Open AccessArticle

Synthesis and Characterization of MgO-Fe₂O₃/γ-Al₂O₃ Nanocomposites: Enhanced Photocatalytic Efficiency and Selective Anticancer Properties

Department of Physics and Astronomy, College of Science, King Saud University, Riyadh 11451, Saudi Arabia

King Abdullah Institute for Nanotechnology, King Saud University, Riyadh 11451, Saudi Arabia

Author to whom correspondence should be addressed.

Catalysts 2024, 14(12), 923; https://doi.org/10.3390/catal14120923

Submission received: 15 November 2024 / Revised: 10 December 2024 / Accepted: 11 December 2024 / Published: 14 December 2024

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Abstract

In the present work, we achieved the fabrication of MgO-Fe₂O₃/γ-Al₂O₃ NCs using a deposition–coprecipitation process. XRD, TEM, and SEM with EDX, XPS, FTIR, and PL spectroscopy were applied to examine the physicochemical properties of the samples. XRD analysis confirmed the successful incorporation of γ-Al₂O₃, MgO, and Fe₂O₃ phases. TEM and SEM images indicate that the nanocomposites exhibited an agglomerated morphology with spherical shapes and particle sizes in the range of 6–12 nm. EDX and XPS spectra revealed a composition of MgO-Fe₂O₃/γ-Al₂O₃ NCs. FTIR spectra identified characteristic vibrational bands corresponding to the chemical bonds present in the samples, confirming their successful synthesis. PL analysis showed the reduced recombination rate of electron–hole pairs and enhanced charge separation efficiency, which are important factors for improved photocatalytic activity. Photocatalysis results show that the MgO-Fe₂O₃/γ-Al₂O₃ NCs exhibited significantly higher photocatalysis efficiencies of 87.5% for Rh B and 90.4% for MB after 140 min, compared to γ-Al₂O₃ NPs and Fe₂O₃/γ-Al₂O₃ NPs. In addition, prepared MgO-Fe₂O₃/γ-Al₂O₃ NCs demonstrated superior stability after six runs. Biochemical data showed that the MgO-Fe₂O₃/γ-Al₂O₃ NCs exhibited significant toxicity toward A549 cancer cells while displaying low toxicity toward IMR90 normal cells. The IC₅₀ values (µg/mL ± SD) for γ-Al₂O₃ NPs, Fe₂O₃/γ-Al₂O₃ NPs, and MgO-Fe₂O₃/γ-Al₂O₃ NCs were 16.54 ± 0.8 µg/mL, 14.75 ± 0.4 µg/mL, and 11.40 ± 0.6 µg/mL, respectively. These results suggest that the addition of Fe₂O₃ and MgO to γ-Al₂O₃ not only enhances photocatalytic activity but also improves biocompatibility and anticancer properties. This study highlights that the MgO-Fe₂O₃/γ-Al₂O₃ NCs warrant further exploration of their potential applications in environmental remediation and biomedicine.

Keywords:

MgO-Fe₂O₃/γ-Al₂O₃ nanocomposite; coprecipitation method; photocatalytic degradation; electron–hole recombination; anticancer activity

1. Introduction

In the field of nanotechnology, nanocomposites (NCs) have emerged as one of the most promising nanomaterials in potential applications due to their excellent physicochemical properties [1,2]. By integrating different nanoscale materials, researchers have been able to develop advanced materials that exhibit improved functionality in areas such as catalysis, photonics, and biomedicine [3,4]. Specifically, organic pollutants in water environments have become a serious environmental emergency due to the fast population increase and human health in developing countries, which remains a major research challenge [5]. To address these issues, semiconductor photocatalysts have been applied as one of the ways to remove these organic pollutants [6,7]. On the other hand, cancer is a common issue in worldwide health, with 13–17 million new cases estimated in 2020, 60% of which were in developed countries [8]. Currently, traditional approaches such as proton therapy, heat treatment, photodynamic therapy, laser therapy, sentinel lymph node biopsy, and cryotherapy are applied to treat cancer [9,10]. Resistance drugs are one of the challenges in using these approaches in a therapeutic system. Nanomaterials, with dimensions below 100 nm, offer unique properties for cancer diagnostics and therapeutics [11,12].

Recently, the gamma aluminum oxide (γ-Al₂O₃) nanoparticles (NPs) have shown potential applications in environmental remediation, biomedicine, and optoelectronics due to their unique physicochemical properties. Various approaches, including nonthermal plasma [13], sol–gel methods [14], arc discharge in water [15], solvent deficiency [16], co-precipitation [17], and hydrothermal methods [17], can be used to synthesize these NPs. Significantly, these approaches can be used to synthesize different NPs to enhance their photocatalytic and therapeutic performance. Abbas et al. [18] synthesized the MgO NPs through a laser ablation process with high antibacterial performance. In addition, a one-step hydrothermal process was used to produce α-Fe₂O₃ nanostructures by Nassar et al. [19]. Additionally, Mohammadi-Aghdam et al. [20] employed the green method to synthesize Ag-ZnO NPs using hedera colchica extract with improved catalytic, anticancer, and antibacterial activity owing to their unique properties.

Doping, co-doping, supporting, and nanocomposite approaches are carried out to enhance the properties of metal oxide NPs in their photocatalytic and medical applications [21]. However, recent studies have explored the synthesis, physicochemical, photocatalytic, and biomedical application for different metal oxide NPs and NCs such as Ag-doped ZnO NPs, γ-Al₂O₃ NPs [22], MgO NPs [23], Fe₂O₃ NPs [24], MgO/Fe₂O₃ NCs [25], and MgO-γ-Al₂O₃ NPs [26]. Similarly, et al. [27] reported that the Ag/Fe₂O₃ NPs exhibit enhanced photocatalytic, antibacterial, and anticancer performance in comparison with pure Fe₂O₃ NPs. Different hybrid nanocomposites (NCs), such as Fe₃O₄/CuO/ZnO/NGP NCs [28], CuO/α-Fe₂O₃/γ-Al₂O₃ NCs [29], NiO/Fe₂O₃/ZnO NCs [30], and CdO/ZnO/MgO NCs [31], have been of interest for use in photocatalytic applications. For instance, Munawar et al. [32] showed that ZnO/CeO₂/Yb₂O₃ NCs have excellent photocatalytic and antibacterial properties. In another example, Khormali et al. [33] reported that the Dy₂O₃/ZnO-Au NCs achieved excellent photocatalytic and antibacterial properties compared to pure ZnO NPs. Additionally, Nassar et al. [34] reported that the TiO₂/Zn₂TiO₂/ZnO/C exhibit excellent photocatalytic performance compared to each sample.

