Abstract
The modified aqueous co-precipitation approach was used to successfully manufacture magnesium dititanate (MgTi2O5) nanoparticles. Thermogravimetric analysis/differential scanning calorimetry (TG/DSC) was used to clearly reveal the thermal stability. Moreover, pseudobrookite structure, and surface morphology of MgTi2O5 nanoparticles were determined using X-ray diffraction (XRD), transmission electron microscope (TEM), and Fourier-transform infrared (FT-IR), and scanning electron microscope (SEM) techniques, respectively. The average size of the crystallites calculated by Scherer approach was compared to Williamson-Hall and TEM images results. The optical band gap of MgTi2O5 nanoparticles was found to be 3.81 eV for direct transitions. The effect of temperature on the conductivity of DC electricity was tested between the rages 303–503 K. The data on antibacterial activity showed that MgTi2O5 nanoparticles were antimicrobial and stopped the test microorganisms from growing. These findings revealed that MgTi2O5 will be extensively promising in environmental pollution control and antibacterial research.
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1 Introduction
Due to their low bulk thermal expansion, the pseudobrookite-type crystal structure-based pigments were developed to provide heat-resistant coloring agents for thermoplastics, industrial paints, and other low-temperature applications. Their various ceramics that have pseudobrookite-type structures (such as MgTi2O5 and Fe2TiO5) were studied. MgTi2O5 with a pseudobrookite-type system has potential applications owing to its good mechanical properties, good thermal stability, and high thermal shock resistance [1,2,3,4,5,6,7]. Furthermore, MgTi2O5 has a high refractive index, high permittivity, low cost, and no dielectric loss [8, 9]. Many techniques, including solid-state reaction, conventional high-temperature, thermal decomposition of precursors, simultaneous hydrolysis, sol–gel method, and co-precipitation, sol–gel, and other methods, have been used in recent years to synthesize MgTi2O5 like-pseudobrookite structure materials [10,11,12,13,14,15,16,17,18].
Pseudobrookite materials have attracted considerable attention as a potential photocatalyst material that might be extensively employed in environmental pollution remediation and antibacterial research [18, 19]. MgTi2O5 has been used for diesel particulate filters with high-temperature steadiness. In addition, MgTi2O5 has been utilized as a porous ceramic membrane and can be used as a white pigment, electrical resistor, catalyst, water purification filter, and photocatalyst [10, 14]. There has been considerable interest in the development of antibacterial materials and coatings for many years. This interest is growing due to the growth of antibacterial-resistant bacteria over the last decade and the prevalence of healthcare-associated illnesses (HCAIs). Anti-anti-bacterial may be used to minimize infection rates in a patient setting, but they also be used in waste-water treatment and the efficient production of clean drinking water via the augmentation of sun sterilization[20,21,22]. The research gap for the study of the antimicrobial activities of MgTi2O5 nanoparticles is significant. There is no published research on this topic and the potential antimicrobial properties of MgTi2O5 nanoparticles have not been investigated at all. In addition to these specific research gaps, there is also a need to develop new methods for synthesizing and characterizing MgTi2O5 nanoparticles. This would enable researchers to produce MgTi2O5 nanoparticles with controlled size, shape, and surface properties, which is important for optimizing their antimicrobial activity. Further research is needed to address the research gaps identified above and to develop MgTi2O5 nanoparticles with optimal antimicrobial activity and safety.
As a result, the current study’s purpose is to synthesize MgTi2O5 nanoparticles using co-precipitation, which is a quick, simple, ecologically friendly, and practical method. XRD, TG/DSC, FT-IR, SEM, EDX, TEM, UV–Vis spectroscopy, and DC measurements were used to analyze the structure, shape, and electrical conductivity of the MgTi2O5 nanoparticles generated, respectively. Antibacterial properties of MgTi2O5 nanoparticles were researched and evaluated.
