antibacterial fabric coating material
To cite this article: B F Bukit et al 2022 J. Phys.: Conf. Ser. 2165 012022
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Preparation and characterization of CTAB surfactant
modified TiO
2nanoparticles as antibacterial fabric coating material
B F Bukit1, E Frida2*, S Humaidi2 and P Sinuhaji2
1Doctoral Program Department of Physics, Universitas Sumatera Utara, 20155, Medan, Indonesia
2Department of Physics Universitas Sumatera Utara, 20155, Medan, Indonesia
E-mail: [email protected]
Abstract. TiO2 preparation has been carried out with the addition of cetyl trimethyl ammonium bromide (CTAB) surfactant. The sol-gel method is used in the preparation of TiO2, where TiCl4
is used as a precursor. The resulting TiO2 was characterized using XRD, FTIR, XRF and SEM.
XRD results show the crystal size of TiO2 17.75 nm with the rutile phase. The FTIR results show a broad absorption band between 800 and 400 cm−1 by Ti–O vibrations in the crystal lattice. The XRF results showed that the TiO2 content was 80.80%. Morphological results showed an irregular ball-like structure that was less aggregated. The characterization results show that TiO2 can be used as a coating on fabrics with antibacterial properties.
1. Introduction
In the last decade, nanostructured materials have attracted significant attention. Size and phase control of nanomaterials can be helpful in a wide variety of applications. For example, titanium dioxide (TiO2) is one of the most attractive materials widely used in various applications [1]. In addition, TiO2
accounts for 70% of the total volume of pigment production worldwide and is included in the top five nanoparticles used [2].
Titania is naturally formed in four main phases: rutile, anatase, brookite, and TiO2(B). The stability of the four phases of titania depends on the particle size. The rutile phase is thermodynamically stable, but anatase is the most stable phase at sizes below 14 nm. Brookite and TiO2(B) are metastable forms that are not commonly observed in minerals and are challenging to synthesize in pure form [3]. In photocatalytic activity, the anatase and rutile phases have an essential role. Thermodynamically, the anatase phase is less stable than the rutile. The structure of anatase and rutile can be described as an octahedral chain of TiO6 in which six O2 surrounds each Ti4+ ion- ions; both crystal structures are distinguished by their octahedral distortion octahedral chain arrangement pattern. The photocatalytic properties of TiO2 can be utilized in the treatment of water contaminated with sewage, as a self- cleaning and anti-bacterial material on fabrics and anti-fogging on glass [4], [5]. The photocatalytic properties of TiO2 can be used when TiO2 is irradiated with light, and the bandgap will produce electron and hole pairs which cause a redox reaction on the surface of TiO . As a result, electrons will
2
is cost-effective [8]. On the other hand, the wet phase or sol method is the best way to control particle size, shape and composition [9]. This control can be achieved by using molecular precursors in combination with organic molecules. Organic molecules act to direct the structure in solution to control and limit the growth of the structure. To obtain small-sized crystals, about < 50 nm, a surface stabilizer can be used to prevent agglomeration and increase solubility. The surface stabilizer is because nanostructures are usually unstable in solution and tend to agglomerate to minimize their surface energy. Stabilization of this system can be achieved by using steric or electrostatic interactions to keep the particles apart. One of the steric interactions carried out is by adding surfactants. These surfactants can slow down the formation of the titania lattice [10].
The use of surfactants has been investigated to produce porous materials [11]. The sol-gel method uses a non-ionic surfactant as a template, such as the sol-gel method's synthesis of TiO2 thin films.