Different nanoparticles (NPs), metal oxide NPs, and their compounds have been of potential interest for their evaluation in anticancer and antibacterial performance. For instance, γ-Al₂O₃ NPs exhibit promising anticancer effects on K562 cells [35] and A549 lung cancer cells [36]. Similarly, Hashemi et al. [36] assessed the anticancer and antibacterial activity of Ag NPs. Likewise, Se NPs have been successfully prepared using green synthesis and have been investigated for their cytotoxicity against breast cancer cells (MCF-7) [37]. In another example, Alangari et al. [38] studied the anticancer potential of Fe₂O₃ NPs against various cell lines, including HeLa, A549, and MDA-MB-231 cells. Kiani et al. [39] showed that the addition of Ag ions to ZnO played a role in enhancing antibacterial and anticancer properties compared with pure ZnO NPs. Karimi et al. [40] reported that synthesized MgO/C-dot/DOX NCs exhibited better-quality photocatalytic and anticancer activity compared with pure MgO NPs. In addition, synthesized Fe₃O₄/CdWO₄/PrVO₄ NCs exhibited high photocatalytic efficiency and cytotoxicity against pancreatic cancer cells that were investigated by Marsooli et al. [41].

The present study is focused on the optimization of the physicochemical properties of the γ-Al₂O₃ NPs through the addition of MgO and Fe₂O₃ NPs via the deposition–coprecipitation process to enhance photocatalytic and selective anticancer performance. The physicochemical properties of the MgO-Fe₂O₃/γ-Al₂O₃ NCs were carefully investigated through XRD, TEM, and SEM with EDX, XPS, FTIR, and PL spectroscopy. The photocatalytic performance of the prepared samples was evaluated by measuring the degradation of MB and Rh B dyes under UV irradiation. For biological assessment, the anticancer and biocompatibility effects of the samples have been fruitfully investigated in A549 cancer cells and normal IMR90 cells.

2. Results and Discussion

2.1. Structural Studies

Figure 1a–c display the XRD patterns of the prepared

γ

-Al₂O₃ NPs, Fe₂O₃/

γ

-Al₂O₃ NPs, and MgO-Fe₂O₃/

γ

-Al₂O₃ NCs. The XRD spectra (Figure 1a) of the

γ

-Al₂O₃ NPs demonstrate the sharp and well-defined peaks at 2θ values of 31.9°, 36.8°, 45.5°, and 66.8° corresponding to the (220), (311), (400), and (440) planes, respectively. These peaks confirmed that synthesized

γ

-Al₂O₃ NPs are the crystallinity and purity, as reported in earlier studies [42,43]. As illustrated in Figure 1b, the additional peaks characteristic of the supported Fe₂O₃ NPs were embedded within the

γ

-Al₂O₃ NPs [44]. As reported in a previous study [45], the addition of 4% Fe dopant produced a change in the crystalline structure of the Al₂O₃ NPs. Figure 1c displays the XRD patterns of the synthesized MgO-Fe₂O₃/

γ

-Al₂O₃ NCs. It can be seen in Figure 1c that the peaks at 21.8°, 34.9°, and 62.9° correspond to the supported MgO NPs, Fe₂O₃ NPs, and

γ

-Al₂O₃ phases, respectively. These peaks indicate a composite structure with interactions between MgO, Fe₂O₃, and

γ

-Al₂O₃. Our XRD results confirmed the diffraction peaks attributed to the

γ

-Al₂O₃, MgO, and Fe₂O₃ phases. The presented results are in good agreement with previous studies [46,47,48].

2.2. Morphological Characterization

2.2.1. TEM Analysis

Figure 2a–c depict the TEM and HRTEM images and SAED analysis of prepared NPs and NCs. It can be observed that the higher magnification of the HRTEM images of each sample is presented as an interpolated image within the corresponding main image. As shown in Figure 2a–c, the TEM and HRTEM images of the

γ

-Al₂O₃ NPs reveal a uniform spherical shape and high crystallinity, with clear details of the crystal lattice in the images and distinct diffraction spots in the SAED patterns [44]. The d-spacing of the

γ

-Al₂O₃ NPs (Figure 2b) was 0.239 nm, corresponding to the (311) plane, which agreed with the XRD data. Compared with the pure

γ

-Al₂O₃ NPs (Figure 2a), the Fe₂O₃/

γ

-Al₂O₃ NPs (Figure 2d) had smaller sizes and clearer structures corresponding to the

γ

-Al₂O₃ NPs and Fe₂O₃ phases. SAED analysis (Figure 2f) demonstrated the effective integration of Fe₂O₃ within the

γ

-Al₂O₃ NPs with d-spacings of 0.232 nm and 0.262 nm for the

γ

-Al₂O₃ NPs with Fe₂O₃, respectively. As shown in the TEM and HRTEM images (Figure 2j,k), the synthesized MgO-Fe₂O₃/

γ

-Al₂O₃ NCs exhibit complex, irregular structures with clear agglomeration. However, SAED patterns show intense diffraction spots and rings and d-spacings of 0.150 nm, 0.219 nm, and 0.200 nm for MgO, Fe₂O₃, and

γ

-Al₂O₃ NPs, respectively [46]. These values indicate the occurrence of advanced structural interactions between the components. As shown in the histogram inside the TEM images, the average particle sizes of the

γ

-Al₂O₃ NPs, Fe₂O₃/

γ

-Al₂O₃ NPs, and MgO-Fe₂O₃/

γ

-Al₂O₃ NCs are 8.68 ± 0.9 nm, 11.12 ± 0.3 nm, and 6.41 ± 0.3 nm, respectively. Similarly, a previous study [49] revealed that prepared Fe₂O₃/Al₂O₃ NPs have shown the presence of α-Al₂O₃ and α-Fe₂O₃ phases with particle sizes of 7–9 nm. As shown in the results, these fine structural analyses confirm the efficient synthesis and integration of NPs and NCs, emphasizing their potential in catalytic and therapeutic applications. Our TEM images are consistent with previous research, highlighting the outstanding performance of mixed metal oxide NCs in advanced application fields [50,51].