2 Experimental details
2.1 Preparation of MgTi2O5 nanoparticles
The building blocks for making magnesium dititanate (MgTi2O5) were magnesium chloride (MgCl2) and titanium tetrachloride (TiCl4). Isopropanol, hydrogen peroxide (H2O2), and ammonia solutions (NH4OH) are also utilized. All the reaction materials were used as received without further purification. MgCl2 and TiCl4 were both dissolved in 100 ml of distilled water and isopropanol, respectively, at a concentration of 0.2 mol of each. A new homogeneous solution was created by combining the two produced solutions. Next, 15 ml of hydrogen peroxide, 20 ml of ammonia, and 165 ml of distilled water are combined to make a solution. A precipitate was generated and filtered after adding MgCl2 and TiCl4 to the prepared solution combination drop by drop. The resulting precipitate was separated by centrifuging and washing it repeatedly with distilled water. The material was then dried in an oven set at 75 °C for six hours and calcined for approximately an hour in a muffle furnace set at around 800 °C. The reactions that go into making MgTi2O5 nanoparticles are shown in Scheme 1.
2.2 Characterization
Thermal analysis was carried out using LINSEIS STA PT-1000 to investigate the thermal stability of MgTi2O5 nanoparticles (about 25 mg of the sample was taken and heated at a rate of 10 °C/min to 800 °C). The XRD pattern was recorded for MgTi2O5 nanoparticles using X-ray diffractometry (Brucker AXS D8 Advance X-ray diffractometer). The sample morphology was investigated using SEM (model JEOL-JSM-IT200). TEM (JEOL, JEMA 2100) equipped with an EDX detector was used to examine crystallites for their form, size, and elemental composition. Chemical characterization of MgTi2O5 nanoparticles was investigated using an FT-IR spectrometer (JASCO, Model 6100) at room temperature in the 400–4000 cm−1 range with a resolution of 4 cm−1. Using a diffuse reflectance UV–Vis spectrophotometer (JASCO 670 UV–Vis-NIR spectrophotometer) with an integrating sphere and a spectral reflectance standard across the range (200–800) nm Discs containing MgTi2O5 nanoparticles were compressed (at 5 tons) and then sintered at 1000 °C in the air for 30 min in order to investigate their electrical conductivity. The silver paste was used to make electrical connections. The DC electrical conductivity of the sample was measured using an electrometer (KEITHLEY 6517A) linked directly to the sample. The temperature of system was regulated in a specific range (303–503 K) with an accuracy of roughly ± 1 K using a temperature controller.
2.3 Antibacterial activity
The antimicrobial effectiveness of the obtained MgTi2O5 nanoparticles was investigated. The tested strains of bacteria were Escherichia coli (E. coli) bacteria (ATCC25922, gram-negative) and Enterococcus faecalis bacteria (ATC29212, Gram-positive). Muller–Hinton agar was used as a culture medium at pH = 7.3 ± 0.1, and then an incubation period of 24–48 h at 37 °C was carried out for the plates [23, 24]. Antibacterial efficiency was specified for the mentioned bacteria by the method of paper disc assay. The Whatman filter paper disc was sterilized using an autoclave at 121 °C for 20 min. To determine the MIC (minimum inhibitory concentration), a concentration of the MgTi2O5 nanoparticles was used, as shown in Table 1. The sterile discs were impregnated with the determined concentration of MgTi2O5 (25 mg/mL) and then diluted [24]. Agar plates were injected into the broth of the used microorganisms with a uniform concentration of approximately 1.5 × 108 CFU ml−1. Chloro-amphenicol with a concentration of 50 mg/mL was applied against the used bacteria as an effective control. The diameter of the growth inhibition halos caused by the examined compounds was calculated and expressed in millimeters. The applied tests were checked in triplicate.
3 Results and discussion
3.1 Structural properties
The thermal stability of MgTi2O5 nanoparticles is investigated using TGA and DTA curves, as displayed in Fig. 1. The weight loss from room temperature to 150 °C is about 28%, and the endothermic peak around 82 °C could be related to the presence of adsorbed water and the structural hydroxyl groups. The exothermic sharp peak at 107 °C corresponds to the beginning of the decomposition of the residual organic precursor groups of Ti-tetrachloride and Mg-chloride. In the range of 150–500 °C, the mass change is about 7% and has a broad exothermic peak around 285 °C. That is attributed to the completed decomposition of the organic deposits and the starting of OH-group (dehydroxylation) removal; this means that MgTi2O5 phase formation begins [25, 26]. The exothermic peak at 509 °C shows the crystallization of the obtained powders. The small mass loss in the range 500–800 °C is accompanied by an action that can be referred to as the elimination of OH-group decomposition [7, 25]. It is obvious that the formation and crystallization of the MgTi2O5 compound occur [1, 12, 27, 28].
