A new powerful magnetic dark catalyst based on rGO/Fe3O4/CdSe nanocomposite for ultrafast degradation of methylene blue dye

doi:10.21203/rs.3.rs-4851672/v1

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A new powerful magnetic dark catalyst based on rGO/Fe3O4/CdSe nanocomposite for ultrafast degradation of methylene blue dye

https://doi.org/10.21203/rs.3.rs-4851672/v1

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published 03 Oct, 2024

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In the present study, rGO/Fe3O4/CdSe as a dark catalyst material was synthesized by a refluxing method. The synthesized magnetic nanocomposites were studied by various analyzes such as Fourier transform infrared (FTIR), energy-dispersive X-ray spectroscopy (EDS), field emission scanning electron microscopy (FESEM), X-ray diffractometer (XRD), Raman, Zeta and vibrating sample magnetometer (VSM). XRD, EDS, FESEM and FTIR spectra showed that the nanocomposites were successfully synthesized. Absorption spectrum was used to determine the dark catalyst activity of rGO/Fe3O4/CdSe nanocomposite. Analysis of the absorption spectrum showed that the prepared nanocomposites degrade the MB organic dye completely after 2 min of stirring in the dark, also doing experiment at different pH showed that the best performance for the degradation of MB occurs in neutral and alkaline media. The Raman spectrum analyzes showed that the Fe3O4/CdSe QDs were correctly incorporated on the reduced graphene oxide (rGO) nanosheets. Zeta potential analysis showed that rGO/Fe3O4/CdSe has a large amount of negative charge on its surface, also the radical scavenger experiment showed that electrons play an essential role in the process of degradation. VSM analysis showed that the prepared nanocomposites have excellent superparamagnetic behavior, this advantage enables the easy collection of nanocatalysts by magnets from wastewater after dye degradation.

rGO/Fe3O4/CdSe

Dark catalyst

Dye degradation

Wastewater treatment

Magnetic nanocomposite

Environmental issues such as the water shortage crisis and increasing the discharge of dye effluents from various industries to the water resources, have become an important challenge. So, in order to reduce the risks caused by water pollutants for humans and the ecology, due to their toxicity and non-biodegradability, the treatment of water pollutant matrices is an issue that should be systematically investigated [1–2]. Todays, preparation and fabrication of nanostructures that can improve catalytic performance and have strong dye degradation in a short time has attracted a lot of attention.

Recently, many efforts have been made to increase the photocatalytic efficiency of various nanostructures in relation to various pollutants under UV light or sunlight [3]. Kumar et al, synthesized rGO/Fe₃O₄ nanocomposites for degradation of MB by solvothermal method [4]. Zhang et al, synthesized CdSe QDs@ Fe-based composites with heterojunction at atmospheric pressure by stirring in oil bath to enhance the photocatalytic degradation efficiency of rhodamine B (RhB) in the visible light conditions [5].

Conventional methods of removing organic dyes from wastewater treatment include filtration processes, chemical precipitation processes, biological decomposition, reverse osmosis and absorption [5–7]. These methods are not very efficient and economical to remove organic dye from wastewater. Advanced oxidation processes (AOP) like as ozonation, fenton and semiconductor-based photocatalyst, have recently attracted much attention for the removal of organic dyes from industrial effluents. In AOP methods, there is a need to create free radical species such as superoxide and hydroxyl radicals [8].