2.2.2. SEM and EDX with Elemental Mapping Analysis

The morphological and surface properties of the produced samples were investigated using the SEM technique as illustrated in Figure 3a–c. It can be observed that the particles of the NPs and NCs are spherical in shape with barely distinguishable contours, as reported in reviews from the literature [52,53]. Specifically, SEM images of the MgO-Fe₂O₃/

γ

-Al₂O₃ NCs (Figure 3c) revealed irregular shapes with increased agglomeration, indicating strong interactions between MgO and Fe₂O₃ within the

γ

-Al₂O₃ NPs, which is in agreement with these studies [54,55]. Remarkably, the sizes of the produced NPs and NCs and their distributions in these samples are difficult to determine due to the high agglomeration of particles. EDX spectra (Figure 3d) confirmed the presence of Mg, Fe, Al, and O in the prepared MgO-Fe₂O₃/

γ

-Al₂O₃ NCs. We observed that these percentages of elements were nearly consistent with the source materials obtained through synthesis. SEM elemental mapping of distribution for the MgO-Fe₂O₃/

γ

-Al₂O₃ NCs reveals distinct spatial patterns of Mg, Fe, and Al elements in the sample surface. It can be seen that Mg, Fe, Al, and O were more homogeneously distributed in the synthesized MgO-Fe₂O₃/

γ

-Al₂O₃ NCs, as supported by the EDX data (Figure 4d). The SEM images and EDX results, as well as the mapping results of the prepared samples, showed excellent agreement with previous studies [56,57].

2.3. XPS Analysis

The chemical compositions and oxidation states of the samples were investigated using XPS analysis. Figure 5a–e display the XPS spectra of the pure

γ

-Al₂O₃ NPs, Fe₂O₃/

γ

-Al₂O₃ NPs, and MgO-Fe₂O₃/

γ

-Al₂O₃ NCs. The XPS survey spectra (Figure 5a) confirmed that the peaks corresponding to the chemical compositions of Al, Fe, Mg, and O were present in the prepared sample. Furthermore, the high-resolution XPS spectra of Al 2p, Fe 2p, O 1 s, and Mg 2p are presented in Figure 5b–e, respectively. In Figure 5b(i), the binding energy (B. E) of the pure

γ

-Al₂O₃ NPs is associated with 73.76 eV, 74.65 eV, and 75.02 eV for Al 2p, while the XPS peaks of the Al 2p of the MgO-Fe₂O₃/

γ

-Al₂O₃ NCs (Figure 5b(ii)) were assigned at 73.60 eV, 74.68 eV, and 75.20 eV, respectively, in agreement with previous studies [58,59]. In comparison, the B. E of the Al 2p peak in the prepared sample is slightly shifted. Similarly, the binding energy (B. E) of Fe 2p in the Fe₂O₃/

γ

-Al₂O₃ NPs (Figure 5c(i)) at 723.33 eV, 715.23 eV, 717.46 eV, 720.61 eV, and 727.10 eV are observed, while they associated with 712.72 eV, 714.17 eV, 716.43 eV, 721.31 eV, and 726.96 eV for the MgO-Fe₂O₃/

γ

-Al₂O₃ NCs (Figure 5c(ii)). These values are in good agreement with these previous investigations [59,60,61]. As observed in the shift in the B.E value of Fe 2p, there is a strong interaction between Fe₂O₃ and the

γ

-Al₂O₃ NPs. Additionally, the oxygen vacancies of the prepared NPs and NCs were determined through XPS analysis for O 1s. Figure 5d(i) shows that the O 1s peak in the

γ

-Al₂O₃ NPs at 530.29 eV and 531.78 eV is due to the C–O–C and C=O bonds, respectively [62]. The B.E values of the O 1s peak shifted to 531.75 eV and 533.27 eV, respectively. Moreover, the XPS peaks corresponding to the Mg 2P peak in the MgO-Fe₂O₃/

γ

-Al₂O₃ NCs are shown in Figure 5e. We revealed that the B. E values of the Mg 2p peak at 50.93 eV, 52.30 eV, and 53.89 eV are attributed to the Mg–O band as compared with these studied [63,64]. XPS results confirmed structural insights into the prepared samples, emphasizing the importance of understanding these shifts in peak positions for use in photocatalytic and medical applications.

2.4. FTIR Study

Figure 6a–c shows the FTIR spectra of the pure

γ

-Al₂O₃ NPs, Fe₂O₃/

γ

-Al₂O₃ NPs, and MgO-Fe₂O₃/

γ

-Al₂O₃ NCs. The absorption bands in Figure 1a–c for all the samples were located at 570.87 cm⁻¹ and 801.16 cm⁻¹, which correspond to the characteristic stretching vibrations of the Al-O bonds in

γ

-Al₂O₃, as reported in these studies [62,65,66]. In agreement with Khodadadi et al., FTIR analysis of

γ

-Al₂O₃ has exhibited absorption bands at 580 cm⁻¹ and 802 cm⁻¹, corresponding to octahedral AlO₆ and tetrahedral AlO₄ sites. The characteristic stretching vibrations of Fe-O and Mg-O are associated with 1013.10 cm⁻¹ and 668.12 cm⁻¹, respectively. Nevertheless, the broad bands in Figure 6a–c for the prepared NPs at 1641.54 cm⁻¹ and 3434.59 cm⁻¹ are due to the O-H vibration and stretching of surface hydroxyl groups, respectively [67]. Additionally, the band at 1402.11 cm⁻¹ in these samples represents the C-O stretching band. In contrast, the intensity of the band between 400 cm⁻¹ and 800 cm⁻¹ for the prepared NPs and NCs increased owing to the addition of the stretching vibrations of Fe-O and Mg-O bonds [68]. This phenomenon confirmed the presence of MgO and Fe₂O₃ phases within

γ

-Al₂O₃ [69,70]. FTIR results highlighted the synergistic interactions between MgO, Fe₂O₃, and

γ

-Al₂O₃ in the nanocomposite structure, as reported in the XRD and XPS results (Figure 1 and Figure 5).

