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NANOSYSTEMS:
PHYSICS, CHEMISTRY, MATHEMATICS Original article
L. Rohmawati, et al. Nanosystems: Phys. Chem. Math., 2022,13 (6), 640-648.
http://nanojournal.ifmo.ru DOI 10.17586/2220-8054-2022-13-6-640-648
The characteristics of TiO2 anatase from tulungagung sand as an antibacterial material
L. Rohmawati1, Istiqomah2, A.A. Pratama1, W. Setyarsih1, N.P. Putri1, Munasir1, Darminto3
1 Physics Department, Faculty of Mathematics and Natural Science, Universitas Negeri Surabaya, Ketintang, Gayungan, Surabaya 60231, Indonesia
2Physics Department, Faculty of Mathematics and Natural Science, Universitas Negeri Malang, Semarang 5, Malang 65145, Indonesia
3Physics Department, Faculty of Science and Data Analytics, Institut TeknologiSepuluh Nopember (ITS), Keputih, Sukolilo, Surabaya 60111, Indonesia
Corresponding author: L. Rohmawati, [email protected]
Abstract TiO2 anatase is a material that has good photocatalytic properties. The synthesis of TiO2 anatase from Tulungagung natural sand used the leaching method. The synthesized samples were characterized by TGA, XRD, FTIR, BET, SEM, UV-DRS and tested for antibacterial effect. In this study, the TiO2 anatase phase was already formed and experiencing three stages of weight loss. It had stretching vibration of the OH group, had a bending mode of water Ti-OH, and Ti-O-Tiat wavenumbers 4000 to 400 cm-1. It also had a mesoporous size, was spherical with a grain size of 58 nm and had an energy gap of 3.42 eV. TiO2 anatase with a 600 ^g/mL concentration could reduce Escherichia coli, Staphylococcus aureus, and Pseudomonas aeruginosa bacteria. Therefore, TiO2 anatase has the potential in an antibacterial agent. Keywords TiO2 anatase, natural sand, antibacterial
For citation RohmawatiL., Istiqomah, Pratama A.A., Setyarsih W., Putri N.P., Munasir, Darminto The characteristics of TiO2 anatase from tulungagung sand as an antibacterial material. Nanosystems: Phys. Chem. Math., 2022, 13 (6), 640-648.
1. Introduction
The rapid development of nanotechnology has increased the number of nanoparticle-based materials. Due to their unique physical properties, nanomaterials have changed their functions in commercial product applications, including food packaging, drug delivery, biosensors and antibacterial agents [1]. One of them is titanium dioxide (TiO2) nano-material, widely studied in the last two decades [2]. TiO2 nanoparticles are considered as an option in biological and environmental remediation applications compared to other semiconductor materials. TiO2 is available in nature, low cost, and non-toxic, has high surface area and has unique physiochemical properties. In addition, this material has also photocatalytic activity, biocompatibility and reasonable thermal stability [3]. TiO2 anatase has a tetragonal structure and is formed at lower temperatures [4]. Anatase has the best photocatalytic properties among the three phases than rutile and brookite [5]. Research of TiO2 in antibacterial agents has been ongoing for the past 20 years. Antibacterial refers to substances that do away or obstruct the growth of microorganisms [6]. Although gram-positive bacteria can form spores and are difficult to inactivate, TiO2 with photocatalytic properties can kill gram-positive and gram-negative bacteria [7]. The antibacterial effect of TiO2 plays an essential role in the medical world because it can kill pathogenic bacteria, such as Escherichia coli, Staphylococcus aureus and Pseudomonas aeruginosa [8]. The antibacterial properties of TiO2 depend on the size of particles and concentration of particles, thus affecting the length of retention time of bacteria [9,10]. Indonesia, especially the Tulungagung region in East Java, has a natural wealth of mineral sand, where the main content in mineral sand is Fe and Ti elements, which are bound to other elements. The elements of Fe and Ti bind to each other to form ilmenite (FeTiO3), hematite (Fe2O3) and magnetite (Fe3O4) compounds [11]. One is the ilmenite compound of the three compounds extracted into titanium dioxide (TiO2) [12]. The anatase compound (TiO2) obtained from the extraction of ilmenite (FeTiO3) is a content of coastal sand that can be used as an antibacterial agent [13].