Due to narrow and favorable conduction band gap (Eg ≈ 1.74 eV) and as effective type in the II-VI group of semiconductor family, also tunable and size-dependent electronic properties, CdSe has been widely studied as photocatalysts [5]. Particularly, the absorption band of CdSe includes the entire visible light region. Also CdSe nanoparticles are introduced as an excellent photocatalyst due to the rapid generation of electron-hole pairs upon light excitation [2–9]. However, photoelectron-hole pairs of CdSe recombine easily and quickly. Therefore, increasing the lifetime of photo-generated pairs, due to the transfer of holes and electrons between the two coupled semiconductors, plays an important role in optical activity [5–10]. In order to prevent recombination of electrons and holes, graphene are a good option that can be used. One of the unique properties of graphene quantum dots (GQDs) is that they can absorb long-wavelengths and emit UV photons with shorter wavelengths, Due to the up conversion effect. Also, the GQDs band confirm the separation of charge and allows to electrons transfers easily from of the excited surface of catalyst and enhance the amount of available charge carriers for reactions in aqueous media. Therefore, it can be find out that the interaction between GQDs and catalyst increases the catalytic performance of the catalyst [2–11]. One of the important challenges in the practical application of graphene-based composites is its easy separation and recycling for reuse. For this purpose, Fe₃O₄ nanoparticles can be added to the compound due to their significant magnetic properties. In addition, due to its unique properties, Fe₃O₄ nanoparticles can interact with graphene oxide and lead to improved properties and overall performance. Also, having high surface area and good catalytic activity, iron oxide nanoparticles can promote efficient charge transfer kinetics and increase the catalytic performance of composite materials [8–12]. Therefore, considering all of above, in this research we have prepared rGO/Fe₃O₄/CdSe magnetic nanocomposite by a refluxing method. Prepared nanocomposite was investigated by different analysis and indicated excellent dark catalyst performance for the degradation of MB organic dye.

2.1. Materials

Cadmium sulfate(CdSO₄), Thioglycolic acid (TGA), Sodium hydroxide (NaOH), Potassium permanganate (KMnO₄), Iron (III) chloride hexahydrate (FeCl₃×6H₂O), Phosphoric acid (H₃PO₄), Sulfuric acid (H₂SO₄), Hydrogen peroxide (H₂O₂) (37%), graphite flakes (99%), Hydrochloric acid (HCl) (37%) and ammonium solution (25%), were purchased from the Merck chemical company. Sodium selenite (Na₂SeO₃) was purchased from Sigma-Aldrich Company.

2.2. Preparation of CdSe

Fast and easy microwave method was used for the synthesis of CdSe QDs [13]. In the first step, 0.064 g of cadmium sulfate was solved in 30 ml of deionized (DI) water for 25 min on a magnetic stirrer, then 50 µl of thioglycolic acid (TGA) was added to the cadmium sulfate solution as a capping agent. Due to the use of thiols as capping agent, to convert the media from acidic to alkaline by adding NaOH, pH reached to 9.5. Separately, 0.43 g of sodium selenite (Na₂SeO₃) was poured into a beaker containing 20 ml of DI water and stirred for 15 min on a magnetic stirrer. In the second step, with the preparation of solutions containing ions, the solution containing Se²⁻ was added to the solution containing Cd²⁺ which was being stirred on the magnetic stirrer. In the third step, the final solution, which was 50 ml, was exposed in the microwave radiation center for 90 s with a power of 720w. Finally, for the next use, the samples must be in powder form, the obtained solution was centrifuged for 5 min at 6000 rpm, then the samples were collected and dried at room temperature.

2.3. Preparation of Fe₃O₄

For the synthesis of Fe₃O₄, in the first step, 0.47 g of sodium sulfite (Na₂SO₃) was added to 12.5 ml of DI water and placed on a magnetic stirrer for 3 min to dissolve. Separately, 250 µl of HCl 0.2 mM and 2.07g of FeCl₃×6H₂O were added to a beaker that contained 20 ml of DI water and sonicated by ultrasonic probe for about 3 min, until the color of solution turns to yellow. In the second step, 10 ml of Na₂SO₃ (0.3 M) solution was slowly added to the beaker containing iron chloride and hydrochloric acid and sonicated for 8 min until the solution turned to yellow again. The solution prepared in the previous step was added to 30 mL of ammonia dissolved in 170 mL of DI water and sonicated for about 30 min. Finally, for the next use the Fe₃O₄ were separated by a magnet and dried at 45°C for 24 h after washing 5 times.