2.5. Photoluminescence Analysis

The recombination rate between of electron–hole pairs of the prepared samples is determined via PL spectroscopy. Figure 7 shows the PL spectra of the

γ

-Al₂O₃ NPs, Fe₂O₃/

γ

-Al₂O₃ NPs, and MgO-Fe₂O₃/

γ

-Al₂O₃ NCs at room temperature and with an excitation wavelength of 320 nm. Therefore, the emission peak of the prepared samples was observed at 340.50 nm in the UV light region. Moreover, emission in the blue-green region (400–465 nm) was also detected, as reported in a previous study [71]. After supporting Fe₂O₃ with

γ

-Al₂O₃ NPs, we observed that the PL intensity decreased due to the decreased recombination rate of charges. Wang et al. [72,73] observed that synthesized

γ

-Al₂O₃ NPs have reduction of the PL intensity due to addition of both MgO and Fe₂O₃. Another previous study by Kaur et al. [74] showed that the Fe-doped MgO NPs exhibited reduced bandgap and PL emissions, which were attributed to surface defects. Likewise, the decrease in the PL intensity of the Fe₂O₃/

γ

-Al₂O₃ NPs (Figure 7) was strongly decreased by supporting the MgO NPs. This reduction in recombination rate can be attributed to enhanced electron transfer efficiency from the valence band (VB) of Fe₂O₃ to the VB of γ-Al₂O₃, improving charge separation efficiency. PL spectra revealed that the MgO-Fe₂O₃/

γ

-Al₂O₃ NCs could be applied in catalytic and cancer therapy applications.

2.6. Photocatalytic Study of NPs and NCs

Figure 8a and b illustrate the results of the photocatalysis of Rh B dye under direct UV light for an exposure time of 140 min. Nevertheless, the decrease in the UV absorption (Figure 8a) of the Rh B solution using the MgO-Fe₂O₃/

γ

-Al₂O₃ NCs was attributed to the decreased recombination rate between the electron (e−)–hole (h⁺) pairs. As shown in Figure 8c, the constant rate for pure

γ

-Al₂O₃ NPs, Fe₂O₃/

γ

-Al₂O₃ NPs, and MgO-Fe₂O₃/

γ

-Al₂O₃ NCs were used for Rh B photocatalysis were 0.00618 min⁻¹, 0.00798 min⁻¹, and 0.01193 min⁻¹, respectively. Additionally, the

γ

-Al₂O₃ NPs, Fe₂O₃/

γ

-Al₂O₃ NPs, and MgO-Fe₂O₃/

γ

-Al₂O₃ NCs (Figure 8d) achieved degradation efficiencies (%) of 56.3%, 69.2%, and 87.5%, respectively, as illustrated in Table 1.

At the same experimental conditions, the results of photocatalytic degradation of MB dye under UV irradiation for 140 min using prepared samples are shown in Figure 9a–d. Similarly, the UV-vis absorption spectra of the MB dye solution around 664 nm (Figure 9a) show the degradation behavior under photocatalytic activity. As observed in Figure 9a, the UV absorption of MB solution degradation for MgO-Fe₂O₃/

γ

-Al₂O₃ NCs was decreased with increasing exposure time. This indicates that prepared MgO-Fe₂O₃/

γ

-Al₂O₃ NCs have excellent ability to degrade organic pollutants. In Figure 9b, the plot of C_t/C₀ vs. irradiation time displays the relative concentration of MB dye (Ct) at any time (t). The kinetic analysis in Figure 9c illustrates the pseudo-first-order kinetics of the photocatalysis process. The constant rate of MB degradation of samples was 0.00598 min⁻¹, 0.00876 min⁻¹, and 0.01574 min⁻¹, respectively. The linearity of the plot (Figure 9c) provides a quantitative measure of the degradation speed. However, the kinetic constant rate (K) of the photocatalysis of MB dye is shown in Table 1. The photocatalysis efficiency (D%) of the synthesized samples is illustrated in Figure 9d. As presented in Table 1, the degradation efficiencies of MB by the synthesized

γ

-Al₂O₃ NPs, Fe₂O₃/

γ

-Al₂O₃ NPs, and MgO-Fe₂O₃/

γ

-Al₂O₃ NCs were 57.3%, 71.7%, and 90.4%, respectively, after 140 min. These values indicate the ability of the catalyst to degrade MB dye under UV exposure efficiently. A comparison of the degradation efficiencies of different dyes with those reported by various catalysts is presented in Table 2. In summary, the synthesized MgO-Fe₂O₃/

γ

-Al₂O₃ NCs revealed a high degradation efficiency of Rh B (87.5%) and MB dyes (90.4%) under UV irradiation. These results confirm that supporting MgO and Fe₂O₃ to

γ

-Al₂O₃ as NCs enhanced the photocatalysis of the polluting dye.

2.6.1. Stability and Recyclability of NPs and NCs

Several cycles of Rh B and MB dye degradation were measured to investigate the stability and recyclability of the synthesized samples. In these experiments, the protocols used to evaluate dye degradation efficiency (D) under UV irradiation for 140 min were applied in each repeat experiment using prepared MgO-Fe₂O₃/

γ

-Al₂O₃ NCs. For each cycle, the degradation efficiencies (D) of the Rh B and MB dyes for the six runs are shown in Figure 10. After six runs (Figure 10), the degradation efficiencies (D) of the Rh B and MB dyes for the MgO-Fe₂O₃/

γ

-Al₂O₃ NCs were 87.5%, 87.3%, 87.0%, 86.9%, 86.8%, 86.6%, and 90.4%; 90.0%, 89.8%, 89.5%, 89.4%, and 89.4%, respectively. The recyclability results showed that the MgO-Fe₂O₃/

γ

-Al₂O₃ NCs have excellent considerable stability and recyclability.