Among the surfactants studied, Tween 80 is the most promising surfactant in film homogeneity, UV absorbance, methylene blue adsorption, and can control the volume and pore size [12]. Mesoporous TiO2 material was synthesized using PVA as a surfactant agent. Synthesis was carried out by sol-gel, ultrasonic, and hydrothermal methods. Mesoporous TiO2 can remove inorganic and organic pollutants because of the large pore volume of TiO2 synthesized using surfactants [13]. The surfactant cetyl trimethyl ammonium bromide (CTAB) has been commonly used to control particle size in methods such as the sol-gel and hydrothermal methods, and non-ionic surfactants such as P123 have also been used to obtain nanorods and nanoneedle structures. However, it should be emphasized that due to the nature of surfactants (anionic, cationic or non-ionic), their behaviour may differ depending on the solvent used for synthesis and the pH level of the medium, leading to differences in morphology and other properties [14], [15].
In this study, TiO2 was synthesized using the sol-gel method where TiCl4 was used as a precursor, and by adding CTAB surfactant, the results of this study were later used as a coating material on fabrics with antibacterial properties.
2. Methods
TiO2 synthesis was carried out using the sol-gel method using TiCl4 as a precursor. First, TiCl4 was mixed with distilled water and stirred for 2 hours using a magnetic stirrer. While stirring, the NH4OH solution is added to the solution little by little until the solution is white for 4 hours at 70 oC. Next, the reaction product in the form of a gel, separated and washed with deionized water to remove chlorine ions. Then CTAB surfactant was added and stirred again. Finally, the gel was dispersed into 300 ml of ethanol solution. The precipitate was dried at 70 oC for 5 hours. From the results of this study, a sample code (TiO2 CTAB) was made. The schematic of the synthesis of TiO2 nanoparticles is shown in Figure 1.
Figure 1. Schematic of TiO2 Nanoparticle Synthesis.
3. Result and Discussion
3.1. X-Ray Diffraction (XRD) Characterization
X-ray diffraction (XRD) analysis was used to measure particle size and structural analysis of commercial TiO2, and TiO2 sol-gel process and CTAB surfactant used a Goniometer type Shimadzu 6000 instrument with a Cu/Kα1 X-ray source with a wavelength, = 1, 54056. The analysis was carried out with an angle of 2θ ranging from 7o to 70o. In addition, the crystal size (D) of the material is carried out using the Debye Scherrer equation.
10 20 30 40 50 60 70
(211)
(110) (220)(101)
Intensity (a.u)
2 Tetha (deg)
TiO2 CTAB (b) TiO2 Comersil (a)
(a) (b)
(101) (200)(004) (105) (211) (204)
(111) (301)(116)
Figure 2. Diffraction pattern of a). Commercial TiO2, b). TiO2 CTAB.
From Figure 2. The diffraction pattern on commercial TiO2 is obtained; the maximum intensity is found at an angle of 2θ = 25.525° with a distance of 3.4897, has an anatase phase (TiO2). Room group I41/amd(141). has a tetragonal system with lattice parameters a = 3.777 c = 9.501 and has a mass of 3.915 g/cm³ with dhkl (101). The particle size of commercial TiO2 obtained from XRD using the Debye Scherrer method is 32.16 nm. Meanwhile, for TiO2 nanoparticles synthesized with CTAB surfactant, the maximum intensity is found at an angle of 2θ = 27.65° with a distance of 3.2414 having a rutile phase (TiO2). The results of the X-ray diffraction pattern have a tetragonal system of space group P42/mnm (136) with lattice parameters a = 4.584 c = 2.953 and have a mass of 4.248 g/cm³ with dhkl (110). The particle size of TiO2 with CTAB surfactant obtained from XRD using the Debye
4
Figure 3. SEM a). Commercial TiO2, b). TiO2 CTAB.
The SEM results in Figure 3b of the nanoparticles become less agglomerated than commercial TiO2
due to the presence of a long CTAB hydrocarbon chain that prevents agglomeration. As a result, a less aggregated irregular ball-like structure is seen in TiO2 CTAB [18], [19].