2.4. Synthesis of CdSe/Fe₃O₄ nanocomposites

For the synthesis of CdSe/Fe₃O₄ nanocomposites, 0.1g of pre-prepared Fe₃O₄ were dispersed in 50 ml DI water for 3 min by ultrasonic probe. Simultaneously, in another beaker, 0.1 g of CdSe powder was dispersed in 50 ml of DI water for 3 min. Then, the Fe₃O₄ solution was slowly injected into the beaker containing the CdSe solution and dispersed by an ultrasonic probe for 30 min. The obtained solution was refluxed for 24 h at 80°C. Then, to obtain the final product, the obtained nanocomposite was washed several times after being separated by a magnet, then dried in an oven at 44°C for 24 h [14].

2.5. Preparation of GO

The synthesis of graphene oxide (GO) was carried out by the previously reported hummer method [15]. Briefly, 67.5 ml of sulfuric acid, 10 ml of phosphoric acid and 22.4 ml of nitric acid were poured into a beaker placed on a magnetic stirrer and mixed for 10 min. Then 1 g of ground graphite powder was slowly added to the acid solution. After adding graphite powder, the solution was stirred for 30 min on a magnetic stirrer. Then, the beaker was placed in an ice bath and 6 g of potassium permanganate was slowly (1 g per 15 min) added to the solution in the ice bath during 90 min. The beaker containing the solution was placed on a heater with a temperature of 40 to 45°C for 2 h until the solution turned a muddy green color. Then the beaker containing the solution was removed from the heater and 100 ml of DI water was added to it at a uniform rate. After that, the beaker containing the solution for 1h was placed in an oil bath whose temperature was set at 85°C. Then the beaker containing the solution was taken out of the oil bath and while stirring on the magnetic stirrer, 15 ml of hydrogen peroxide and 120 ml of DI water simultanesly were added to the solution. The remaining solution was passed through filter until the acid was separated from the solution. Then washed with DI water and hydrochloric acid (HCl) at a ratio of 10:1. The remaining sediments were sonicated for 30 min to disperse, then washed several times until the pH of the compound reached to 5–7. Finally, the solution was placed in a centrifuge at 6000 rpm for 10 min, and then the collected sediments were dried in an oven at 40°C.

2.6. Preparation of rGO /Fe₃O₄

For the synthesis of rGO/F₃O₄, in the first step, 2.07 g of FeCl₃×6H₂O was dissolved in a beaker containing 20 ml of DI water. Then the obtained solution was dispersed by adding 250 µl of 0.2 mM HCl for 3 min by using an ultrasonic probe until it turned to yellow. In the second step, 10 ml of prepared Na₂SO₃ (0.3 M) solution was added to the solution prepared in the previous step, and then it was dispersed by an ultrasonic probe for 8 min until it turned to yellow again. Separately, 0.02 g of prepared GO powder was dispersed in 30 ml of DI water for 30 min by ultrasonic probe until the solution turned to brown. The solution contain GO was added to the solution prepared in the second step and subjected to sonication for 10 min, then added to a beaker containing 30 ml of ammonia 33% mixed in 170 ml of DI water and dispersed by ultrasonic probe for 30 min. Finally, the rGO/F₃O₄ compound was collected by a magnet and separated from aqueous media, then after washing 5 times, dried an oven in 45°C for 24 h.

2.7. Synthesis of rGO /Fe₃O₄/CdSe magnetic nanocomposites

For the synthesis of rGO/Fe₃O₄/CdSe nanocomposites, first, 0.1 g of pre-prepared rGO/F₃O₄ was dispersed in 50 ml of DI water. Separately, 0.1 g of pre-prepared CdSe QDs were dispersed in 50 ml of DI water. Then, the solution containing CdSe was added to the rGO/F₃O₄ solution. The obtained compound was refluxed for 24 h at 80°C. Finally, the rGO/Fe₃O₄/CdSe sediments were collected by a magnet and separated from aqueous media and dried for 24 h at 44°C to obtain rGO/Fe₃O₄/CdSe nanocomposites.