2.6.2. Photoreaction Mechanism

Many previous studies have shown that the photocatalytic degradation of organics using catalysts occurs through several mechanisms [81,82,83,84]. Figure 11 describes one of these mechanisms for degrading organic dyes (Rh B and MB) using the obtained MgO-Fe₂O₃/

γ

-Al₂O₃ NCs. Primarily, when synthesized, MgO-Fe₂O₃/

γ

-Al₂O₃ NCs were exposed to UV light. Rapidly, the produced holes (h⁺) in the valence band (VB) and electrons (e⁻) in the conductor band (CB) pairs were further created in the prepared MgO, Fe₂O₃, and

γ

-Al₂O₃ NPs as shown in Equation (1). At that time, some of the electrons (e⁻) in the CB of the MgO NPs were moved to the CB of the Fe₂O₃ NPs, as revealed in Equation (2). Regarding the dyes, the LUMO levels of Rh B and MB are approximately −1.3 V and −0.6 V versus NHE, respectively, which are more negative than the CB of γ-Al₂O₃. As displayed in Equation (3), the electrons in the CB of Fe₂O₃ NPs transferred to

γ

-Al₂O₃ NPs. Furthermore, the electrons react with molecular oxygen (O₂) to generate superoxide radical (

O_{2}^{*}

), as shown in Equation (4). Similarly, the holes (h⁺) in the valence band (VB) of the Fe₂O₃ NPs were transferred to the valence band (VB) of the

γ

-Al₂O₃ NPs. On the other hand, hydroxyl radicals (OH^*) were produced due to the presence of reactive holes (h⁺) in the valence band (VB) of

γ

-Al₂O₃ NPs or Fe₂O₃ NPs with water or hydroxyl ions (HO⁻) as presented in Equation (5). To end, both produced free radicals (

O_{2}^{*}

and OH^*) directly react with dye molecules to yield products (CO₂ + H₂O), as shown in Equation (7). The above reactions are presented in the following equations:

MgO-Fe₂O₃/γ-Al₂O₃ NCs + hv → MgO-Fe₂O₃/γ-Al₂O₃ NCs (h⁺ + e⁻)

(1)

MgO(e⁻) → Fe₂O₃(e⁻)

(2)

Fe₂O₃(e⁻) → γ-Al₂O₃(e⁻defect site)

(3)

γ - A l_{2} O_{3} (e^{-}) + O_{2} \to O_{2}^{*}

(4)

MgO (h⁺) or γ-Al₂O₃(h⁺) + HO⁻ → OH^*

(5)

{(O}_{2}^{*} a n d O H^{*}) + P o l l u t a n t s d y e \to C O_{2} + H_{2} O (P r o d u c e s)

(6)

2.7. Anticancer and Biocompatibility Evaluations

The anticancer and antibacterial activity of NPs and NCs have attracted increased interest in the biomedical field, as shown in several studies [33,85,86,87]. In the present work, the MTT assay was applied to investigate the anticancer efficacy and biocompatibility of synthesized NPs and NCs toward A549 cancer cells and IMR90 normal cells. Figure 12a,b show the percentages of cancer and normal cells after treatment with the prepared NPs and NCs for 24 h at different concentrations (0, 0.5, 1, 2.5, 5, 10, and 25 μg/mL). As shown in Figure 12a, the MgO-Fe₂O₃/

γ

-Al₂O₃ NCs had greater anticancer efficacy at high concentrations (25 μg/mL) than the pure

γ

-Al₂O₃ NPs and Fe₂O₃/

γ

-Al₂O₃ NPs. This result indicates that the addition of Fe₂O₃ and MgO to pure

γ

-Al₂O₃ NPs as NCs killed A549 cancer cells. As illustrated in Table 3, the inhibitory concentration (IC₅₀ (µg/mL ± SD)) values for

γ

-Al₂O₃ NPs, Fe₂O₃/

γ

-Al₂O₃ NPs, and MgO-Fe₂O₃/

γ

-Al₂O₃ NCs were 16.54 ± 0.8, 14.75 ± 0.4, and 11.40 ± 0.6, respectively. On the other hand, assessing the biocompatibility of these samples is important. Figure 12b shows that the prepared NPs and NCs have lower toxicity toward normal cells (at an IMR90) after 24 h of exposure. The MTT results suggest that the prepared samples have high cytotoxicity against cancer cells, while the biocompatibility of the prepared samples was excellent toward normal cells.

The selective anticancer performance of the synthesized NPs and NCs was evaluated using the MTT assay. A possible mechanism for their anticancer impact can include the production of reactive oxygen species (ROS). These reactive oxygen species (ROS) are oxygen radicals capable of inducing oxidative damage to crucial cellular macromolecules such as DNA, ultimately leading to the destruction of cancer cells. Previous studies have shown that the metal oxide NPs and NCs have induced oxidative stress, resulting in the disturbance of mitochondrial membrane potential in cancer cells and cell death [41,83,88,89].

3. Methods and Chemicals

3.1. Chemicals and Cells

All chemical materials in these experiments were applied without further purification. Gamma-alumina (γ-Al₂O₃), iron (III) nitrate nonahydrate (Fe (NO₃)·9H₂O), magnesium nitrate hexahydrate (Mg(NO₃)₂·6H₂O), and ammonium carbonate ((NH4)₂CO₃) were obtained from Sigma, Aldrich, India. Rhodamine B (Rh B) and methyl blue (MB) dyes were further supplied from Sigma-Aldrich. Human lung cancer cells (A549) and normal lung fibroblasts (IMR90) were obtained from the American Type Culture Collection (ATTC, Manassas, WV, USA). Double distilled water (DW) and ethanol were used throughout these experiments.

3.2. Preparation of MgO-Fe₂O₃/Al₂O₃ NCs

The present work applied the deposition–coprecipitation process to synthesize MgO-Fe₂O₃/

γ

-Al₂O₃ NCs with 70%

γ

-Al₂O₃, 15% Fe₂O₃, and 15% MgO. Initially, 5.1 g of

γ

-Al₂O₃ (0.05 mol), 8.5 g of Fe(NO₃)·9H₂O (0.021 mol), and 2.7 g of Mg(NO₃)₂·6H₂O (0.0105 mol) were mixed in 50 mL of DW, and sonicated for 1 h. Then, this solution was further placed in a closed round flask under stirring at 75 °C for 5 h as the first solution. After that, 5 g of (NH₄)₂CO₃ was dissolved in 50 mL of DW as the second solution. Subsequently, the second solution was slowly added to the first solution as the temperature increased to 75 °C and stirred in a closed flask for 5 h. Next, the obtained precipitate was filtered, washed many times with water/ethanol (3:1), and dried in an oven at 80 °C for 24 h. This precipitate was further annealed at 500 °C for 5 h. Under the same conditions, Fe₂O₃-supported Al₂O₃ NPs were produced without Mg(NO₃)₂·6H₂O.