Several researchers have extracted TiO2 from the Ilmenite sands of the Indonesian island of Bangka with specific methods. Lalasari et al. [14] synthesized TiO2 using the hydrothermal method using NaOH, but as for the results of their research, there were two phases, namely rutile TiO2 and ilmenite (FeTiO3). Aristanti et al. [15] reported that TiO2 could be synthesized using a caustic fusion process using NaOH and a leaching process with H2SO4. As a result, he produced anatase and rutile phases of TiO2 with impurities in the form of a-Fe2O3. Likewise, in Wahyuningsih et al.'s research [16], anatase TiO2 can be synthesized using a dissolution roasted ilmenite process with Na2S followed by a leaching process with H2SO4. The roasted ilmenite process requires a high temperature of 900 °C for 6 hours. Supriyatna et al. [17] also carried out the same process, but the leaching process used HCl solvent, and the products obtained were rutile TiO2 (94.6 %) and ilmenite impurities.
© Rohmawati L., Istiqomah, Pratama A.A., Setyarsih W., Putri N.P., Munasir, Darminto, 2022
Each sand in Indonesia has different characteristics, such as in the Tulungagung area, where it is known that the TiO2 and Fe2O3 contents in the Tulungagung mineral sand are 12.2 and 83.35 %, correspondingly [13]. So far, Tulungagung sand has only been used as a building material, and there has been no further use. Thus, to increase the usefulness of Tulungagung sand, innovation is needed to explore the sand's content. As explained above, TiO2 can be applied as an antibacterial material. Based on the literacy results from previous studies, the antibacterial characteristics of the anatase TiO2 compound from Tulungagung sand have never been reported. The novelty of this research is the analysis of the antibacterial aspect of TiO2 anatase from Tulungagung sand. In addition, anatase TiO2 nanoparticles were synthesized using the leaching method with the chemical solvent 8 M H2SO4 and low temperature in this study. High concentrations of sulfuric acid in the leaching process can produce TiO2 anatase [16]. In this study, Tulungagung mineral sand was not roasted like some of the studies above but was carried out with a simple method, namely taking ilmenite sand from the Tulungagung sand using a magnetic rod carried out by the leaching process. Therefore, the results expect that TiO2 anatase from these natural ingredients can be excellent antibacterial material.
2. Materials and method
2.1. Materials
The materials needed in this research include mineral sand in Tulungagung, East Java, Indonesia, H2SO4 (Sigma Aldrich 99 %), and demineralized water. Equipment needed for the synthesis process includes bar magnet, mortar pestle, 200 mesh sieve, vacuum pump, hot plate stirrer, pH meter, glass beaker, and furnace.
2.2. Experimental methods and data analysis
In the first stage, Tulungagung mineral sand was washed first and dried. The next stage was to separate magnetic and non-magnetic sand using a magnetic rod. After that, the magnetic sand is sieved using a 200 mesh strainer to obtain a fine homogeneous powder. Next was the leaching process, where the powder was dissolved with H2SO4 8 M and heated using a hot plate stirrer at a temperature of 110 °C for 30 minutes until it formed a slurry solution. After that, it was vacuum pumped to separate the TiOSO4 filtrate and FeSO4 precipitate, with reaction presented below:
FeTiO3(s) + 2H2SO4(aq) FeSO4(s) + TiOSO4(aq) + 2H2O(i). (1)
TiOSO4 filtrate was added with distilled water and heated using a hot plate stirrer at 100 °C until forming sediment, with the following hydrolysis reaction:
TiOSO4(aq) + 2H2O(i) TiO(OH)2(s) + H2SO4(aq). (2)
Furthermore, the sediment was washed with demineralized water to obtain a pH of 7, then filtered and calcined at 600 °C during 2 hours, with condensation reaction as:
TiO(OH)2(s) TiO2(s) + H2O(i). (3)
