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Photocatalytic properties of ZnFe-mixed oxides synthesized via a simple route for water remediation

  • Milica Hadnadjev-Kostic EMAIL logo , Djurdjica Karanovic , Tatjana Vulic , Jasmina Dostanić and Davor Lončarević
Published/Copyright: April 26, 2023
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Green Processing and Synthesis
From the journal Green Processing and Synthesis Volume 12 Issue 1

Abstract

ZnFe photocatalysts have been increasingly investigated for water remediation due to the high demands in this field, such as activity, toxicity, cost, and stability. The presented study was focused on the simple, safe, non-toxic, and eco-friendly synthesis and characterization of ZnFe-mixed metal oxides in correlation with their functional properties. Photocatalytic performance of these materials was evaluated by rhodamine B photodegradation under simulated solar light irradiation. The synthesized mixed oxides contained hexagonal wurtzite ZnO as the predominant phase, whereas, after thermal treatment, the formation of the spinel-structured ZnFe2O4 phase was observed. The photocatalysts with the additional spinel phase and thermally treated at 300°C and 500°C exhibited superior photocatalytic activity probably due to the highest amount of the ZnFe2O4 spinel phase, favourable mesoporous structure, and an optimal energy band gap of ∼2.30 eV that initiated higher light-harvesting efficiency. The rhodamine B photodegradation followed zero-order kinetics, indicating complete coverage of active sites by the pollutant substrate. Additionally, photocatalysts showed the highest efficiency at the natural pH (6.8), being in accordance with green synthesis principles. Simple, green route assembling synthesis method, high photodegradation efficiency, and good reusability make these ZnFe-mixed oxides great candidates for potential application in practical wastewater treatments.

Keywords: mixed metal oxides; organic dye pollutant; rhodamine B; photodegradation efficiency

1 Introduction

The exponential increase of environmental pollution with no systematic solution has become an overwhelming concern in the scientific community [1]. As a consequence of the rapid growth of industrial regions, enormous amounts of wastewater are daily generated that represent a serious risk to the environment and human health [2,3]. Major organic pollutants are residual dyes from different industries, and considering their toxicity, unpleasant colouring, and non-biodegradation properties, these pollutants are sought to be extremely hazardous to the environment and capable of destroying aquatic organisms if present in water and/or wastewater [4,5,6]. In printing, textile, and photographic industries, organic dyes are frequently used and when released into the effluent water streams cannot usually be degraded without a catalytic assistance [7,8]. Rhodamine B (RhB), as a water-soluble, persistent synthetic cationic dye, is frequently employed in the industry and when released in wastewater, it is extremely difficult to be removed by physical methods considering its conjugations of aromatic rings (benzene, naphthalene) [9]. Therefore, effective removal methods present a challenging as well as motivating task that needs to be addressed with great precision in order to decrease or completely eliminate environmental problems regarding dye pollutants in wastewater [10]. Even though many processes have been developed, there is still an urgent need for further progress of removal processes that would fulfil all the requirements and would be simultaneously efficient and economically viable [1]. Numerous physical and chemical methods (adsorption, membrane filtration, electrolysis, sedimentation, coagulation, flocculation, chemical treatments, oxidation, biological treatments) have been reported for the removal of toxic molecules and bacteria from contaminated water [11]. Most of the mentioned methods have proven to have disadvantages in various aspects of applications and have the capability of only transferring harmful contaminants from one phase to another without decomposing toxic pollutants to nontoxic substances [11]. Various advanced oxidation processes have received much interest due to their high efficiency in degradation of chemical contaminations from wastewater, the most promising being photocatalysis, well known as a cost-effective and environmentally friendly method [12,13]. Considering that photocatalytic oxidation reactions are based on the free-radical reaction initiated by light irradiation of a photocatalyst (semiconductor) surface, the efficiency is influenced by various factors and depends on the mobility of electron–hole pairs as well as the accessibility of active sites on the surface of photocatalysts [1]. Moreover, due to the environmentally friendly process and consequent energy conservation with the use of solar light, semiconductor-based photocatalysis has recently become one of the most promising technologies in wastewater purification [4,6]. Taking into consideration that photocatalysis is a surface phenomenon, structural, textural, and optical properties of semiconductors mostly influence and determine their photocatalytic activity [1]. For efficient elimination of various pollutants, metal oxides, such as TiO2, WO3, CeO2, and MnO2, are frequently used as heterogeneous photocatalysts [14,15]. One of the most resourceful candidates in green environmental management has been zinc oxide (ZnO) because of its strong oxidation ability, good photocatalytic properties, and low cost [4,16,17]. Additional coupling of ZnO and a semiconductor with a narrow energy band gap would result in a more enhanced photocatalytic activity that could be a route to the efficient exploitation of the solar light source [12]. Mutual transfer of charge carriers, i.e. transfer of excited electrons from the conduction band of the narrow band gap semiconductor to the wide band gap semiconductor increases the photocatalytic performance [15]. Considering these advantages, mixed oxides are already widely used in heterogeneous catalysis because of their possibility to combine the properties of different metal oxides having different oxidation states, triggering the synergetic effect, increasing the number of lattice defects, and the number of active sites [5,18].

Inspired by the current research trend, in this study, ZnFe-mixed oxides were synthesized with the aim to induce solar-efficient photocatalytic properties. The chosen co-precipitation method has been emphasized as a robust, dependable, and time-saving process, without hazardous organic solvents, high-pressure or -temperature treatment and can be easily scaled-up for industrial applications [19,20]. In order to encourage sustainable processes and eliminate the use of toxic chemicals that are harmful to the environment, the motivation for this study was to apply the co-precipitation method in the synthesis path for ZnFe-mixed metal oxides that follows a simple, safe, nontoxic, eco-friendly, and cost-effective green route. Different thermal treatment/activation temperatures of synthesized materials were used to induce a variation in the crystallite size, energy band gap, and textural properties that influence photocatalytic activity in order to enhance photocatalytic performance in the rhodamine B photodegradation. Furthermore, in order to establish optimal reaction conditions and possible mechanism, stability, and pH influence of the most effective photocatalysts were also studied.