3.3. Characterization of NPs and NCs

X-ray diffraction (XRD) (PanAnalytic X’Pert Pro, Malvern Instruments, UK) was applied to study the crystal structure of the synthesized NPs and NCs. Morphological examination was performed via transmission electron microscopy (TEM) (200 kV, 2100F, JEOL, Inc., Tokyo, Japan). and scanning electron microscopy (SEM) (JSM-7600F, JEOL, Inc., Tokyo, Japan). The chemical states and compositions of these samples were examined via X-ray photoelectron spectroscopy (XPS) (PHI-5300 ESCA PerkinElmer equipment from Boston, MA, USA). The molecular structure and group function were confirmed using an FTIR spectrometer (PerkinElmer Paragon 500, USA). PL spectra were recorded using fluorescence (DW-F97) spectroscopy. The phase composition of samples was determined using OriginPro 2018 (OriginLab Corporation, Northampton, MA, USA).

3.4. Photocatalytic Test of NPs and NCs

Rhodamine B (Rh B) and methyl blue (MB) dyes were employed to test the photocatalytic performance of the prepared

γ

-Al₂O₃ NPs, Fe₂O₃/

γ

-Al₂O₃ NPs, and MgO-Fe₂O₃/

γ

-Al₂O₃ NCs. An amount of 50 mg of each sample was added to 50 mL of the Rh B solution (10 ppm) at the specified concentration. In the dark, the resulting solution was stirred with a magnetic stirrer for 30 min to reach adsorption–desorption equilibrium for the toxic dye on the surface of the sample system. After adsorption equilibrium was reached, the mixture was exposed to a UV source for 140 min. During this period, the photocatalysis efficiency was measured periodically. After 20 min of exposure, 3.0 mL of the colloidal suspension sample was collected using a micropipette and then centrifuged at 4000 rpm for 10 min to separate the sample from the dye solution. Hence, the degradation efficiency of the dyes was estimated using Equation (7) as follows:

D e g r a d a t i o n e f f i c i e n c y (%) = [\frac{C_{0} - C_{t}}{C_{0}}] \times 100

(7)

where C₀ is the initial absorbance, and C_t is the absorbance after the time (t). Additionally, the kinetic constant rate (K) of the polluting dye was estimated using Equation (8) as given:

K t = \ln [\frac{C_{0}}{C_{t}}]

(8)

Additionally, K is the kinetic constant rate of degradation C₀ in the initial absorbance, C_t is the absorbance after exposure time (t), and t is the exposure time (t). In the present work at the same experimental conditions, the stability and recyclability were evaluated using MgO-Fe₂O₃/

γ

-Al₂O₃ NCs for six cycles.

3.5. Cell Growth and Preparation of Samples for Cell Treatment

A549 and IMR90 cells were cultured in improved Eagle’s medium (DMEM) (Invitrogen, Carlsbad, CA, USA) at 37 °C under 5% CO₂ in an incubation chamber. After reaching 75% confluence, the cells were sub-cultured for subsequent experiments.

γ

-Al₂O₃ NPs, Fe₂O₃/

γ

-Al₂O₃ NPs, and MgO-Fe₂O₃/

γ

-Al₂O₃ NCs were dispersed in culture media to create a stock solution (1 mg/mL) and sonicated at 80 kHz for 30 min to prevent aggregation. The NP and NC suspensions were further diluted to various concentrations (0, 0.5, 1, 2.5, 5, 10, and 25 μg/mL) for each sample.

3.6. Cell Viability Assessment

In the present study, the MTT assay was performed as previously described in the literature with some adjustments [90,91,92] to assess the anticancer and biocompatibility activity of these samples. After the cells were sub-cultured, approximately 10,000 cells per well were seeded into a 96-well plate and incubated for 24 h at 37 °C with 5% CO₂. Subsequently, different concentrations (0, 0.5, 1, 2.5, 5, 10, and 25 μg/mL) of each sample were added to a 96-well plate and incubated for 24 h at 37 °C with 5% CO₂. The next day, the medium in each well (DMEM) was removed. After that, 100 µL of MTT solution was added to each well and incubated for 3 h to allow the formation of blue formazan crystals. Then, 10 µL of dimethyl sulfoxide (DMSO) was added to each well to dissolve these crystals. A microplate reader (Synergy-HT, Winooski, Vermont, USA) was used to measure the absorbance of the dissolved crystals at 570 nm to assess cell viability.

3.7. Statistical Analysis

The SPSS program was used to determine the mean ± standard deviation (SD) and the statistical data for the biological experiments. Significant differences were determined between groups using one-way analysis of variance (ANOVA). In the present work, the p value (p

<

0.05) was used to indicate significant differences.

4. Conclusions

MgO-Fe₂O₃/γ-Al₂O₃ NCs were successfully synthesized using the coprecipitation method and characterized for their physicochemical properties by different analytical techniques such as XRD, TEM, SEM, EDX, XPS, FTIR, and PL spectroscopy. As shown in the characterization results, XRD analysis confirmed the presence of γ-Al₂O₃, MgO, and Fe₂O₃ phases, while TEM and SEM images showed spherical particles with a tendency for agglomeration. EDX and XPS analysis verified that the elements (Al, Fe, Mg, O, and C) existed in the MgO-Fe₂O₃/γ-Al₂O₃ NCs. The enhanced photocatalytic and selective anticancer activities observed in these NCs to the combined effects of MgO and Fe₂O₃ on γ-Al₂O₃led to a reduced electron–hole recombination rate, as evidenced by the PL spectra. The MgO-Fe₂O₃/γ-Al₂O₃ NCs demonstrated high photocatalysis efficiencies for Rhodamine-B (87.5%) and methylene blue (90.4%) under UV irradiation. Furthermore, the MgO-Fe₂O₃/γ-Al₂O₃ NCs exhibited superior anticancer activity (IC₅₀ = 11.40 ± 0.6 µg/mL) against A549 cells, with excellent biocompatibility toward normal IMR90 cells. This study addresses global challenges of environmental pollution through the degradation of toxic organic dyes in wastewater and the development of more effective and safer cancer treatments. These findings highlight the potential of these samples for applications in environmental remediation and cancer therapy. Future research should focus on evaluating their performance in vivo models.

Author Contributions

Z.M.A. conceptualized the study, and the investigations and methods were carried out by Z.M.A., H.A.A., M.A. and S.A. The original draft was prepared by Z.M.A. Review and editing were conducted by Z.M.A., H.A.A., M.A. and S.A. All authors have read and agreed to the published version of the manuscript.