2.8. Dark catalyst study

To study about the degradation rate of MB organic dye, absorption spectrum was used to determine the dark catalyst activity of rGO/Fe₃O₄/CdSe nanocomposite. For this purpose, 30 mg of catalyst was dispersed in 22.5 ml of DI water in an ultrasonic bath for about 3 min. Subsequently, the prepared solution was reacted with 10 ppm of MB organic dye, then it was stirred in a dark chamber with different time intervals.

3.1. Studying the structural characteristics and morphology

3.1.1. XRD pattern

An X-ray diffractometer (Cu Kα) was used to study the crystalline phase of the produced nanocomposites. Figure 1A shows the XRD pattern of the samples. Pattern (a) in Fig. 1A, corresponds to the pure Fe₃O₄, which has distinct peaks at 2Ѳ = 30.17^∘, 35.53^∘, 43.2^∘, 53.55^∘, 57.12^∘ and 62.69^∘, which is refers to the lattice planes points of (220), (311), (400), (422), (511) and (440). The existing peaks indicate that Fe₃O₄ corresponds to the cubic structure [16–17]. Also, Pattern (b) in Fig. 1A shows the XRD corresponding to pure CdSe, which has peaks at 2Ѳ = 26.12^∘, 30.11^∘ and 43.3^∘, that respectively refer to (111), (220), and (311) lattice planes. CdSe exists in both zinc-blend (FCC) and wurtzite (hexagonal) structures. Comparing the peaks in pattern (b) with previous studies shows that the structure of CdSe is cubic [5–18]. Pattern (c) in Fig. 1A shows the XRD of CdSe/Fe₃O₄ nanocomposite, the diffraction peaks indicate the overlapping of CdSe with Fe₃O₄ and the formation of CdSe/Fe₃O₄ structure [19]. Pattern (d) in Fig. 1A is the XRD of rGO/Fe₃O₄/CdSe nanocomposite. It can be seen that, due to the deposition of iron oxide and cadmium selenide particles on the rGO surface, the peaks of rGO not appear clearly [16].

3.1.2. VSM analysis

VSM was used to determine the magnetic properties of Fe₃O₄/CdSe and rGO/Fe₃O₄/CdSe at room temperature. From the obtained results that are shown in Fig. 1B, it can be seen that both prepared composites have superparamagnetic behavior [20]. The obtained magnetic saturation (Ms) values were about 64.48 and 62.50 emu/g for Fe₃O₄/CdSe and rGO/Fe₃O₄/CdSe, respectively. Compared with Fe₃O₄/CdSe, it can be inferred that the saturation magnetization of rGO/Fe₃O₄/CdSe decreased, that may be related to the low percentage of Fe₃O₄ in the rGO/Fe₃O₄/CdSe composite [21]. Saturation magnetization of rGO/Fe₃O₄/CdSe nanocomposites indicates that it has excellent superparamagnetic behavior. Therefore, the challenge of separating nanocatalyst from the wastewater can be solved simply by a magnet after the degradation process [22].

3.1.3. FTIR spectrums

In order to analyze the functional group and determine the structural integrity of the catalysts, FTIR spectroscopy of the composites was performed. FTIR involves observing the vibration of molecules excited by infrared radiation. Figure 2A indicates the FTIR spectrum of GO, Fe₃O₄/CdSe binary and rGO/Fe₃O₄/CdSe ternary nanocomposite. As can be seen in the relevant spectrum, there are peaks in the wave numbers of 547, 1228, 1379, 1655, 3449 and 3725cm^− 1. The bands near 547 cm^− 1 and 1228 cm^− 1 originate from the stretching vibrations of Fe-O and the vibrational absorption of C-O bonds, which indicates that Fe₃O₄ QDs are coordinated with rGO [5–23]. The peaks in wave number 1379 and 1655 cm^− 1 are respectively referred to C-OH and C = C bonds [2–7]. The distinctive broad band that exists from the wave number of 3250 to 3750 cm^− 1 are related to the OH groups involved in H bonds [5].

