the beginning concentration of the dye [\u003cspan citationid=\"CR42\" class=\"CitationRef\"\u003e42\u003c/span\u003e]. In this study, to ensure the reliability and comparability of results across different photocatalysts, all experimental conditions\u0026mdash;such as photocatalyst dosage, initial concentration, pH value, ambient temperature of MB, and light intensity\u0026mdash;were kept constant. The only variable in these experiments was the type of photocatalyst utilized. It is noteworthy that the pH of the MB solution was consistently maintained at around 6\u0026ndash;7, with no significant fluctuations observed throughout the photocatalytic tests, thereby eliminating pH as a potential factor influencing the degradation process. 3 ppm aqueous solution of methylene blue in deionized water was prepared as the substrate for photocatalytic degradation experiments. From this stock solution, 100 ml aliquots were extracted for each experimental run. To these aliquots, 0.1 g of the respective photocatalyst was added. In order to ensure both sufficient dispersion and adsorption/desorption equilibrium, the dye-catalyst suspensions were first subjected to ultrasonic treatment for 10 minutes. This was followed by a 30-minute incubation period in the dark to account for any non-photocatalytic adsorption effects prior to light exposure. After this pre-treatment phase, an initial 2 ml sample was withdrawn from each solution, and the absorbance spectrum was recorded using a UV-Visible spectrometer to determine the baseline concentration of MB.\u003c/p\u003e \u003cp\u003eThe photocatalytic degradation experiments were conducted in a photoreactor controlled at a controlled temperature of 22\u0026ndash;25\u0026deg;C, and continuous stirring was provided by a magnetic stirrer to ensure homogeneity within the reaction mixture. At predetermined time intervals during the photocatalytic process, 2 ml aliquots were collected for further absorbance measurements. These measurements were taken periodically until the absorbance values reached a minimum, indicating near-complete degradation of the dye. The experimental protocol was repeated for all photocatalysts synthesized in this study to comprehensively assess their photocatalytic efficiency under visible light conditions.\u003c/p\u003e \u003cp\u003eAbsorbance spectra were recorded across the 400\u0026ndash;700 nm wavelength range using a UV-Visible spectrometer. The photocatalytic efficiency was evaluated by monitoring the reduction in absorbance at the characteristic peak of MB (664 nm), and the changes in the spectra were analyzed to quantify the degradation performance. The degradation profiles of all photocatalysts are presented below, highlighting the comparative efficiency of each material in promoting the photocatalytic breakdown of MB under visible light irradiation.\u003c/p\u003e \u003cp\u003eAs represented in Fig.\u0026nbsp;\u003cspan refid=\"Fig13\" class=\"InternalRef\"\u003e6\u003c/span\u003e and Fig.\u0026nbsp;\u003cspan refid=\"Fig14\" class=\"InternalRef\"\u003e7\u003c/span\u003e, it was observed that the aqueous solution of methylene blue was approximately 100% degraded after 2 minutes under the influence of visible light with the S1-coded nanocatalyst. Similarly, the aqueous solution of methylene blue exhibited approximately 100% degradation after 6 minutes under visible light with the S2-coded nanocatalyst, and after 10 minutes with the S3-coded nanocatalyst. This observation provides evidence that an increase in the SiO\u003csub\u003e2\u003c/sub\u003e ratio within the nanocomposite enhances the activity of the photocatalytic material under visible light.\u003c/p\u003e \u003cp\u003eIn addition to their photocatalytic properties, the nanocomposites were further characterized by SEM and EDS analyses, which confirmed their nanoscale structure and homogeneity. The observed nanoscale morphology is critical for maximizing surface area and enhancing photocatalytic interactions with pollutants. A key novelty of this thesis lies in the synthesis approach and its contribution to the literature. Unlike most previous studies where the nanostructures are synthesized separately and later combined through doping processes, this research utilized a hydrothermal method to co-synthesize the SiO\u003csub\u003e2\u003c/sub\u003e and TiO\u003csub\u003e2\u003c/sub\u003e nanocomposite in a single step under identical conditions. This methodological approach is relatively underexplored in the field, offering a more integrated synthesis route that potentially enhances the interaction between the two components, leading to improved photocatalytic performance.