The XRD pattern of MgTi2O5 nanoparticles synthesized by precipitation technique is shown in Fig. 2. Comparing the XRD pattern to the standard database (JCPDS) revealed that it belonged to the MgTi2O5 compound. The phase analysis of the sample is done using X’pert high score plus program, and the result is matched with JCPDS 82-1125. The estimated unit cell parameters and their values are indicated in Table 2. From Fig. 2, it can be indicated that there are no other phases presented (i.e., pure orthorhombic phase MgTi2O5). That means that no other impurity peaks are detected. The average crystallite size L is calculated using the Debye–Scherrer formula [29,30,31,32,33].
where, θ is Bragg’s angle, β is the FWMH (full width at half maximum) in radian, λ = 0.15406 nm is the wavelength of the used X-ray, and K = 0.94 is constant. The two key factors responsible for the change in peak broadening in an XRD pattern are crystallite size and lattice strain. The dispersion of lattice constants due to defects in the crystal structure is quantified using the Williamson-Hall (W–H) technique is used to assess the L and assuming that two components contribute to peak broadening and are independent of one another, the observed peak width is expressed as the sum of L and H, as shown in the following W–H equation [34]:
Figure 3 depicts a plot with \(4\mathrm{sin\theta }\) along the x-axis and \({\upbeta }_{\mathrm{hkl}}\mathrm{cos\theta }\) along the y-axis for MgTi2O5 nanoparticles. L is determined from the y-intercept and from the slope of Fig. 3 based on the linear fit to the data. The quantity of defects and vacancies (dislocation density, δ) in the MgTi2O5 can be determined using L and the following equation [33,34,35]:
Values of L, δ, and ε for MgTi2O5 are obtained by the Scherer and Williamson-Hall treatments are shown in Table 2. Due to the elimination of the strain contribution to the FWHM of the XRD peak by W–H analysis, the crystallite size obtained by W–H analysis is slightly higher than that predicted using the Scherrer formula [33].
Various magnifications SEM images of MgTi2O5 nanoparticles prepared are shown in Fig. 4(a–c). SEM images show the interconnected spherical microstructure of MgTi2O5, which clearly shows the formation of spherical particles. The particle shapes are quasi-round and have the ability to combine, forming agglomerates of a few hundred nanometers in the 0.4–1.5 µm size range.
Figure 5(a and b) shows TEM images of MgTi2O5 nanoparticles at various magnifications. The MgTi2O5 nanoparticles are homogeneous, well distributed, quasi-round, and tend to aggregate and form clusters. The TEM images show that the MgTi2O5 nanoparticles are composed of nanoscale crystallites with an average size of around 30 nm. This value is quite close to the findings produced by W–H and Scherrer’s approach. EDX analysis is used to verify the homogeneity of the resulting MgTi2O5 nanoparticles. The EDX spectrum of MgTi2O5 nanoparticles is shown in Fig. 6. The significant peaks in the spectrum corresponded to titanium, magnesium, and oxygen elements. Also, the metallic ratios of Ti, Mg, and O elements match well with the expected elemental ratio, which indicates that the synthesized nanoparticles are MgTi2O5.
The FT-IR spectra for MgTi2O5 nanoparticles are displayed in Fig. 7. The wideband at 3425 cm−1 is imputed to the stretching of the O–H group of water [36]. The intensive peak at 1630 cm−1 is due to the bending vibrations of H2O particles [37]. The two bands at 1518 cm−1 and 1420 cm−1 are ascribed to the stretching vibrations of C–O and C–H, respectively [38]. The stretching of the O–H group of water is attributed to the wideband at 3425 cm−1 [36]. The bending vibrations of H2O particles cause an intense peak at 1630 cm−1 [37]. The stretching vibrations of C–O and C–H are attributed to the two bands at 1518 cm−1 and 1420 cm−1, respectively. The existence of bending vibrations of the intercalated Mg–O and Ti–O bonds is shown by the weak band at 500 cm−1 and the weak band at 605 cm−1 [38], respectively, demonstrating the development of a pure nanocomposite form of synthesized MgTi2O5.