2 Materials and methods

2.1 Sample preparation

Mixed oxides (ZnFe-MO) were synthesized by a high supersaturation coprecipitation method with the use of 0.7 M Zn(NO3)2·6H2O and 0.3 M Fe(NO3)3·9H2O solution precursors that were added to the base solution (0.67 M Na2CO3 and 2.25 M NaOH) and vigorously stirred at a constant temperature (40°C). The precipitates were aged for 15 h and then washed with deionized water until pH 7 was reached. The schematic view of the synthesis path is presented in Figure 1. The products were dried for 24 h at 100°C (sample denoted as ZnFe100) and thermally treated for 5 h at different temperatures in the air: 300°C, 500°C, 700°C, and 900°C (samples denoted as ZnFe300, ZnFe500, ZnFe700, and ZnFe900, respectively).

Figure 1 Schematic representation of the co-precipitation synthesis path followed by the thermal treatment.
Figure 1

Schematic representation of the co-precipitation synthesis path followed by the thermal treatment.

2.2 Characterization

X-ray powder diffraction (XRD) was used for the interpretation of the phase composition. The analysis was conducted using a Rigaku MiniFlex 600 with Cu-Kα radiation, wavelength of λ = 0.15406 nm, at 40 kV and 40 mA in the 2θ range from 10° to 80° and angular steps of 0.02° with a step time of 3 s. The crystallite sizes were calculated using the Scherrer formula and the full-width at half-maximum (FWHM) of the most intense diffraction peak (Eq. 1):

(1) D = k λ β cos θ

where D is the crystallite size (nm), k is the shape function (0.9), λ is the X-ray wavelength, θ  is the angle of diffraction, and β  is the FWHM of the considered peak.

The Fourier transform infrared spectroscopy (FTIR) spectra of the powdered samples were recorded using an Alpha FTIR spectrometer (BRUKER Optics, Germany). The FTIR spectra were recorded with a spectral resolution of 4 cm−1 in the range of 4,000–400 cm−1 with 24 averaged scans per measurement.

The morphology of samples was investigated with a scanning electron microscope (SEM, Hitachi, TM3030).

The texture of samples was analysed by low-temperature nitrogen adsorption at −196°C (Micromeritics ASAP 2000). The surface area of the samples was calculated by the Brunauer–Emmett–Teller (BET) method. The pore size distribution and the cumulative pore volume were determined by the Brunauer–Joyner–Halenda (BJH) method applied to the desorption branch of the isotherm.

The energy band gap, E g, of samples was calculated by applying the Tauc plot as a direct allowed transition function to diffuse reflectance spectra (DRS). DR UV-Vis spectra were recorded on a Nicolet Evolution 500 spectrometer, with a diffuse reflectance accessory (Thermo Electron Corporation).

2.3 Photocatalytic degradation of rhodamine B

Photocatalytic tests were performed in an open cylindrical thermostatic Pyrex reaction vessel using an Osram Ultra Vitalux 300 W lamp with the emission spectrum that simulates solar light, housed 45 cm above the top surface of the dye solution. The suspensions were exposed to air without additional aeration throughout the duration of each experiment. The photocatalytic efficiency of all the prepared samples was estimated by RhB photodegradation, monitoring the decrease of RhB concentration with time. In order to ensure the required adsorption/desorption equilibrium between the RhB dye and the catalyst surface, the reaction mixtures (50 mg of catalysts and 100 mL of 4.8 mg·L−1 RhB solution) were stirred in the dark for 30 min, before exposure to light. When the equilibrium was established, reaction mixtures were irradiated with light and aliquots were analysed at defined time intervals using an UV-Vis spectrophotometer. Prior to the reaction on active sites, the first step of every heterogeneous catalytic reaction is the adsorption of reactive species on the catalysts’ surface. In order to evaluate only the photocatalytic efficiency and eliminate any possible adsorption that is not related to the photocatalytic reaction, blank samples (reaction solution with the catalyst) were retained in the dark, and the RhB concentration was measured at the defined time intervals. The photodegradation efficiency was estimated by the RhB photodegradation and calculated based on the total conversion using the following equation:

(2) Photodegradation efficiency ( % ) = C 0 − C t C 0 × 100

where C 0 is the RhB concentration of the blank sample and C t is the RhB concentration of irradiated samples, both measured at defined time intervals. The RhB concentration was measured by UV-Vis spectrophotometry (EVOLUTION 600 spectrophotometer) at λ = 554 nm.

An inductively coupled plasma optical emission spectrometer (ICP–OES), iCAP 6500 Duo ICP (Thermo Fisher Scientific) was used to quantify the potential leaching of Zn2+ ions from the catalyst after the photocatalytic test.

2.4 Kinetics of the RhB photocatalytic reaction

In order to investigate the data obtained during the photodegradation process, the zero-order kinetic model was used to describe the photocatalytic kinetic process (Eq. 3):

(3) C t = C 0 − k · t

where C 0 and C t are initial and reaction time (t) concentrations and k is the zero-order rate constant [21,22].

3 Results and discussion

3.1 Structural properties

XRD diffraction peaks of all synthesized and thermally treated photocatalysts are presented in Figure 2 and can be correlated with the series of Bragg reflections corresponding to the standard JCPDS. In the sample ZnFe100, sharp intense diffraction peaks were observed at 31.8°, 34.4°, 36.2°, 47.5°, 56.6°, 62.8°, and 68.0° that correspond to (100), (002), (101), (102), (110), (103), and (112) crystalline lattice, respectively, for the ZnO phase (JCPDS File no. 79-2205) [23,24]. These results imply that the phase composition of as-synthesized materials was ZnFe-mixed oxide phase with predominant properties of the wurzite ZnO phase.