\u003c/p\u003e \u003c/div\u003e"},{"header":"Conclusion","content":"\u003cp\u003eIn this study, nano SiO\u003csub\u003e2\u003c/sub\u003e-doped nano TiO\u003csub\u003e2\u003c/sub\u003e nanocomposites were synthesized using the hydrothermal method under varying reaction conditions. The primary motivation for incorporating nano SiO\u003csub\u003e2\u003c/sub\u003e was to improve the photocatalytic efficiency of nano TiO\u003csub\u003e2\u003c/sub\u003e from being limited to UV light to include the visible light spectrum, thereby enhancing its potential applications in broader environmental conditions. The investigation of the structure of the synthesized nanocomposites was carried out through a combination of advanced analytical techniques, including XRD, SEM-EDS, FT-IR, and UV-DRS Spectrophotometry. These techniques confirmed the successful formation of the nanocomposite materials and provided detailed insights into their morphological and compositional features.\u003c/p\u003e \u003cp\u003eThe photocatalytic behavior of the nanocomposites under visible light was studied by studying the degradation of organic dye pollutants, specifically methylene blue. The results demonstrated that the nanocomposites presented significant photocatalytic activity in the visible light region. Among the synthesized samples, the nanocomposite with a 100% SiO\u003csub\u003e2\u003c/sub\u003e/TiO\u003csub\u003e2\u003c/sub\u003e ratio, designated as S1, was found to be the most effective in degrading the organic pollutant, achieving complete degradation of the methylene blue solution within an exceptionally short time of approximately two minutes under visible light irradiation. This rapid degradation rate is a rare phenomenon in the existing literature and highlights the superior efficiency of the S1 nanocomposite, positioning it as a promising material for future photocatalytic applications and further studies.\u003c/p\u003e \u003cp\u003eFurthermore, the study revealed that the photocatalytic efficiency of the nanocomposites varied proportionally with the SiO\u003csub\u003e2\u003c/sub\u003e content. The nanocomposite labeled S2, containing a 50% SiO\u003csub\u003e2\u003c/sub\u003e/TiO\u003csub\u003e2\u003c/sub\u003e ratio, while not as effective as S1, still exhibited noteworthy photocatalytic activity under visible light, demonstrating a significant degradation rate in a relatively short time. The nanocomposite designated as S3, with a 10% SiO\u003csub\u003e2\u003c/sub\u003e/TiO\u003csub\u003e2\u003c/sub\u003e ratio, although less efficient compared to S1 and S2, still outperformed pure anatase TiO\u003csub\u003e2\u003c/sub\u003e in terms of visible light-induced photocatalytic activity. These findings collectively suggest that the incorporation of SiO\u003csub\u003e2\u003c/sub\u003e into the TiO\u003csub\u003e2\u003c/sub\u003e matrix enhances the visible light responsiveness of the nanocomposite, with the photocatalytic activity being closely tied to the SiO\u003csub\u003e2\u003c/sub\u003e content.\u003c/p\u003e"},{"header":"Declarations","content":"\u003cp\u003e\u003cstrong\u003eFunding:\u0026nbsp;\u003c/strong\u003eNo fund is received for this work.\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003eConflict of interest\u003c/strong\u003e: The authors declare no competing interests.\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003eEthics and consent to participate:\u003c/strong\u003e Not Applicable.\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003eConsent for publication:\u003c/strong\u003e No Applicable.