3.3. Fourier-transform Infrared Spectroscopy (FTIR) Characterization.
Characteristics of the compounds that compose it. One chemical property is brought from the functional groups of the compounds that make up the material. Each functional group of the compound has specific energy to vibrate in several modes. The energy absorbed by each functional group is detected to vibrate in various modes. The amount of energy absorbed (frequency) can be determined by what compounds are contained in the material. Several other aspects of the measurement can be used as material to analyze the material being tested. It can be characterized using FTIR.
4000 3500 3000 2500 2000 1500 1000 500
C-H C-H
3682.95
660.79 C-H
C-H C=CC-H
Transmittance (%)
Wavenumber (cm-1)
TiO2 CTAB(b) TiO2Com(a)
a b
926.70 1637.5
3284.09
3248.3 1637.51412.5 819.31
2015,9
C=C O-H
Figure 4. FTIR Nanoparticles a). Commercial TiO2, b). TiO2 CTAB.
Figure 4 shows a broad absorption band between 800 and 400 cm−1 correspondings to Ti–O vibrations in the crystal lattice. The broad absorption bands between 3600 and 3000 cm−1 and bands at 1637 cm−1 are due to the deformation and strain vibration of the OH group, respectively, and these
bands indicate the presence of weakly bound water molecules on TiO2. This characteristic is needed in photocatalysis because the OH group can react with holes and prevent the recombination of electron- hole pairs. The 2,015.9 absorption band in the FTIR spectrum of the CTAB samples can be attributed to the CH bond vibrations of the methyl and methylene groups, respectively, of the surfactant residues [20]–[22].
3.4. X-Ray Fluorescence (XRF) Characterization
XRF characterization of TiO2 samples was carried out using XRF PANalytical Minipal 4. This tool can be used to test the elemental content of a material ranging from Sodium-Uranium. Samples can be solid, powder and liquid. The X-ray tube of this instrument allows the use of different target materials to avoid the possibility of masking the sample spectrum with the tube spectrum. The rhodium target is standard, with chromium, molybdenum and tungsten target materials available as options. Table 1 shows the compound content of commercial TiO2 and TiO2 CTAB obtained from characterization using XRF.
Table 1. Compound content of commercial TiO2 and TiO2 CTAB.
Compound TiO2 Comersil (%)
TiO2 CTAB (%)
TiO2 99.01 80.80
K2O 0.14 -
CaO 0.10 0.18
P2O5 0.31 -
Fe2O3 - 0.75
Cl - 16.5
V2O5 - 0.64
WO3 0.26 -
PtO2 0.18 0.089
BrO - 0.15
Yb2O3 - 0.17
ZnO - 0.13
The content of commercial TiO2 compounds is 99.01%, while TiO2 CTAB is 80.80%, followed by 16.5 Cl. Thus, the Cl content is most likely obtained from the TiCl4 residue that is not entirely lost.
Likewise, the presence of BrO content most likely comes from CTAB [23], [24]. TiO2 can be used as a coating because it has antimicrobial properties on photocatalyst activity. TiO2 coating can prevent the emergence of gram-positive bacteria, gram-negative bacteria, viruses, and fungi. When TiO2 is irradiated with light, the bandgap will produce electron-hole pairs, which cause a redox reaction on the TiO2 surface. Therefore, electrons will move from the valence band to the conduction band so that a pair of electrons and holes will be formed on the surface of the photocatalyst. Negatively charged electrons and oxygen will combine to form O2- while positively charged holes and water will produce hydroxyl radicals. Therefore, various radical oxygen species (ROS) can be oxidized to carbon dioxide (CO2) and water (H2O) [25].
4. Conclusion
From the results of preparation and characterization of TiO2 nanoparticles modified by CTAB surfactants, it was found that these materials can be used as coatings on fabrics. After the modification, there was a decrease in particle size and a reduction in agglomeration of TiO2 CTAB compared to commercial TiO2. The rutile phase obtained from TiO2 CTAB allows photocatalyst activity to prevent bacterial contamination. In addition, with the modification, the TiO2 content is sufficient. TiO2 as a
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