Figure 2 XRD diffraction peaks of thermally treated samples ZnFe100, ZnFe300, ZnFe500, ZnFe700, and ZnFe900 at different temperatures.
Figure 2

XRD diffraction peaks of thermally treated samples ZnFe100, ZnFe300, ZnFe500, ZnFe700, and ZnFe900 at different temperatures.

It was observed that the crystallinity increased upon increase of the thermal treatment temperature. Additional diffraction patterns were detected for thermally treated samples with sharp intense peaks at 0.05°, 35.4°, 42.8°, 53°, 56.8°, and 62.2° that correspond to the spinel phase ZnFe2O4 with (220), (311), (400), (422), (511), and (440) crystalline lattice, respectively (JCPDS File no. 89-1012) [25]. Previous reports suggested that for ZnFe samples at low temperatures (<400°C), only the ZnFe-mixed oxide phase with predominant properties of the wurzite ZnO phase can be distinguished, whereas higher thermal activation temperatures trigger the formation of an additional ZnFe2O4 spinel phase [26]. The presented XRD results are in accordance with these findings where, at temperatures higher than 300°C, the formation of the ZnFe2O4 spinel was pronounced, whereas XRD patterns at 300°C showed a slight, but not evident, beginning of this phase formation. Additionally, with the increase in the thermal treatment temperature, the amount of the ZnFe2O4 phase with the cubic structure also increased. Furthermore, in samples thermally treated at 700°C and 900°C, a low-intense peak (at 2θ = 37°) was noticed that could be assigned to the presence of either the Fe2O3 or Fe3O4 phase in accordance with JCPDS (File no. 87-2334) [27]. The calculated crystallite sizes of all samples, presented in Table 1, showed that the crystallite size increased with an increase in the temperature of thermal treatment, since the temperature increase results in the grain growth triggering a greater crystallite size [26,28].

Table 1

Crystallite size, textural properties, energy band, and kinetic parameters for all investigated mixed oxides

Sample Crystallite size (nm) 2θ for crystallite size BET surface area (m2·g−1) Average pore diameter (nm) Energy band (eV) Rate constant (mg·L−1·min−1) Correlation coefficient R 2 (−)
ZnFe-100 20.7 36.2 110 6.8 2.27 0.0089 0.9886
ZnFe-300 22.4 36.3 46 12 2.29 0.0173 0.9979
ZnFe-500 25.5 36.4 16 27.6 2.31 0.0174 0.981
ZnFe-700 33.7 36.2 9 18.2 2.27 0.0135 0.982
ZnFe-900 41.3 36.3 3 12.8 2.14 — —

FTIR spectroscopy was conducted in order to gain more information on the structure, composition, and functional groups of the synthesized and thermally treated samples. The FTIR spectra of all samples are shown in Figure 3a. Broad bands detected at ∼3,430 and ∼1,630 cm−1 in ZnFe100 were attributed to bending and stretching vibrations of O–H bonds, respectively, due to water molecules adsorbed on the surface of ZnFe100 that was still present after the thermal treatment at 100°C [5,11,13]. In FTIR spectra of ZnFe300, ZnFe500, ZnFe700, and ZnFe900 samples, no bands around 3,400 and 1,630 cm−1 were detected that indicated the absence of any OH vibrations of water molecules. Furthermore, three bands at 1,471, 1,365, and 1,205 cm−1 were distinguished in all samples and could be attributed to C–O stretching, confirming the presence of carbonate species that decreased with the increase of the thermal treatment temperature [13,18]. The bands in the range of 400–800 cm−1 can be considered as lattice vibration modes of metal–OH and metal–oxygen (M–O) [11]. Figure 3b is presented to distinguish the FTIR bands in the mentioned spectral region. All samples with the exception of ZnFe100 revealed distinct vibration band for M–O at ∼530 cm−1 that could reflect the stretching vibration of the M–O bond in the ZnFe2O4 spinel related to the metal cations at the octahedral sites of the spinel lattice [29]. This vibration band was also detected in the ZnFe100 sample but considering the broad and low intensive peaks it can be concluded that the presence of the ZnFe2O4 phase was low. The obtained FTIR results were in accordance with the XRD analysis.

Figure 3 FTIR spectra of ZnFe100, ZnFe300, ZnFe500, ZnFe700, and ZnFe900 in the spectral range from (a) 4,000 to 1,000 cm−1 and (b) 650 to 450 cm−1.
Figure 3

FTIR spectra of ZnFe100, ZnFe300, ZnFe500, ZnFe700, and ZnFe900 in the spectral range from (a) 4,000 to 1,000 cm−1 and (b) 650 to 450 cm−1.

3.2 Morphological properties

SEM images of the investigated samples are shown in Figure 4. As observed from the images, the ZnFe samples had the same morphology indicating the formation of large particles with irregular shapes [15] that are aggregates of very small ones [18]. A slightly different morphology was detected for the ZnFe900 sample that demonstrated a similar surface morphology but with larger compact aggregates of more spherical particles. From the obtained SEM results, it can be concluded that compared to other samples, the ZnFe900 sample formed agglomerations of organized, uniformly sized spherical particles that could most probably have been triggered by higher crystallinity observed by the XRD analysis [5].

Figure 4 SEM images of (a) ZnFe100, (b) ZnFe500, (c) ZnFe700, and (d) ZnFe900.
Figure 4

SEM images of (a) ZnFe100, (b) ZnFe500, (c) ZnFe700, and (d) ZnFe900.