The calcined samples were then characterized by TGA, XRD, FTIR, BET, SEM, UV-DRS, and antibacterial activity test. Thermo Gravimetric Analyzer (TGA) Linseis model STA PT 1000 was used to observe the mass change from the sample thermal decomposition. The phase identification of the sample used data from X-ray Diffraction (XRD) type Phillips X'Pert MPD (multi-purpose diffraction) with monochromatic wavelength CuKa, voltage 40 kV/40 mA and scattering angle of 10 to 90°. The data from the XRD were analyzed qualitatively using the QualX Software. The sample's Ti-O-Ti, Ti-OH, and OH functional groups could be identified by characterization using the Fourier transform infrared (FTIR) brand Shimadzu type IRPrestige 21 with 4000 - 400 cm-1 of wavenumber. The data obtained from the Brunauer-Emmett-Teller (BET) characterization of Quantrachome TouchWin 1.2 type were analyzed using the Barret-Joyner-Halenda (BJH) method to determine the sample pore size and surface area. Characterization Scanning Electron Microscopy (SEM), the Inspect-S50 type FEO, operated at 20 kV, 60 A, magnifying 150,000 times equipped with EDX (Energy Dispersive X-ray), was used to observe the samples' morphology. The grain diameter distribution in the sample was analyzed using ImageJ software. The Ultra Violet-Visible Diffuse Reflectance Spectroscopic (UV-Vis DRS) characterization of the Analytical Jena type Specord 200 Plus was carried out to observe the UV-visible absorbance spectrum in samples with 190 - 800 nm of wavelength. The data from UV-DRS could also be identified as the sample bandgap using Tauc plot analysis.
2.3. Preparation of antibacterial test
Antibacterial testing on samples was carried out using the International Normative ASTM E2149-10 standard on gram-positive (Staphylococcus aureus) and gram-negative (Escherichia coli and Pseudomonas aeruginosa) bacteria. The first stage was to perform cell culture of each bacterium in a stationary phase and measure it using a spectrometer of 600 nm. After that, it was stored in liquid medium and incubated at 37 °C until it reached bacterial concentration 108 CFU/mL. To obtain the concentration of bacteria about 105 CFU/mL, it was carried out three times dilute from 1/10. In the second stage, sample TiO2 powder was dissolved with water demineralized until it formed suspension. The sample TiO2 with concentrations of 100, 200, 300, 400, 500, and 600 ^g/mL were each given a bacterial solution with a
105 CFU/mL concentration and irradiated using a UVA lamp for 3 hours. Then each 10 ^L of the test solution was grown in a petri dish at 37 °C for 24 hours, and observations were made.
3. Results and discussion
3.1. Thermo gravimetric analysis (TGA)
Thermogravimetric analysis allows one to study the magnitude of the reduction in sample weight due to thermal treatment, with the test starting at room temperature up to 850 °C. Based on the TGA curve (Fig. 1), one concludes that there were three stages of sample weight loss with increasing temperature, and significant weight loss occurred at temperatures less than 580 °C. After 580 °C, the thermogravimetric curve was almost flat, indicating that the sample did not lose weight up to 680 °C. The sample weight loss was easier to observe using a weight derivative of thermogravimetric curve. In the first stage, the sample lost weight at a temperature of 200 to 330 °C by 8.1 % because the absorbed water was dehydrated. At a temperature of 330 to 580 °C in the second stage, the sample experienced a weight loss of 10.53 % due to the decomposition of hydroxyl compounds and changes due to the crystallization process from the amorphous phase to anatase transformation. The product was utterly transformed into the anatase TiO2 phase at 580 °C. The same observation at this temperature had also been reported by Zablotsky et al. [18] where TiO2 anatase was fully formed at 560 °C. There was no weight loss at a temperature of 580 to 640 °C, so there was no phase change. The third stage was a phase change from the anatase to rutile phase at 680 to 810 °C followed by 9.5 % sample weight loss because of removal of impurity. At last, at the temperature of 810 until 850 °C, the curve was almost flat.