3.1.4. Raman spectrums

Raman spectroscopy can determine the presence of CdSe, Fe₃O₄ and rGO in the nanocomposites [24]. Figure 2B indicates the Raman spectrum of Fe₃O₄/CdSe, GO and rGO/Fe₃O₄/CdSe. Pattern (a) in Fig. 2B shows the Raman spectrum of Fe₃O₄/CdSe nanocomposites, which has peaks at 235, 415, 439 and 800 cm^− 1. The two peaks around 235 cm^− 1and 415 cm^− 1 are related to LO₁ and LO₂ phonon modes in CdSe [25]. Weak peaks around 439 and 800 cm^− 1 are attributed to Fe₃O₄ [26]. GO is usually analyzed by two peaks. Pattern (b) in Fig. 2B indicates the Raman spectrum of pure GO, and pattern (c) shows the Raman spectrum of rGO/Fe₃O₄/CdSe nanocomposites. There are two peaks at 1320 cm^− 1and 1605 cm^− 1, which respectively represent the D and G bands of rGO. G pattern is related to the first order scattering of E₂g photons produced by sp2 carbon atom and D pattern is produced by sp3 carbon atom, which shows the graphitization degree of graphene [24]. A high value of intensity ratio indicates that the graphite structure has more crystal defects in its lattice and has a more distortion. The D/G ratio for rGO/Fe₃O₄/CdSe was 1.15. As shown in pattern (c) in Fig. 2B, there is a small shift to the left in the characteristic peak in the D band for rGO/Fe₃O₄/CdSe, indicating that the Fe₃O₄/CdSe QDs are correctly grown on the rGO nanosheets [27].

3.1.5. FESEM and EDS analyses

3.2. Dye degradation study

3.2.1. MB degradation

Absorption spectrum was used to study the ability of magnetic nanocomposites to degrade MB dye. The reduction of the characteristic absorption peak is a way that can be used to measure the degradation of MB dye molecules after the catalytic reaction. To investigate the effectiveness of Fe₃O₄/CdSe and rGO/Fe₃O₄/CdSe magnetic nanocomposite in degradation of MB, 30 mg of catalyst was reacted with 10 ppm of MB. The degradation rate of the samples are shown in Fig. 5. As shown in Fig. 5a, degradation efficiency of Fe₃O₄/CdSe was 55%, but, Fig. 5b indicate that by adding graphene to the compound, the degradation efficiency reached to 100% only after 2 min stirring in the darkness. Table 1 shows the reaction time and degradation efficiency of different dark catalysts and photocatalysts with MB dye in comparison with prepared rGO/Fe₃O₄/CdSe magnetic dark nanocatalyst.

Table 1

Comparisons of MB dye degradation between the prepared rGO/ Fe₃O₄/CdSe nanocomposite and some previous reported dark and photocatalysts.
S. NO.	Nanocatalyst	Photo/Dark catalyst	Degradation efficiency	Time (min)	Ref.
1	MnTiO₃	Photocatalyst	75%	240	[31]
2 3	CdSe- rGO CdTe/ZnSe	Photocatalyst Photocatalyst	70% 76%	210 120	[32] [3]
4	ZnO–SnO₂	Photocatalyst	96.53%	60	[33]
5	GO/TiO₂	Photocatalyst	99%	60	[34]
6	rGO/TiO₂	Photocatalyst	90%	15	[35]
7	Ag–In–Ni– S	Dark catalyst	98%	12	[36]
8	rGO/Fe₃O₄/CdSe	Dark catalyst	100%	2	Present work