3.3 Textural properties: Surface area and pore size distribution

The textural analysis results are presented in Table 1 and Figure 5. According to the experimental data, the isotherms of all samples could be associated with type IV with a combined H1/H3 hysteresis loop, clearly suggesting that all investigated samples have mesoporous structures (Figure 5a).

Figure 5 Textural analysis of all investigated photocatalysts: (a) nitrogen adsorption–desorption isotherm curves and (b) BJH pore size distribution curves.
Figure 5

Textural analysis of all investigated photocatalysts: (a) nitrogen adsorption–desorption isotherm curves and (b) BJH pore size distribution curves.

Furthermore, the formation of a hysteresis loop at a higher relative pressure (P/P 0) in the range of 0.4–1.00 directly indicated that the mesopores are non-uniform in all investigated photocatalysts [30]. As expected, the surface area of samples decreased with the increase of the thermal treatment temperature due to the decrease of smaller mesopores, particularly obvious for the ZnFe900 sample. The ZnFe100 sample revealed a developed pore size distribution with two peaks: an intense peak at ∼3 nm and a broad peak at ∼30 nm. Upon thermal treatment, the presence of pores with diameters ∼3 nm decreased and completely disappeared in samples thermally treated at temperatures above 500°C (Figure 5b). Additionally, a higher presence of larger mesopores (∼30 nm) was observed in ZnFe300 and ZnFe500 samples, which also gradually disappeared with the temperature increase in ZnFe700 and ZnFe900 samples, being in correlation with the calculated pore volume of samples (Table 1).

3.4 Optical properties

The UV-Vis DRS were applied for energy band gap determination (E g) using the Kubelka–Munk transformation. The reflectance spectra and the plot F(R)2 as a function of E g for the investigated samples are presented in Figure 6. The calculated data for E g for direct transition are presented in Table 1.

Figure 6 Optical measurements for all samples: (a) UV-Vis DRS and (b) Tauc plot for the determination of the energy band gap.
Figure 6

Optical measurements for all samples: (a) UV-Vis DRS and (b) Tauc plot for the determination of the energy band gap.

The results showed that there was no significant difference in E g among investigated samples, ranging from 2.14 to 2.31 eV. The determined E g corresponds to visible light energy. A slightly lower E g achieved for the samples ZnFe900 is likely a consequence of the Fe2O3/Fe3O4 phase formation [4,15].

3.5 Photocatalytic performance

The investigation of photocatalytic efficiency was conducted at room temperature using solar light source radiation (Figure 7). Prior to illumination, the RhB photodegradation without catalysts (photolysis experiments) was also monitored and the results indicated that the RhB pollutant was stable and could not be degraded solely by solar light [31,32]. Additional adsorption measurements were carried out in the dark in the presence of photocatalysts (Figure 7a). Based on these experiments, the RhB concentration did not significantly change during the 90 min dark reaction. Moreover, it can be clearly seen that the adsorption equilibrium was reached after 30 min dark reaction. These results further confirmed that the photocatalytic performance of the samples was attributed only to the photocatalytic reaction, eliminating the possibility of self-degradation and adsorption of RhB solution. The results demonstrated that both photocatalyst and light were required for effective RhB dye degradation.

Figure 7 Photocatalytic tests of ZnFe samples: (a) pre-adsorption measurement of RhB in the dark, followed by RhB photodegradation and (b) photocatalytic efficiency.
Figure 7

Photocatalytic tests of ZnFe samples: (a) pre-adsorption measurement of RhB in the dark, followed by RhB photodegradation and (b) photocatalytic efficiency.

The photocatalytic efficiency of ZnFe samples in RhB photodegradation is presented in Figure 7b. All samples that were thermally treated at temperatures lower than 900°C were active in the RhB photodegradation reaction, whereas the sample ZnFe900 did not show any photocatalytic activity. The samples ZnFe300 and ZnFe500 showed the highest photocatalytic efficiency. When compared to the as-synthesized ZnFe100 sample, the thermal treatment at 300°C and 500°C elevated the photodegradation efficiency significantly. On the contrary, with higher thermal treatment temperatures (700°C and 900°C), the photodegradation efficiency declined probably due to the sintering process that occurred in these samples and could be suggested based on their specific surface areas that were drastically low (9 m2·g−1 for ZnFe700 and 3 m2·g−1 for ZnFe900). These findings are in accordance with previous studies that stated that insufficient photocatalytic performance can be directly related to their poor textural properties such as low surface area and agglomeration [21,22]. The enhanced photocatalytic activity could be additionally explained by the structural, textural, and optical properties. The explanation for the highest photocatalytic activity of ZnFe300 and ZnFe500 could be due to the presence of the highest amount of the ZnFe2O4 spinel phase. Considering that with a further temperature increase, an additional Fe2O3 phase was detected that negatively affected the photocatalytic performances due to the fact that the Fe2O3 phase could act as a charge carrier centre [5]. Additionally, the mesoporous structure of ZnFe300 and ZnFe500 could be beneficial for the adsorption of dye molecules, causing higher photodegradation efficiency. In these samples, the coupling of ZnO and ZnFe2O4 phases resulted in energy bands (from 2.1 to 2.3 eV) that elevated the photodegradation in the solar light spectrum. It was reported that the single ZnFe2O4 phase exhibited significantly lower optical band gap (1.9 eV) when compared to pure ZnO (∼3.1 eV) [30,33]. The energy band gap for the most active samples was ∼2.3 eV, which initiated stronger absorption of light-enabling photogenerated electrons (e−) to facilely transfer between ZnFe2O4 and ZnO and prevent the e−/h+ recombination. Therefore, in general, the photocatalytic performance of photocatalysts under the same irradiation conditions depends on the photoabsorption ability, the surface reaction between photogenerated carriers and surface adsorbed reactants, and the rate of e−/h+ recombination [22].