Funding

The authors extend their sincere appreciation to researchers supporting project number (RSPD2024R813), King Saud University, Riyadh, Saudi Arabia, for funding this research.

Data Availability Statement

The data in this work can be obtained by contacting the corresponding author.

Conflicts of Interest

The authors declare no conflicts of interest.

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Figure 1. XRD pattern: (a)

γ

-Al₂O₃ NPs, (b) Fe₂O₃/

γ

-Al₂O₃ NPs, and (c) MgO-Fe₂O₃/

γ

-Al₂O₃ NCs.

Figure 1. XRD pattern: (a)

γ

-Al₂O₃ NPs, (b) Fe₂O₃/

γ

-Al₂O₃ NPs, and (c) MgO-Fe₂O₃/

γ

-Al₂O₃ NCs.

Figure 2. TEM images, HRTEM images, and SAED analysis: (a–c)

γ

-Al₂O₃ NPs, (d–f) Fe₂O₃/

γ

-Al₂O₃ NPs, and (g–i) MgO-Fe₂O₃/

γ

-Al₂O₃ NCs.

Figure 2. TEM images, HRTEM images, and SAED analysis: (a–c)

γ

-Al₂O₃ NPs, (d–f) Fe₂O₃/

γ

-Al₂O₃ NPs, and (g–i) MgO-Fe₂O₃/

γ

-Al₂O₃ NCs.

Figure 3. SEM images: (a)

γ

-Al₂O₃ NPs, (b) Fe₂O₃/

γ

-Al₂O₃ NPs, (c) MgO-Fe₂O₃/

γ

-Al₂O₃ NCs, and (d) EDX analysis of MgO-Fe₂O₃/

γ

-Al₂O₃ NCs.

Figure 3. SEM images: (a)

γ

-Al₂O₃ NPs, (b) Fe₂O₃/

γ

-Al₂O₃ NPs, (c) MgO-Fe₂O₃/

γ

-Al₂O₃ NCs, and (d) EDX analysis of MgO-Fe₂O₃/

γ

-Al₂O₃ NCs.

Figure 4. Elemental mapping of the distribution of MgO-Fe₂O₃/

γ

-Al₂O₃ NCs: (a) electron, (b) aluminum (Al), (c) iron (Fe), (d) magnesium (Mg), and (e) oxygen (O).

Figure 4. Elemental mapping of the distribution of MgO-Fe₂O₃/

γ

-Al₂O₃ NCs: (a) electron, (b) aluminum (Al), (c) iron (Fe), (d) magnesium (Mg), and (e) oxygen (O).

Figure 5. XPS spectra: (a) XPS survey spectra and high-resolution XPS spectra of (b) Al 1p, (c) Fe 2p, (d) O 1 s, and (e) Mg 2p for

γ

-Al₂O₃ NPs, Fe₂O₃/

γ

-Al₂O₃ NPs, and MgO-Fe₂O₃/

γ

-Al₂O₃ NCs.

Figure 5. XPS spectra: (a) XPS survey spectra and high-resolution XPS spectra of (b) Al 1p, (c) Fe 2p, (d) O 1 s, and (e) Mg 2p for

γ

-Al₂O₃ NPs, Fe₂O₃/

γ

-Al₂O₃ NPs, and MgO-Fe₂O₃/

γ

-Al₂O₃ NCs.

Figure 6. FTIR spectra of the synthesized samples: (a)

γ

-Al₂O₃ NPs, (b) Fe₂O₃/

γ

-Al₂O₃ NPs, and (c) MgO-Fe₂O₃/

γ

-Al₂O₃ NCs.

Figure 6. FTIR spectra of the synthesized samples: (a)

γ

-Al₂O₃ NPs, (b) Fe₂O₃/

γ

-Al₂O₃ NPs, and (c) MgO-Fe₂O₃/

γ

-Al₂O₃ NCs.

Figure 7. Photoluminescence spectra of

γ

-Al₂O₃ NPs, Fe₂O₃/

γ

-Al₂O₃ NPs, and MgO-Fe₂O₃/

γ

-Al₂O₃ NCs.

Figure 7. Photoluminescence spectra of

γ

-Al₂O₃ NPs, Fe₂O₃/

γ

-Al₂O₃ NPs, and MgO-Fe₂O₃/

γ

-Al₂O₃ NCs.

Figure 8. (a) UV-Vis absorption of the Rh dye solution, (b) plot (C_t/C₀) vs. irradiation time (min), (c) kinetics of the photocatalysis of Rh B solutions for the prepared samples, and (d) photocatalysis efficiency (D%) of the Rh B solution using the synthesized catalyst.

Figure 9. (a) UV-Vis absorption of MB dye solution, (b) plot (C_t/C₀) vs. irradiation time (min), (c) kinetics of the photocatalysis of MB solutions for prepared samples, and (d) photocatalysis efficiency (D%) of MB solution using synthesized catalyst.

Figure 10. The number of recycled Rh B and MB dye photocatalysis agents using the prepared MgO-Fe₂O₃/

γ

-Al₂O₃ NCs under UV irradiation for 140 min.

Figure 10. The number of recycled Rh B and MB dye photocatalysis agents using the prepared MgO-Fe₂O₃/

γ

-Al₂O₃ NCs under UV irradiation for 140 min.

Figure 11. Schematic diagram of the photoreaction mechanism of organic dyes using MgO-Fe₂O₃/

γ

-Al₂O₃ NCs.

Figure 11. Schematic diagram of the photoreaction mechanism of organic dyes using MgO-Fe₂O₃/

γ

-Al₂O₃ NCs.

Figure 12. The percentage of viable cells after exposure to the

γ

-Al₂O₃ NPs, Fe₂O₃/

γ

-Al₂O₃ NPs, or MgO-Fe₂O₃/

γ

-Al₂O₃ NCs after 24 h: (a) A549 cells and (b) normal IMR90 cells. The symbol (*) indicates a significant difference (p < 0.05) between the treated sample and the control.

Figure 12. The percentage of viable cells after exposure to the

γ

-Al₂O₃ NPs, Fe₂O₃/

γ

-Al₂O₃ NPs, or MgO-Fe₂O₃/

γ

-Al₂O₃ NCs after 24 h: (a) A549 cells and (b) normal IMR90 cells. The symbol (*) indicates a significant difference (p < 0.05) between the treated sample and the control.