3.2.2. Study effect of rGO/Fe₃O₄/CdSe catalyst mass

Another important factor that was studied in the dye degradation efficiency was the mass of the catalyst. To investigate the effect of rGO/Fe₃O₄/CdSe mass on the degradation rate of methylene blue, 10, 20, 30 and 40 mg of catalyst were reacted with 10 ppm of MB dye, then stirred in darkness. As shown in Fig. 6a, it can be find out that the best catalyst weight can be use is 30 mg, because it obtained the highest dark degradation efficiency of 100% and the MB solution was degradated completely after 2 min. Degradation efficiency increased from 10 to 30 mg due to the increase in the number of active sites in the degradation process, increasing the mass more than 30 mg did not change the degradation time [27]. Therefore, 30 mg was selected as the optimal condition of magnetic nanocomposite in the degradation process for more detailed study.

3.2.3. Study reusability of rGO/Fe₃O₄/CdSe

Figure 6b, shows the effect of prepared rGO/Fe₃O₄/CdSe nanocomposite during reuse analysis. The stability and recyclability of nanocatalysts are also very important for practical applications. Surface electrons play an important role in the dark degradation process. Since the number of surface electrons decreases during the reaction with dye molecules in the degradation process, it is expected that the degradation efficiency will decrease in the subsequent cycles [7]. In order to check the reuse of the prepared catalyst after the degradation in the first step, the reacted nanocomposite with MB was separated from the media by a magnet. Then, in the second step, the degradation process was repeated by adding 10 ppm of MB with the same samples of the first step. After 4 reuse of the prepared dark nanocatalysts for degradation of MB, it still has 83% degradation efficiency. This level of degradation indicate that, the prepared dark catalyst still has the necessary surface electrons for the degradation of organic dyes.

3.2.4. Study of pH effect on degradation

The pH was studed as another factor that can be effective in the practical use of prepared nanocomposites and degradation efficiency. Sodium hydroxide (NaOH) and Hydrochloric acid (HCl) were used for this purpose. According to the pH study, which are shown in the Fig. 7a, as the pH increases from 1 to 3, the degradation efficiency increases considerably, then, the highest degradation occurs in neutral and alkaline media. Therefore, it can be understood that prepared nanocomposites perform much better in neutral and alkaline media than in acidic media.

3.2.5. Zeta potential analysis

Figure 7b shows the Zeta potential of the samples. Zeta potential was used to measure the amount of charge on the surface of CdSe/Fe₃O₄ and rGO/CdSe/Fe₃O₄ nanocomposites. Depending on its sign and amount, surface charges strongly affects the degradation of organic dyes [28].The results of zeta potential showed that the amount of negative charge on the Fe₃O₄/CdSe surface is about − 12 mV, which increases to -28 mV by adding graphene to the structure. Graphene is known as a two-dimensional semimetal with a tiny overlap between the valence and conduction bands and exhibits a strong dipole electric field effect [29]. The increasing trend of about 16 mV in the value of zeta potential for rGO/Fe₃O₄/CdSe nanocomposite may be due to the functionalization of rGOs during partial reduction, and hence it has a higher surface negative charge density than Fe₃O₄/CdSe [30]. Therefore, by increasing the surface charge, it can be expected that the ability of rGO/Fe₃O₄/CdSe as a dark catalyst in the dye degradation will increase [27].

3.2.6. Scavenger results

In order to find out which factor plays the main role in the degradation of MB by rGO/ Fe₃O₄/CdSe nanocomposites, radical scavenger experiment was performed. For this purpose, the determining active radical in dye degradation was investigated. Hydroxyl (OH⁻), Electrons (e⁻), and holes (h⁺) radicals, are among the radicals that play the main role in degradation processes [7]. Hydrogen peroxide (H₂O₂) and silver nitrate (AgNO₃) were used as electron trap. Ethylenediaminetetraacetic acid (EDTA) was used as a hole trap and sodium iodide (NaI) was used as a hydroxyl species trap [3–27].