3.6 Kinetic studies

The results of the kinetic study indicated that the photodegradation of RhB dye follows the zero-order reaction model (Figure 8 and Table 1). Even though previously published studies suggested that the kinetics of organic dye photodegradation can be described with the pseudo-first-order model, recent studies indicated that zero-order kinetics was satisfactory in describing these photocatalytic reactions [34]. The photocatalytic degradation of dye follows the zero-order rate due to (i) the photocatalysts’ surface saturation with organic reactants and/or (ii) the reaction limitation by other participants (electron transfer to O2, oxygen mass transfer, or light supply) [34,35,36].

Figure 8 Photocatalytic degradation zero-order kinetic model (the solid lines show linear fitting for the zero-order kinetic model).
Figure 8

Photocatalytic degradation zero-order kinetic model (the solid lines show linear fitting for the zero-order kinetic model).

3.7 Photodegradation mechanism study

When a photocatalyst is irradiated by light with energy greater than the photocatalyst band gap, the valence band holes ( h VB + ) and conduction band electrons ( e CB − ) are generated. Depending on their oxidation, i.e. reduction power, h VB + and e CB − can initiate a wide range of chemical reactions. The holes can directly oxidize the pollutant dye or react with OH− or H2O, oxidizing them to ˙OH radicals. Furthermore, the photogenerated e CB − can directly reduce the pollutant molecule or react with O2, reducing them to the superoxide radical anion · O 2 − . Therefore, the most important reactive species are e CB − , h VB + , hydroxyl (˙OH), and superoxide ( · O 2 − ) radicals. The contribution of each reactive species in the photocatalytic reaction depends not only on the pollutant chemical properties but also on the type of the used photocatalyst. It was reported that both photogenerated · O 2 − and holes played a critical role in the dye photodegradation using the ZnO/In2O3 composite as a photocatalyst [37]. Additionally, ·OH radicals are found to be the main reactive species in the photodegradation of methylene blue using Au cube-ZnO core–shell nanoparticles [38]. The RhB photodegradation using Ag nanoparticles-decorated ZnO microspheres was found to proceed mainly through the ˙OH radical mechanism [39]. ZnO/Co3O4 hetero-nanostructures were applied for methylene blue removal, and the results showed that the use of ammonium oxalate as hole scavenger increased the degradation efficiency, while the presence of silver nitrate as an electron scavenger diminished the removal efficiency, concluding that both electrons and holes take part in dye photodegradation [40]. Among the active species trapping experiments, LC-MS/MS analysis [41] and DFT calculations [42] were also used as successful tools to elucidate the photodegradation mechanism. Using DFT calculations, the authors found that the nitrogen atoms are the sites most susceptible to the radical attack, followed by tertiary cyclocarbon atoms in RhB photodegradation with Pd-modified TiO2/Bi2O3 as a photocatalyst [42]. The results from LC-MS analysis showed that the mineralization of RhB dye proceeds via de-ethylation, chromophore cleavage, ring-opening, and fragmentation [42]. According to a recent study [41], there are two possible RhB photodegradation pathways. In the first proposed mechanism, following the ˙OH radical attack, de-ethylated product of RhB is formed, after which de-amination and ring opening occur, leading to the formation of hydroquinone and further smaller molecules. The second proposed mechanism suggests that the positive amino group of the RhB molecule is first attacked by ˙O2 −, leading to the elimination of the benzoic acid moiety and formation of the 3,9a-dihydroxanthen-9-one structure with nitro and amino groups, which further decomposed to resorcinol and smaller molecules.

3.8 Effect of pH

The photodegradation efficiency can be strongly influenced by pH variations due to surface charge changes. The effect of pH on photodegradation efficiency can be explained by the following: (i) the dye adsorption on photocatalyst surfaces is affected by pH variations, (ii) the concentration and formation rate of hydroxyl radicals are enhanced in alkaline media; therefore, the number of hydroxide ions available on surfaces are different from acidified solution, and (iii) pH-dependent agglomeration indirectly affects the available surface area for dye adsorption and photon absorption [1,43]. In order to investigate the effect of the initial pH of reaction solutions on the RhB photodegradation efficiency, photocatalytic tests were conducted in the pH range from 2 to 12 for the most efficient photocatalysts (ZnFe300 and ZnFe500). Aqueous solutions of HCl and NaOH were added for adjusting the initial pH and the results are shown after 180 min of solar light irradiation (Figure 9). The initial pH of the RhB solution with photocatalysts was 6.8. It can be observed that the highest efficiency for both the studied photocatalysts was reached at an initial pH of 6.8. Considering that RhB is a cationic dye, the adsorption of cationic species is favoured close to neutral and alkaline pH solutions that initiate negatively charged surfaces of photocatalysts. On the contrary, low pH values trigger positively charged surfaces preventing the adsorption of the RhB cationic dye and acting as repulsive forces towards cationic dyes [1,43].

Figure 9 Effect of pH on the RhB photodegradation efficiency in the presence of ZnFe300 and ZnFe500.
Figure 9

Effect of pH on the RhB photodegradation efficiency in the presence of ZnFe300 and ZnFe500.

These findings are in agreement with other studies, where the optimum working condition for the photodegradation of cationic dyes was pH 7 [9]. Furthermore, the presented results are correlated with the green route intentions where the highest photodegradation efficiency was achieved without any additional adjustment or use of chemicals.

3.9 Stability test

Since the catalysts ZnFe300 and ZnFe500 exhibited the highest efficiency, stability tests were conducted on these photocatalysts. In order to determine the photocatalytic stability, four consecutive photodegradation cycles for RhB were performed under the same operating conditions (Figure 10). For the ZnFe300 photocatalyst, it was observed that after four cycles of consecutive decomposition reactions, there was no reduction in the catalyst efficiency (Figure 10a). The ZnFe500 photocatalyst showed similar photostability as the ZnFe300 catalyst with no significant loss after four consecutive reaction cycles (Figure 10b).