\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003eAuthor Contributions Statement\u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003eOğuzhan Avcıata and Mustafa Borucu conceptualized and designed the study. Mustafa Borucu conducted the experiments and performed the data analysis. Semih G\u0026ouml;rd\u0026uuml;k contributed to the interpretation of the data. Mustafa Borucu and Oğuzhan Avcıata drafted the manuscript. Semih G\u0026ouml;rd\u0026uuml;k critically revised the manuscript for important intellectual content. All authors have reviewed and approved the final version of the manuscript and agree to be accountable for all aspects of the work.\u003c/p\u003e"},{"header":"References","content":"\u003col\u003e\u003cli\u003e\u003cspan\u003eJ. Yi, G. Zhang, Y. Wang, W. Qian, X. Wang, Mater. 16(11) (2023) \u003cspan class=\"ExternalRef\"\u003e\u003cspan class=\"RefSource\"\u003ehttps://doi.org/10.3390/ma16113980\u003c/span\u003e\u003cspan address=\"10.3390/ma16113980\" targettype=\"DOI\" class=\"RefTarget\"\u003e\u003c/span\u003e\u003c/span\u003e\u003c/span\u003e\u003c/li\u003e \u003cli\u003e\u003cspan\u003eT. Su, X. 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The reason for doping with nano SiO\u003csub\u003e2\u003c/sub\u003e is to ensure that nano TiO\u003csub\u003e2\u003c/sub\u003e gains photocatalytic activity in the visible region instead of showing photocatalytic properties only under ultraviolet (UV) light. The synthesis process was carried out by changing the nano SiO\u003csub\u003e2\u003c/sub\u003e percentage in order to compare the nanocomposite materials formed in the synthesis part of these photocatalysts in terms of structure and to customize the content. A total of 3 different SiO\u003csub\u003e2\u003c/sub\u003e\u0026ndash;TiO\u003csub\u003e2\u003c/sub\u003e nanocomposites and anatase form of TiO\u003csub\u003e2\u003c/sub\u003e were successfully synthesized using the hydrothermal method. Nano SiO\u003csub\u003e2\u003c/sub\u003e ratios were synthesized in the total nano TiO\u003csub\u003e2\u003c/sub\u003e material as 100%, 50% and 10%, respectively. The structure of the obtained nanocomposite was elucidated by X-ray diffraction (XRD), Scanning Electron Microscopy (SEM), Energy Dispersive Spectroscopy (EDS), Ultraviolet-Visible Diffuse Reflectance Spectroscopy (UV-DRS) and Fourier Transform Infrared Spectroscopy (FT-IR) techniques. Studies on the degradation of organic pollutants of nanocomposite under visible light showed that the obtained nanocomposite exhibits photocatalytic activity under visible light. Additionally, unlike the studies in the literature, SiO\u003csub\u003e2\u003c/sub\u003e and TiO\u003csub\u003e2\u003c/sub\u003e were synthesized from raw materials in the same environment, and synthesis was not performed separately. Due to this feature, it is seen as a method that has less effort and can make a difference compared to previous studies, and that can affect future studies.\u003c/p\u003e","manuscriptTitle":"Hydrothermal Synthesis of Visible Light Photocatalytic SIO2 - TIO2 Nanocomposites","msid":"","msnumber":"","nonDraftVersions":[{"code":1,"date":"2025-03-03 17:08:48","doi":"10.21203/rs.3.rs-6095977/v1","editorialEvents":[{"type":"communityComments","content":0}],"status":"published","journal":{"display":true,"email":"[email protected]","identity":"researchsquare","isNatureJournal":false,"hasQc":true,"allowDirectSubmit":true,"externalIdentity":"","sideBox":"","snPcode":"","submissionUrl":"/submission","title":"Research Square","twitterHandle":"researchsquare","acdcEnabled":true,"dfaEnabled":false,"editorialSystem":"","reportingPortfolio":"","inReviewEnabled":false,"inReviewRevisionsEnabled":true}}],"origin":"","ownerIdentity":"97be6d81-7d5d-486d-874e-217b17f222cc","owner":[],"postedDate":"March 3rd, 2025","published":true,"recentEditorialEvents":[],"rejectedJournal":[],"revision":"","amendment":"","status":"posted","subjectAreas":[],"tags":[],"updatedAt":"2025-03-14T10:38:55+00:00","versionOfRecord":[],"versionCreatedAt":"2025-03-03 17:08:48","video":"","vorDoi":"","vorDoiUrl":"","workflowStages":[]},"version":"v1","identity":"rs-6095977","journalConfig":"researchsquare"},"__N_SSP":true},"page":"/article/[identity]/[[...version]]","query":{"redirect":"/article/rs-6095977","identity":"rs-6095977","version":["v1"]},"buildId":"8U1c8b4HqxoKbykW_rLl7","isFallback":false,"isExperimentalCompile":false,"dynamicIds":[84888],"gssp":true,"scriptLoader":[]}