3.2 Optical properties of MgTi2O5 nanoparticles
The optical properties of MgTi2O5 nanoparticles are studied using diffuse reflection spectra. Reflectance spectroscopy (RS) is utilized for powders that are difficult to analyze by transmission measurements. Reflectance measurements are divided into two categories: internal and exterior reflectance. To investigate the diffuse reflectance spectra that weakly absorbing materials produce, use the Kubelka–Munk hypothesis. The Kubelka–Munk equation for any wavelength is written as the following equation [39, 40]:
where R is the sample reflectance and F(R) is the Kubelka–Munk function. Figure 8 shows the diffuse reflectance of the MgTi2O5 nanoparticles. The synthesized MgTi2O5 nanoparticles absorbed mainly UV light, as shown in Fig. 9. The optical band gap \({\mathrm{E}}_{\mathrm{g}}\) of MgTi2O5 can be calculated using a rewritten version of Tauc’s equation [41,42,43,44,45] for diffuse reflectance calculations [40]:
where α is the coefficient of absorption (\(\alpha =\mathrm{F}\left(\mathrm{R}\right)\mathrm{h\nu }/\mathrm{t}\)), \(\mathrm{h\nu }\) is the photon energy, t is the pellet thickness (approximately 0.5 mm), and r is a constant that defines the nature of optical transitions. Also, A is a constant known as the Tauc parameter that provides insight into the disorder in the sample [43,44,45,46], and its value may be calculated from the slope of the straight line. In the case of MgTi2O5, the best fit for Eq. (5) is obtained at r = 1/2, suggesting that the type of electronic transition is direct allowed transitions, which is demonstrated in Fig. 10. The value of \({\mathrm{E}}_{\mathrm{g}}\) is determined from the intercept of the plot of \({\left(\mathrm{F}\left(\mathrm{R}\right)\mathrm{h\nu }/\mathrm{t}\right)}^{2}\) versus \(\mathrm{h\nu }\) for direct transition, as shown in Fig. 10 which is equal to 3.81 ± 0.01 eV. Moreover, the value of A1/2 is equal to 776 ± 2 (cm eV)1/2. The optical bandgap value of MgTi2O5 nanoparticles is matched with some previously reported work on their doped and thin-film materials [2, 12, 28, 47].
3.3 Electrical conductivity of MgTi2O5 nanoparticles
The electrical conductivity of the synthesized MgTi2O5 nanoparticles was investigated through the temperature-dependent conductivity within the range of temperature (303–503 K). Figure. 11 shows the DC electrical conductivity of the prepared MgTi2O5 nanoparticles. It is shown from Fig. 11 that the DC conductivity increases as temperature rises. The curve in Fig. 11 can be divided into three linear regions (1, 2, and 3). The electrical conductivity in these regions can be estimated by the following equation [39, 48, 49]:
where σdc is the dc electrical conductivity, σo is the electrical conductivity at zero temperature, kB is Boltzmann’s constant, ΔEσ is the activation energy of the three regions, and T is the absolute temperature. From the slope and intercept of the straight lines of the curve, the variation in activation energy of MgTi2O5 nanoparticles for different temperature regions can be determined (ΔEσ1, ΔEσ2 and ΔEσ3, and σo1, σo2, and σo3). Estimated values for region (1) at the lower temperature range, region (2) at the intermediate temperature range, and region (3) at the higher temperature range are tabulated in Table 3, respectively. In intrinsic semiconductors, it is probable that the activation energy is less than half the value of the optical energy gap, which is already convenient with the determined values ΔEσ1, ΔEσ2, and ΔEσ3 for MgTi2O5 nanoparticles. The electrical study shows that the electrical conduction mechanism for the MgTi2O5 nanoparticles is thermally activated, and the DC conductivity enhances exponentially in the used temperature range (303–503 K), where the electrons are thermally excited from donor levels to the conduction band with temperature increasing. The determined values of the activation energy match the levels of defect energy in the optical bandgap of the MgTi2O5 nanoparticles. The results denote that these materials are promising for electronic device applications, as reported by previous researchers [49,50,51,52].