Fig. 1. TGA and the first derivative weight of sample
3.2. X-ray diffraction (XRD)
The diffraction pattern of the synthesized sample is shown in Fig. 2. The data obtained from XRD were analyzed using QualX software to identify the TiO2 anatase phase. The diffractogram in Fig. 2 shows that the anatase phase TiO2 has been completely formed in the sample. The anatase phase is formed at a diffraction angle of 25.35°. It is the highest diffraction intensity with crystal orientation (101). Other diffraction peaks which show the anatase phase is 37.03, 37.86, 38.6, 48.11, 53.94, 55.09, 62.13, 62.76, 68.80, 70.32, 75.08, 75.35, and 82.73 ° with miller indices (013), (004), (112), (200), (105), (211), (213), (204), (116), (220), (215), (301), and (224), which are appropriate with Joint Committee on Powder Diffraction Standard (JCPDS) data number 9015929. The results are similar to those reported by several researchers [19-21].
3.3. Fourier transform infrared (FTIR)
The chemical bonding functional group of a sample can be determined by FTIR characterization. This characterization was carried out using infrared spectroscopy in the wavenumber of 4000 - 400 cm-1. The results of the FTIR characterization can be seen in Fig. 3. In this study, the synthesized samples had absorption peaks at wave numbers of 3423.76, 1641.48, 1087.89, 669.32, 551.15 cm-1. Firm absorption peaks at wave numbers 551.15 and 669.32 cm-1 indicated Ti-O-Ti bonds in the TiO2 lattice and were characteristic of TiO2 anatase [21]. Al-Taweel and Saud [22] also observed this type of bond and Dicastillo et al. [23], namely, the absorption peak occurred at 700 - 400 cm-1 of wavenumber. The absorption peak at a wavenumber of 1087.89 cm-1 was a stretching or deviational vibration of the Ti-O-Ti bond in TiO2 [24]. The peak of 1641.48 cm-1 showed a bending mode of water Ti-OH which indicated the presence of some
Fig. 2. XRD pattern of sample
H2O [23,25] and was a type of scissors deformation of adsorbed water protonation [26,27]. The functional groups at 3423.76 cm-1 of wavenumber indicated stretching vibration of the OH group [23] and adsorbed water molecules [28]. The same results were also observed by several researchers, Al-Taweel and Saud [22], who reported that the absorption peak at 3600 - 3400 cm-1 indicated an intermolecular connection in the hydroxyl group for water molecules with TiO2 surfaces. The functional group hydroxyl group had an essential role in the microbicidal mechanism [29,30].
3.4. Brunauer-Emmett-Teller (BET)
Pore size, pore structure and pore surface area in the sample can be investigated using BET characterization. Fig. 4 shows that the isotherm curve forms a hysteresis loop in the relative pressure range (0.9 - 1.0 P/P0). The TiO2 isotherm curve formed belongs to the V type with the H1 type hysteresis loop in the form of a cylindrical pore, which shows the characteristics of mesoporous materials [31]. The adsorption-desorption isotherm curve has an open end, wherein the adsorption process nitrogen gas will be absorbed and enter the pores; thus, the volume of nitrogen gas absorbed will be greater than that released. When used as antibacterial material, it has the potential to inhibit bacteria well. Several researchers have revealed that the mesoporous material in TiO2 is very efficient as an antimicrobial agent [32,33].
Fig. 3. FTIR spectra of sample
Fig. 4. The isotherms of sample
Based on the analysis of Barret Joyner Hallenda (BJH), it is known that the pore size distribution of the synthesized sample from the desorption curve (Fig. 5) is 3.06 nm (pore radius 15.31 A). The size belongs to the mesoporous category (2 nm < d < 50 nm). The BET analysis represents that the TiO2 sample had 727,590 m2/g of surface area. This value is greater than the results of several researchers, including 266 m2/g [33], 65.65 m2/g [34], 124 m2/g [35]. The large pore surface area possessed by the synthesized TiO2 sample can be the main determining factor in increasing antimicrobial activity because it provides good contact between nanoparticles and microorganisms [36].
0 10 20 30 40 50 60 70 80 90 100 Pore radius (a)
Fig. 5. Desorption curve on the sample
3.5. Scanning electron microscopy (SEM)
Figure 6 depicts the surface morphology of the anatase TiO2 sample. The figure shows that the sample's morphology is spherical, although there is still agglomeration at some points. Based on the Energy Dispersive X-ray (EDX) results, 100 % anatase TiO2 samples were formed from Ti and O elements without any other elements.