Table 1. The values of the first-order kinetic rate constant (k) and degradation efficiency (D) of the prepared NPs and NCs for Rh B and MB under UV irradiation.

Catalyst Used	Rh B Dye			MB Dye
Catalyst Used	K (min⁻¹)	R²	D (%)	k (min⁻¹)	R²	D (%)
$γ$ -Al₂O₃ NPs	0.0618	0.9883	56.3	0.00598	0.9891	57.2
Fe₂O₃/ $γ$ -Al₂O₃ NPs	0.00798	0.9957	69.2	0.00876	0.9906	71.7
MgO-Fe₂O₃/ $γ$ -Al₂O₃ NCs	0.01193	0.9894	87.5	0.01574	0.9891	90.4

Table 2. Comparison of degradation efficiency of various reported catalysts for different dyes.

Catalyst Used	D (%)	Time (min)	Dyes	Ref.
MgO-Fe₂O₃/ $γ$ -Al₂O₃ NCs	88.5	140	Rh B	This study
MgO-Fe₂O₃/ $γ$ -Al₂O₃ NCs	90.4	140	MB	This study
CdO/ZnO/MgO NCs	87.5	120	MB	[75]
ZnO/CeO₂/Yb₂O NCs	78.0	40	CR	[76]
CuO/MgO/ZnO NCs	88.5	100	MB	[77]
CuO/MgO/ZnO NCs	75.9	100	Rh B	[77]
NiO/Fe₂O₃/ZnO	81.4	250	MO	[78]
ZnO/Er₂O₃/Nd₂O₃/RGO NCs	99.2	60	MB	[79]
CuO/α-Fe₂O₃/γ-Al₂O₃ NCs	98.0	240	MO	[80]

Table 3. IC₅₀ values of the prepared samples for A549 cells after 24 h.

Prepared Samples	IC₅₀ (µg/mL ±SD)
$γ$ -Al₂O₃ NPs	16.54 ± 0.8
Fe₂O₃/ $γ$ -Al₂O₃ NPs	14.75 ± 0.4
MgO-Fe₂O₃/ $γ$ -Al₂O₃ NCs	11.40 ± 0.6

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Alaizeri, Z.M.; Alhadlaq, H.A.; Aldawood, S.; Ahamed, M. Synthesis and Characterization of MgO-Fe₂O₃/γ-Al₂O₃ Nanocomposites: Enhanced Photocatalytic Efficiency and Selective Anticancer Properties. Catalysts 2024, 14, 923. https://doi.org/10.3390/catal14120923

AMA Style

Alaizeri ZM, Alhadlaq HA, Aldawood S, Ahamed M. Synthesis and Characterization of MgO-Fe₂O₃/γ-Al₂O₃ Nanocomposites: Enhanced Photocatalytic Efficiency and Selective Anticancer Properties. Catalysts. 2024; 14(12):923. https://doi.org/10.3390/catal14120923

Chicago/Turabian Style

Alaizeri, ZabnAllah M., Hisham A. Alhadlaq, Saad Aldawood, and Maqusood Ahamed. 2024. "Synthesis and Characterization of MgO-Fe₂O₃/γ-Al₂O₃ Nanocomposites: Enhanced Photocatalytic Efficiency and Selective Anticancer Properties" Catalysts 14, no. 12: 923. https://doi.org/10.3390/catal14120923

APA Style

Alaizeri, Z. M., Alhadlaq, H. A., Aldawood, S., & Ahamed, M. (2024). Synthesis and Characterization of MgO-Fe₂O₃/γ-Al₂O₃ Nanocomposites: Enhanced Photocatalytic Efficiency and Selective Anticancer Properties. Catalysts, 14(12), 923. https://doi.org/10.3390/catal14120923

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Synthesis and Characterization of MgO-Fe₂O₃/γ-Al₂O₃ Nanocomposites: Enhanced Photocatalytic Efficiency and Selective Anticancer Properties

Abstract

1. Introduction

2. Results and Discussion

2.1. Structural Studies

2.2. Morphological Characterization

2.2.1. TEM Analysis

2.2.2. SEM and EDX with Elemental Mapping Analysis

2.3. XPS Analysis

2.4. FTIR Study

2.5. Photoluminescence Analysis

2.6. Photocatalytic Study of NPs and NCs

2.6.1. Stability and Recyclability of NPs and NCs

2.6.2. Photoreaction Mechanism

2.7. Anticancer and Biocompatibility Evaluations

3. Methods and Chemicals

3.1. Chemicals and Cells

3.2. Preparation of MgO-Fe₂O₃/Al₂O₃ NCs

3.3. Characterization of NPs and NCs

3.4. Photocatalytic Test of NPs and NCs

3.5. Cell Growth and Preparation of Samples for Cell Treatment

3.6. Cell Viability Assessment

3.7. Statistical Analysis

4. Conclusions

Author Contributions

Funding

Data Availability Statement

Conflicts of Interest

References

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Synthesis and Characterization of MgO-Fe₂O₃/γ-Al₂O₃ Nanocomposites: Enhanced Photocatalytic Efficiency and Selective Anticancer Properties

Abstract

1. Introduction

2. Results and Discussion

2.1. Structural Studies

2.2. Morphological Characterization

2.2.1. TEM Analysis

2.2.2. SEM and EDX with Elemental Mapping Analysis

2.3. XPS Analysis

2.4. FTIR Study

2.5. Photoluminescence Analysis

2.6. Photocatalytic Study of NPs and NCs

2.6.1. Stability and Recyclability of NPs and NCs

2.6.2. Photoreaction Mechanism

2.7. Anticancer and Biocompatibility Evaluations

3. Methods and Chemicals

3.1. Chemicals and Cells

3.2. Preparation of MgO-Fe2O3/Al2O3 NCs

3.3. Characterization of NPs and NCs

3.4. Photocatalytic Test of NPs and NCs

3.5. Cell Growth and Preparation of Samples for Cell Treatment

3.6. Cell Viability Assessment

3.7. Statistical Analysis

4. Conclusions

Author Contributions

Funding

Data Availability Statement

Conflicts of Interest

References

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3.2. Preparation of MgO-Fe₂O₃/Al₂O₃ NCs