3.4 Antibacterial activity of MgTi2O5 nanoparticles
The present study examines the antibacterial properties of MgTi2O5 nanoparticles for the purpose of ensuring safety and promoting health. The minimum inhibitory concentration (MIC) is determined based on concentrations of nanoparticles impregnated onto sterile discs, as outlined in Table 1. The antibacterial activity of tested MgTi2O5 nanoparticles is determined by the existence of clear inhibition zones. It was seen that increasing the concentration of MgTi2O5 nanoparticles led to the inhibitory zone expanding faster. Different types of bacteria and different amounts of MgTi2O5 nanoparticles can cause the inhibitory zone to have different sizes. Table 4 presents the recorded values of the inhibitory zone for the bacterial strains employed in this study, namely E. coli and E. faecalis. The average values of the inhabitation zone often fall within the range of 10–15 mm. According to the data presented in Fig. 12 and Table 4, the observed highest growth inhibition zone for E. coli was 11 mm, whereas for E. faecalis, the maximum inhibition halo measured 14 mm. Hence, the findings pertaining to the antibacterial activity of MgTi2O5 indicate that the nanoparticles produced by MgTi2O5 exhibit notable efficacy in inhibiting bacterial growth.
MgTi2O5 nanoparticles’ distinctive features make them interesting for antibacterial applications from a physics point of view. MgTi2O5 nanoparticles have a high surface-to-volume ratio, meaning they have a large surface area. This enormous surface area allows MgTi2O5 nanoparticles to interact with bacteria in several ways. Physical disruption of bacterial cell membranes is one way MgTi2O5 nanoparticles interact with bacteria. The sharp edges of MgTi2O5 nanoparticles may penetrate the cell membrane, leaking and killing germs. MgTi2O5 nanoparticles may interact with bacteria by generating reactive oxygen species (ROS). ROS are reactive chemicals that destroy microorganisms. MgTi2O5 nanoparticles create ROS through photocatalysis [53]. In addition to their antibacterial characteristics, MgTi2O5 nanoparticles offer additional antimicrobial benefits. Biocompatible MgTi2O5 nanoparticles are safe for living things. MgTi2O5 nanoparticles are cheap to create, making them a viable large-scale antibacterial contender.
4 Conclusions
Facile co-precipitation method was used to synthesis MgTi2O5 nanoparticles that have a structure similar to pseudobrookite. The synthesized MgTi2O5 nanoparticles were thermally analyzed using TGA and DSC. The crystallite sizes measured by the Scherer and W–H equations were in the 27–37 nm range. MgTi2O5 nanoparticles were found to have quasi-round forms in SEM and TEM images. The direct band gap (3.81 ± 0.01 eV) of the synthesized MgTi2O5 nanoparticles was investigated using diffuse reflectance spectra. The temperature-dependent conductivity in the temperature range was used to study the DC electrical conductivity (303–503 K). These temperature-dependent measurements display that the electrical conduction mechanism for the MgTi2O5 nanoparticles was dominated by thermally activated processes. MgTi2O5 nanoparticles had excellent antibacterial capability and were effective against both gram-positive and gram-negative bacterial strains. Thus, it was concluded that the MgTi2O5 nanoparticles will be promising for antimicrobial applications and water purification.
Data availability
This manuscript has associated data in a data repository. [Authors’ comment: all data included in this manuscript are available upon request by contacting the corresponding author.]
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Elnobi, S., Abuelwafa, A.A., Abd El-sadek, M.S. et al. Facile synthesis and physical properties of magnesium dititanate nanoparticles for antibacterial applications. Indian J Phys 98, 2417–2427 (2024). https://doi.org/10.1007/s12648-023-03028-9
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DOI: https://doi.org/10.1007/s12648-023-03028-9