Figure 10 Stability tests for (a) ZnFe300 and (b) ZnFe500 samples for RhB photodegradation under solar light irradiation.
Figure 10

Stability tests for (a) ZnFe300 and (b) ZnFe500 samples for RhB photodegradation under solar light irradiation.

From these analyses, it can be concluded that the stability of these photocatalysts was high and satisfactory, and thus they meet one of the many conditions for their applications in environmental protection in wastewater treatment.

After stability experiments, a leaching test was performed to determine the release of Zn from the ZnFe500 photocatalyst. The results showed that the Zn content after the photocatalytic test was 4.9 mg·L−1, which is below the permissible limits for drinking water (Public Health Service Agency for Toxic Substances and Disease Registry, Public Health Statement, CAS#: 7440-66-6). The detected slight leaching of Zn ions from the photocatalysts after the stability tests could be responsible for the loss of active sites, resulting in a slight reduction of photodegradation efficiency in the presented sample [44].

4 Conclusions

The photocatalytic efficiency of the eco-friendly synthesized Zn/Fe mixed oxides was evaluated in degradation of the cationic RhB dye. The synthesized mixed oxides contained hexagonal wurtzite ZnO as the predominant phase. The thermal treatment led to the formation of the additional ZnFe2O4 spinel phase, while the presence of either the Fe2O3 or Fe3O4 phase was observed in photocatalysts thermally treated at 700°C and 900°C. Textural analysis revealed mesoporous structures in all mixed oxides with non-uniform mesopores, as well as a decrease in the surface area with the increase of the thermal treatment temperature. Investigation of optical properties showed energy band gaps that proved the advantages of mixed oxides synthesis, having narrow bands (from 2.14 to 2.31 eV) when compared to the pure ZnO photocatalyst. The photocatalytic results revealed that ZnFe300 and ZnFe500 mixed oxides exhibited the highest photocatalytic efficiency, probably due to the highest amount of the ZnFe2O4 spinel phase, mesoporous structure, and the optimal energy band gap of ∼2.30 eV that initiated higher light-harvesting efficiency. The RhB photodegradation followed zero-order kinetics, indicating complete coverage of active sites by the RhB substrate. The photocatalysts showed the highest efficiency at the natural pH (6.8), in accordance with green synthesis principles. ZnFe300 and ZnFe500 photocatalysts showed high stability with negligible leaching of Zn2+ ions, indicating their potential application in environmental protection processes. The results demonstrated that the developed simple, safe, non-toxic, eco-friendly, and cost-effective synthesis method enabled favourable interactions among active phases triggering excellent photocatalytic performance making these photocatalysts suitable for use in wastewater remediation.

  1. Funding information: This work was financially supported by the Ministry of Science, Technological Development and Innovation of the Republic of Serbia (Grant No. 451-03-9/2021-14/200134 and Grant No. 451-03-47/2023-01/200026).

  2. Author contributions: Milica Hadnadjev-Kostic: writing – original draft, conceptualization, methodology, investigation, formal analysis, data curation, validation; Djurdjica Karanovic: formal analysis, data curation, validation; Tatjana Vulic: writing – review and editing, conceptualization, validation; Jasmina Dostanić: formal analysis, data curation; Davor Lončarević: formal analysis, data curation. All authors have read and agreed to the published version of the manuscript.

  3. Conflict of interest: The authors state no conflict of interest.

  4. Data availability statement: All relevant data are within the article.

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Received: 2022-12-27
Revised: 2023-03-15
Accepted: 2023-03-28
Published Online: 2023-04-26

© 2023 the author(s), published by De Gruyter

This work is licensed under the Creative Commons Attribution 4.0 International License.

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https://doi.org/10.1515/gps-2022-8153
Keywords for this article
mixed metal oxides; organic dye pollutant; rhodamine B; photodegradation efficiency
Creative Commons
BY 4.0