Analysis of the grain size distribution of the anatase TiO2 sample using ImageJ software, the results of which are shown in Fig. 7. The grain size of the anatase TiO2 sample is 58 nm, which results from considering about 100 grains, indicating a size smaller than 100 nm, and includes nanoparticles.
3.6. Ultra violet-visible diffuse reflectance spectroscopic analysis (UV-Vis DRS)
The absorbance of the sample at a specific wavelength of light can be determined using UV-DRS analysis. In Fig. 8(a), it appears that the sample has a strong UV absorption with a wavelength of less than 400 nm. However, at a wavelength
40 60 80 100
Diameter (nm)
Fig. 7. Distribution of sample grain sizes from SEM image
in visible light, no absorption is observed by the sample in this region. It means that the photon energy at that wavelength does not stimulate electrons to move to a higher energy level [37]. The energy gap of the sample can be determined using the Tauc plot analysis, the results of which can be seen in Fig. 8(b). The sample has an energy gap of 3.42 eV and includes TiO2 anatase [38,39].
3.7. Antibacterial behaviour
In this study, the bacteria used were E. coli, E. aureus, and P aeruginosa, with concentrations of TiO2 200, 300, 400, 500, and 600 ^g/ml. Table 1 displays the antibacterial behaviour of TiO2 with several cell concentrations and log reduction. Bacteria dissolved in demineralized water without UV radiation were used as a control. When irradiated with UV light, TiO2 showed antibacterial activity characterized by wane in the number of bacteria as the concentration of TiO2 increased. It shows that UV radiation can obstruct the growth of bacteria. The 600 ^g/mL concentration of TiO2 has the highest inhibitory ability for both gram-positive and gram-negative bacteria which is characterized by the number of live bacteria around 3.7 • 103 CFU/mL. At concentrations of 400 to 600 ^g/mL, it was found that there was a slight decrease in the number of live bacterial colonies for E. coli, S. aureus, and P. aeruginosa bacteria, as shown in Fig. 9, where it was inhibited the number of bacterial growth although slowly. It is because the dilution factor affects the diffusion process, where a high concentration of TiO2 allows low solubility, causing limited diffusion rates. It influences the ability of TiO2 to inhibit the growth of bacteria such as E. coli, S. aureus, and P. aeruginosa. Valgas et al. [40] stated that the deposition of antibacterial compounds could cause a limited diffusion rate. This study was limited to a concentration of 600 ^g/mL. It is because the data at that concentration is already sufficient to show the ability of TiO2 as an antibacterial in both gram-positive and gram-negative bacteria.
The antibacterial behaviour of TiO2 can be explained by an oxidation reaction when exposed to UV radiation [41]. TiO2 surface exposed to UV radiation will produce hydroxyl and superoxide, reactive oxygen species (ROS). The surface
Fig. 8. (a) Uv-vis spectra of sample, (b) UV-Tauc plot of sample
Table 1. Antibacterial behaviour of TiO2 at different concentrations
Bacteria Escherichia coli Staphylococcus aureus Pseudomonas aeruginosa
TiO2 Cell conc. Log Cell conc. Log Cell conc. Log (^g/mL) (CFU/mL) Reduction (CFU/mL) Reduction (CFU/mL) Reduction
0 2.6 105 5.41 ± 0.03 3.4 105 5.54 ± 0.04 2.6 ■ 105 5.41 ± 0.11
200 4.0 104 4.60 ± 0.02 4.3 104 4.63 ± 0.09 2.8 ■ 104 4.44 ± 0.15
300 3.3 104 4.51 ± 0.05 2.9 104 4.46 ± 0.02 2.1 ■ 104 4.32 ± 0.12
400 4.5 103 3.65 ± 0.11 3.8 103 3.57 ± 0.04 2.1 ■ 103 3.32 ± 0.08
500 4.1 103 3.61 ± 0.09 3.2 103 3.50 ± 0.03 1.8 ■ 102 2.25 ± 0.06
600 3.7 103 3.50 0.07 3.4 102 2.53 0.03 1.2 102 2.07 0.09
Fig. 9. Antibacterial activity with the concentration of TiO2
of the bacteria will come into contact with TiO2 particles, which are oxidized when exposed to UV radiation. Makowski and Wardas [42] stated that the generation of reactive oxygen compounds could destroy bacteria through damage to bacterial cell walls. Observation of the TiO2 antibacterial activity for 24 hours showed that TiO2 was effective in obstructing the accretion of S. aureus, P. aeruginosa, and E. coli. The antibacterial activity of S. aureus and P. aeruginosa as grampositive bacteria was higher than that of E. coli as gram-negative bacteria. It is because the three bacteria have different cell wall structures and thicknesses [41]. Cell wall helpfulness is to protect bacteria from antibacterial compounds that can enter and kill bacteria. The cell wall structure of gram-negative bacteria is more complex and has a layer of peptido-glycan, and a layer of lipopolysaccharide, which acts as a barrier to the entry of antibacterial compounds into bacterial cells. Gram-negative bacteria are more resistant to antibacterial from TiO2 when compared to gram-positive bacteria.