The experiment was done in such a way that H₂O₂ was added as an electron trap to the solution containing nanocomposite and MB, and the test was performed according to the previous procedure, the result showed a serious impairment in the degradation process. Then, to ensure the role of electrons in the degradation process, AgNO₃ was tested as another electron trap, which confirmed the role of electrons in the degradation process. Then, EDTA was added to the compound as a hole trap and the experiment was repeated, the result showed that the holes didn't play a role in the degradation of the dye and the degradation process was carried out without any disturbance. Also, to determine the role of hydroxyls, the degradation process was carried out with NaI, which showed that it has no effect on the degradation process [8]. Therefore, according to the results of the scavenger tests, which are shown in Fig. 8, it can be concluded that the main role in MB degradation is the surface electrons produced by rGO/Fe₃O₄/CdSe magnetic nanocomposite. [5–27]. Also, to ensure that the process of degradation has taken place and not absorption. After the degradation process, the nanocomposite was separated from the aqueous media by a magnet. Then after drying at room temperature, it was added to a beaker containing 25 ml of DI water and dispersed by an ultrasonic probe for 30 min, but no dye was observed in the aqueous media. Therefore, considering this case, and the fact that the addition of electron traps caused a disruption in the degradation process, it can be sure that the degradation took place and not absorption.

3.2.7. Degradation process mechanism

The path of dark catalytic degradation of MB by rGO/Fe₃O₄/CdSe nanocomposite was studied. According to the results in Fig. 5b, it can be seen that MB has a characteristic absorption peak at 662 nm. After reaction with rGO/Fe₃O₄/CdSe nanocomposite, this peak is significantly reduced and after 2 min of stirring in the darkness, it disappears completely. In combination with the results of the trap experiments, it was found that the main role in MB degradation is the active species of electron (e⁻). Also, it can be seen from the zeta potential that rGO/Fe₃O₄/CdSe magnetic nanocomposite has the ability to create a large amount of negative charge on its surface, which makes it an ideal option for degradation. Finally, based on all that was studied and discussed above, a catalytic degradation mechanism for MB by rGO/Fe₃O₄/CdSe in the dark was proposed. As shown in Fig. 9. The electrons on the surface of the nanocomposite react with the oxygen in the water and produce superoxide •O₂ radicals. On the other hand, reactive hydroxyl species () can also be created from the reaction of superoxide species by H⁺ ions. Therefore, as a result, the reaction between the radicals created by the electrons on the surface of the nanocomposite with MB removes the dye molecules from the wastewater [27].

Briefly, in this research, Fe₃O₄/CdSe and rGO/Fe₃O₄/CdSe magnetic nanocomposites were synthesized fast and simple by refluxing method. Characteristic spectra of XRD, Raman, FTIR, and SEM showed that Fe₃O₄/CdSe and rGO/Fe₃O₄/CdSe magnetic nanocomposites were successfully synthesized. VSM spectrum showed that the samples have superparamagnetic behavior. Zeta potential spectrum showed that the samples have negative surface charge necessary for degradation and also the surface charge of rGO/Fe₃O₄/CdSe was increased compared to Fe₃O₄/CdSe. The dark degradation ability of prepared magnetic nanocomposites was tested on MB dye. The experiment showed that Fe₃O₄/CdSe magnetic nanocomposite has 55% degradation ability, but by adding graphene to the compound, rGO/Fe₃O₄/CdSe magnetic nanocomposites were able to completely and 100% degrade MB dye within 2 min. Also, the investigation of the effect of pH showed that rGO/Fe₃O₄/CdSe magnetic nanocomposites have excellent performance in neutral and alkaline media. The results of radical scavenger test also showed that electrons play the main role in the degradation of MB organic dye. So, due to excellent performance in the degradation, reducing the duration of degradation time and amount of catalyst weight used, the prepared nanocomposites are economical compared to similar samples.