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  22. Electrochemical analysis of the dissolution of gold in a copper–ethylenediamine–thiosulfate system
  23. Characterisation of carbonate lake sediments as a potential filler for polymer composites
  24. Evaluation of nano-selenium biofortification characteristics of alfalfa (Medicago sativa L.)
  25. Quality of oil extracted by cold press from Nigella sativa seeds incorporated with rosemary extracts and pretreated by microwaves
  26. Heteropolyacid-loaded MOF-derived mesoporous zirconia catalyst for chemical degradation of rhodamine B
  27. Recovery of critical metals from carbonatite-type mineral wastes: Geochemical modeling investigation of (bio)hydrometallurgical leaching of REEs
  28. Photocatalytic properties of ZnFe-mixed oxides synthesized via a simple route for water remediation
  29. Attenuation of di(2-ethylhexyl)phthalate-induced hepatic and renal toxicity by naringin nanoparticles in a rat model
  30. Novel in situ synthesis of quaternary core–shell metallic sulfide nanocomposites for degradation of organic dyes and hydrogen production
  31. Microfluidic steam-based synthesis of luminescent carbon quantum dots as sensing probes for nitrite detection
  32. Transformation of eggshell waste to egg white protein solution, calcium chloride dihydrate, and eggshell membrane powder
  33. Preparation of Zr-MOFs for the adsorption of doxycycline hydrochloride from wastewater
  34. Green nanoarchitectonics of the silver nanocrystal potential for treating malaria and their cytotoxic effects on the kidney Vero cell line
  35. Carbon emissions analysis of producing modified asphalt with natural asphalt
  36. An efficient and green synthesis of 2-phenylquinazolin-4(3H)-ones via t-BuONa-mediated oxidative condensation of 2-aminobenzamides and benzyl alcohols under solvent- and transition metal-free conditions
  37. Chitosan nanoparticles loaded with mesosulfuron methyl and mesosulfuron methyl + florasulam + MCPA isooctyl to manage weeds of wheat (Triticum aestivum L.)
  38. Synergism between lignite and high-sulfur petroleum coke in CO2 gasification
  39. Facile aqueous synthesis of ZnCuInS/ZnS–ZnS QDs with enhanced photoluminescence lifetime for selective detection of Cu(ii) ions
  40. Rapid synthesis of copper nanoparticles using Nepeta cataria leaves: An eco-friendly management of disease-causing vectors and bacterial pathogens
  41. Study on the photoelectrocatalytic activity of reduced TiO2 nanotube films for removal of methyl orange
  42. Development of a fuzzy logic model for the prediction of spark-ignition engine performance and emission for gasoline–ethanol blends
  43. Micro-impact-induced mechano-chemical synthesis of organic precursors from FeC/FeN and carbonates/nitrates in water and its extension to nucleobases
  44. Green synthesis of strontium-doped tin dioxide (SrSnO2) nanoparticles using the Mahonia bealei leaf extract and evaluation of their anticancer and antimicrobial activities
  45. A study on the larvicidal and adulticidal potential of Cladostepus spongiosus macroalgae and green-fabricated silver nanoparticles against mosquito vectors
  46. Catalysts based on nickel salt heteropolytungstates for selective oxidation of diphenyl sulfide
  47. Powerful antibacterial nanocomposites from Corallina officinalis-mediated nanometals and chitosan nanoparticles against fish-borne pathogens
  48. Removal behavior of Zn and alkalis from blast furnace dust in pre-reduction sinter process
  49. Environmentally friendly synthesis and computational studies of novel class of acridinedione integrated spirothiopyrrolizidines/indolizidines
  50. The mechanisms of inhibition and lubrication of clean fracturing flowback fluids in water-based drilling fluids
  51. Adsorption/desorption performance of cellulose membrane for Pb(ii)
  52. A one-pot, multicomponent tandem synthesis of fused polycyclic pyrrolo[3,2-c]quinolinone/pyrrolizino[2,3-c]quinolinone hybrid heterocycles via environmentally benign solid state melt reaction
  53. Green synthesis of silver nanoparticles using durian rind extract and optical characteristics of surface plasmon resonance-based optical sensor for the detection of hydrogen peroxide
  54. Electrochemical analysis of copper-EDTA-ammonia-gold thiosulfate dissolution system
  55. Characterization of bio-oil production by microwave pyrolysis from cashew nut shells and Cassia fistula pods
  56. Green synthesis methods and characterization of bacterial cellulose/silver nanoparticle composites
  57. Photocatalytic research performance of zinc oxide/graphite phase carbon nitride catalyst and its application in environment
  58. Effect of phytogenic iron nanoparticles on the bio-fortification of wheat varieties
  59. In vitro anti-cancer and antimicrobial effects of manganese oxide nanoparticles synthesized using the Glycyrrhiza uralensis leaf extract on breast cancer cell lines
  60. Preparation of Pd/Ce(F)-MCM-48 catalysts and their catalytic performance of n-heptane isomerization
  61. Green “one-pot” fluorescent bis-indolizine synthesis with whole-cell plant biocatalysis
  62. Silica-titania mesoporous silicas of MCM-41 type as effective catalysts and photocatalysts for selective oxidation of diphenyl sulfide by H2O2
  63. Biosynthesis of zinc oxide nanoparticles from molted feathers of Pavo cristatus and their antibiofilm and anticancer activities
  64. Clean preparation of rutile from Ti-containing mixed molten slag by CO2 oxidation
  65. Synthesis and characterization of Pluronic F-127-coated titanium dioxide nanoparticles synthesized from extracts of Atractylodes macrocephala leaf for antioxidant, antimicrobial, and anticancer properties
  66. Effect of pretreatment with alkali on the anaerobic digestion characteristics of kitchen waste and analysis of microbial diversity
  67. Ameliorated antimicrobial, antioxidant, and anticancer properties by Plectranthus vettiveroides root extract-mediated green synthesis of chitosan nanoparticles
  68. Microwave-accelerated pretreatment technique in green extraction of oil and bioactive compounds from camelina seeds: Effectiveness and characterization
  69. Studies on the extraction performance of phorate by aptamer-functionalized magnetic nanoparticles in plasma samples
  70. Investigation of structural properties and antibacterial activity of AgO nanoparticle extract from Solanum nigrum/Mentha leaf extracts by green synthesis method
  71. Green fabrication of chitosan from marine crustaceans and mushroom waste: Toward sustainable resource utilization
  72. Synthesis, characterization, and evaluation of nanoparticles of clodinofop propargyl and fenoxaprop-P-ethyl on weed control, growth, and yield of wheat (Triticum aestivum L.)
  73. The enhanced adsorption properties of phosphorus from aqueous solutions using lanthanum modified synthetic zeolites
  74. Separation of graphene oxides of different sizes by multi-layer dialysis and anti-friction and lubrication performance