In contrast, gram-positive bacteria have no lipopolysaccharide layer, allowing antibacterial compounds to enter the cell and cause lysis. The single-layered gram-positive cell wall structure is relatively simple, making it easier for antibacterial compounds to enter cells and inhibit bacterial growth. In addition to cell wall thickness, the duration of UV radiation also affects the antibacterial activity of TiO2. TiO2 concentration of 600 ^g/mL was able to reduce bacteria E. coli, S. aureus and P. aeruginosa, respectively 3.7 • 103; 3.4 • 102 and 1.2 • 102 CFU/mL. The longer the UV radiation, the more ROS produced and can obstruct the growth of more bacteria. The size of TiO2 nanoparticles also inhibited bacterial growth [39].
4. Conclusion
TiO2 anatase has been successfully synthesized from mineral sands of Tulungagung using the hydrothermal leaching method in this study. The characteristics of TiO2 anatase can be seen from the results of XRD, TGA, FTIR, BET, SEM, UV-DRS, and antibacterial tests on E. coli, S. aureus, and P. aeruginosa bacteria. The results of the characterization include: TiO2 anatase phase has been formed, has 3 stages of weight loss, has Ti-O-Ti, Ti-OH, and OH functional groups. It also had a pore size of 3.06 nm with a surface area of 727.590 m2/g and mesoporous category. The synthesized TiO2 had a spherical morphology with a grain size of 58 nm. TiO2 had strong absorption of UV light with a wavelength of less than 400 nm and had an energy gap of 3.42 eV. TiO2 with a 600 g/mL concentration had the most optimum reducing ability on E. coli, S. aureus and P. aeruginosa bacteria, respectively 3.7 • 103; 3.4 • 102 and 1.2 • 102 CFU/mL for 24 hours.
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Submitted 15 November 2021; revised 14 June 2022; accepted 16 October 2022
Information about the authors:
L. Rohmawati - Physics Department, Faculty of Mathematics and Natural Science, Universitas Negeri Surabaya, Ket-intang, Gayungan, Surabaya 60231, Indonesia; [email protected]
Istiqomah - Physics Department, Faculty of Mathematics and Natural Science, Universitas Negeri Malang, Semarang 5, Malang 65145, Indonesia; [email protected]
A. A. Pratama - Physics Department, Faculty of Mathematics and Natural Science, Universitas Negeri Surabaya, Ket-intang, Gayungan, Surabaya 60231, Indonesia; [email protected]
W Setyarsih - Physics Department, Faculty of Mathematics and Natural Science, Universitas Negeri Surabaya, Ketintang, Gayungan, Surabaya 60231, Indonesia; [email protected]
N. P. Putri - Physics Department, Faculty of Mathematics and Natural Science, Universitas Negeri Surabaya, Ketintang, Gayungan, Surabaya 60231, Indonesia; [email protected]
Munasir - Physics Department, Faculty of Mathematics and Natural Science, Universitas Negeri Surabaya, Ketintang, Gayungan, Surabaya 60231, Indonesia; [email protected]
Darminto - Physics Department, Faculty of Science and Data Analytics, Institut Teknologi Sepuluh Nopember (ITS), Keputih, Sukolilo, Surabaya 60111, Indonesia; [email protected]
Conflict of interest: the authors declare no conflict of interest.