Funding Declaration:

There was no Funding

CRediT authorship contribution statement

Mehdi Molaei: Supervision, Writing – review & editing.

Tao Fang: Adviser, review & editing,

Afrasiab Salehi Moghanlou: Investigation, Methodology, Writing-original draft, Conceptualization, Data curation and Formal analysis.

Declaration of Competing Interest

The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper.

Data availability

All data will be made available on request.

Ethics Approval Declaration

There was no Ethics Approval

Acknowledgements

The authors wish to thank the University of Vali-e-Asr Rafsanjan (Iran) for the support provided.

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No competing interests reported.

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You are reading this latest preprint version

A new powerful magnetic dark catalyst based on rGO/Fe3O4/CdSe nanocomposite for ultrafast degradation of methylene blue dye

Status:

Journal Publication

Version 1

Abstract

Figures

1. Introduction

2. Experimental

2.1. Materials

2.2. Preparation of CdSe

2.3. Preparation of Fe₃O₄

2.4. Synthesis of CdSe/Fe₃O₄ nanocomposites

2.5. Preparation of GO

2.6. Preparation of rGO /Fe₃O₄

2.7. Synthesis of rGO /Fe₃O₄/CdSe magnetic nanocomposites

2.8. Dark catalyst study

3. Results and discussions

3.1. Studying the structural characteristics and morphology

3.1.1. XRD pattern

3.1.2. VSM analysis

3.1.3. FTIR spectrums

3.1.4. Raman spectrums

3.1.5. FESEM and EDS analyses

3.2. Dye degradation study

3.2.1. MB degradation

3.2.2. Study effect of rGO/Fe₃O₄/CdSe catalyst mass

3.2.3. Study reusability of rGO/Fe₃O₄/CdSe

3.2.4. Study of pH effect on degradation

3.2.5. Zeta potential analysis

3.2.6. Scavenger results

3.2.7. Degradation process mechanism

4. Conclusion

Declarations

References

Additional Declarations

Status:

Journal Publication

Version 1

A new powerful magnetic dark catalyst based on rGO/Fe3O4/CdSe nanocomposite for ultrafast degradation of methylene blue dye

Status:

Journal Publication

Version 1

Abstract

Figures

1. Introduction

2. Experimental

2.1. Materials

2.2. Preparation of CdSe

2.3. Preparation of Fe3O4

2.4. Synthesis of CdSe/Fe3O4 nanocomposites

2.5. Preparation of GO

2.6. Preparation of rGO /Fe3O4

2.7. Synthesis of rGO /Fe3O4/CdSe magnetic nanocomposites

2.8. Dark catalyst study

3. Results and discussions

3.1. Studying the structural characteristics and morphology

3.1.1. XRD pattern

3.1.2. VSM analysis

3.1.3. FTIR spectrums

3.1.4. Raman spectrums

3.1.5. FESEM and EDS analyses

3.2. Dye degradation study

3.2.1. MB degradation

3.2.2. Study effect of rGO/Fe3O4/CdSe catalyst mass

3.2.3. Study reusability of rGO/Fe3O4/CdSe

3.2.4. Study of pH effect on degradation

3.2.5. Zeta potential analysis

3.2.6. Scavenger results

3.2.7. Degradation process mechanism

4. Conclusion

Declarations

References

Additional Declarations

Status:

Journal Publication

Version 1

2.3. Preparation of Fe₃O₄

2.4. Synthesis of CdSe/Fe₃O₄ nanocomposites

2.6. Preparation of rGO /Fe₃O₄

2.7. Synthesis of rGO /Fe₃O₄/CdSe magnetic nanocomposites

3.2.2. Study effect of rGO/Fe₃O₄/CdSe catalyst mass

3.2.3. Study reusability of rGO/Fe₃O₄/CdSe