  75. Visible-light-assisted base-catalyzed, one-pot synthesis of highly functionalized cinnolines
  76. The experimental study on the air oxidation of 5-hydroxymethylfurfural to 2,5-furandicarboxylic acid with Co–Mn–Br system
  77. Highly efficient removal of tetracycline and methyl violet 2B from aqueous solution using the bimetallic FeZn-ZIFs catalyst
  78. A thermo-tolerant cellulase enzyme produced by Bacillus amyloliquefaciens M7, an insight into synthesis, optimization, characterization, and bio-polishing activity
  79. Exploration of ketone derivatives of succinimide for their antidiabetic potential: In vitro and in vivo approaches
  80. Ultrasound-assisted green synthesis and in silico study of 6-(4-(butylamino)-6-(diethylamino)-1,3,5-triazin-2-yl)oxypyridazine derivatives
  81. A study of the anticancer potential of Pluronic F-127 encapsulated Fe2O3 nanoparticles derived from Berberis vulgaris extract
  82. Biogenic synthesis of silver nanoparticles using Consolida orientalis flowers: Identification, catalytic degradation, and biological effect
  83. Initial assessment of the presence of plastic waste in some coastal mangrove forests in Vietnam
  84. Adsorption synergy electrocatalytic degradation of phenol by active oxygen-containing species generated in Co-coal based cathode and graphite anode
  85. Antibacterial, antifungal, antioxidant, and cytotoxicity activities of the aqueous extract of Syzygium aromaticum-mediated synthesized novel silver nanoparticles
  86. Synthesis of a silica matrix with ZnO nanoparticles for the fabrication of a recyclable photodegradation system to eliminate methylene blue dye
  87. Natural polymer fillers instead of dye and pigments: Pumice and scoria in PDMS fluid and elastomer composites
  88. Study on the preparation of glycerylphosphorylcholine by transesterification under supported sodium methoxide
  89. Wireless network handheld terminal-based green ecological sustainable design evaluation system: Improved data communication and reduced packet loss rate
  90. The optimization of hydrogel strength from cassava starch using oxidized sucrose as a crosslinking agent
  91. Green synthesis of silver nanoparticles using Saccharum officinarum leaf extract for antiviral paint
  92. Study on the reliability of nano-silver-coated tin solder joints for flip chips
  93. Environmentally sustainable analytical quality by design aided RP-HPLC method for the estimation of brilliant blue in commercial food samples employing a green-ultrasound-assisted extraction technique
  94. Anticancer and antimicrobial potential of zinc/sodium alginate/polyethylene glycol/d-pinitol nanocomposites against osteosarcoma MG-63 cells
  95. Nanoporous carbon@CoFe2O4 nanocomposite as a green absorbent for the adsorptive removal of Hg(ii) from aqueous solutions
  96. Characterization of silver sulfide nanoparticles from actinobacterial strain (M10A62) and its toxicity against lepidopteran and dipterans insect species
  97. Phyto-fabrication and characterization of silver nanoparticles using Withania somnifera: Investigating antioxidant potential
  98. Effect of e-waste nanofillers on the mechanical, thermal, and wear properties of epoxy-blend sisal woven fiber-reinforced composites
  99. Magnesium nanohydroxide (2D brucite) as a host matrix for thymol and carvacrol: Synthesis, characterization, and inhibition of foodborne pathogens
  100. Synergistic inhibitive effect of a hybrid zinc oxide-benzalkonium chloride composite on the corrosion of carbon steel in a sulfuric acidic solution
  101. Review Articles
  102. Role and the importance of green approach in biosynthesis of nanopropolis and effectiveness of propolis in the treatment of COVID-19 pandemic
  103. Gum tragacanth-mediated synthesis of metal nanoparticles, characterization, and their applications as a bactericide, catalyst, antioxidant, and peroxidase mimic
  104. Green-processed nano-biocomposite (ZnO–TiO2): Potential candidates for biomedical applications
  105. Reaction mechanisms in microwave-assisted lignin depolymerisation in hydrogen-donating solvents
  106. Recent progress on non-noble metal catalysts for the deoxydehydration of biomass-derived oxygenates
  107. Rapid Communication
  108. Phosphorus removal by iron–carbon microelectrolysis: A new way to achieve phosphorus recovery
  109. Special Issue: Biomolecules-derived synthesis of nanomaterials for environmental and biological applications (Guest Editors: Arpita Roy and Fernanda Maria Policarpo Tonelli)
  110. Biomolecules-derived synthesis of nanomaterials for environmental and biological applications
  111. Nano-encapsulated tanshinone IIA in PLGA-PEG-COOH inhibits apoptosis and inflammation in cerebral ischemia/reperfusion injury
  112. Green fabrication of silver nanoparticles using Melia azedarach ripened fruit extract, their characterization, and biological properties
  113. Green-synthesized nanoparticles and their therapeutic applications: A review
  114. Antioxidant, antibacterial, and cytotoxicity potential of synthesized silver nanoparticles from the Cassia alata leaf aqueous extract
  115. Green synthesis of silver nanoparticles using Callisia fragrans leaf extract and its anticancer activity against MCF-7, HepG2, KB, LU-1, and MKN-7 cell lines
  116. Algae-based green AgNPs, AuNPs, and FeNPs as potential nanoremediators
  117. Green synthesis of Kickxia elatine-induced silver nanoparticles and their role as anti-acetylcholinesterase in the treatment of Alzheimer’s disease
  118. Phytocrystallization of silver nanoparticles using Cassia alata flower extract for effective control of fungal skin pathogens
  119. Antibacterial wound dressing with hydrogel from chitosan and polyvinyl alcohol from the red cabbage extract loaded with silver nanoparticles
  120. Leveraging of mycogenic copper oxide nanostructures for disease management of Alternaria blight of Brassica juncea
  121. Nanoscale molecular reactions in microbiological medicines in modern medical applications
  122. Synthesis and characterization of ZnO/β-cyclodextrin/nicotinic acid nanocomposite and its biological and environmental application
  123. Green synthesis of silver nanoparticles via Taxus wallichiana Zucc. plant-derived Taxol: Novel utilization as anticancer, antioxidation, anti-inflammation, and antiurolithic potential
  124. Recyclability and catalytic characteristics of copper oxide nanoparticles derived from bougainvillea plant flower extract for biomedical application
  125. Phytofabrication, characterization, and evaluation of novel bioinspired selenium–iron (Se–Fe) nanocomposites using Allium sativum extract for bio-potential applications
  126. Erratum
  127. Erratum to “Synthesis, characterization, and evaluation of nanoparticles of clodinofop propargyl and fenoxaprop-P-ethyl on weed control, growth, and yield of wheat (Triticum aestivum L.)”
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