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Fabrication of magnetically separable Ag–ZnFe2O4 hollow nanospheres with efficient photocatalytic activity

  • Zhenxing Liu ORCID logo EMAIL logo
Published/Copyright: March 5, 2024
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International Journal of Materials Research
From the journal International Journal of Materials Research Volume 115 Issue 4

Abstract

Environmental pollution seriously affects the survival of human beings. Semiconductor photocatalysis technology is considered to be one of the most effective ways to solve environmental pollution and energy shortage. The high degradation efficiency of nanometric photocatalysts has attracted extensive attention, but the photocatalysts are difficult to recycle and reuse, which limits their application. ZnFe2O4 hollow nano-photocatalysts loaded with different contents of Ag were successfully prepared by template-assisted calcination and photoreduction, and can be conveniently separated from water in a magnetic environment. The results indicate that Ag–ZnFe2O4 possess a hollow nano-shell structure with a particle size distribution of about 280 nm and a shell thickness of about 24 nm. Ag–ZnFe2O4 shows the strongest photocurrent intensity and photocatalytic performance compared to bulk ZnFe2O4 and nano ZnFe2O4. When the concentration of AgNO3 solution is 0.2 mmol, Ag–ZnFe2O4 has the strongest photodegradation efficiency to degrade RhB under visible light irradiation. After several photodegradation experiments, the photodegradation efficiency is only decreased by 2.8 %, further proving that Ag–ZnFe2O4 possess good application value in wastewater treatment.

Keywords: Ag–ZnFe2O4; Photocatalysis; Magnetic recovery; Nanometric materials

1 Introduction

The increase in the global population demands rapid growth of industrialization and urbanization, which in turn act to increase the level of environmental pollution [1]. In recent years, ZnFe2O4 has attracted widespread attention in the field of waste water treatment, because of its narrow band gap, strong photocatalytic properties, excellent magnetic properties, outstanding stable chemical properties, as well as low cost, and so has great research potential [2], [3], [4]. However, the application of ZnFe2O4 is limited due to its high photogenerated electron hole recombination rate. In order to overcome this limitation, there are many approaches to optimize the quantum efficiency of photocatalysts, such as nanostructuring [5, 6], doping with metal ions [7], constructing heterojunctions [8], loading with precious metals [9, 10], etc. Among these methods, Ag-loaded ZnFe2O4 can form a Schottky junction at the interface between semiconductor and metal to inhibit photogenerated carrier recombination [11], which is very promising to improve the photocatalysis efficiency. Moreover, the nanometer size of the photocatalyst is also one of the most important means to improve the photodegradation efficiency, and many forms of ZnFe2O4 with nanostructure have been successfully synthesized by different processes, such as nanoparticles [12], nanowires [13, 14] and nanospheres [15]. To our best knowledge, the preparation of Ag–ZnFe2O4 hollow nanospheres by template is rarely studied.

In this study, ZnFe2O4 hollow nano-photocatalyst with magnetically separable properties was prepared. Then, the samples were studied by X-ray powder diffraction (XRD), scanning electronic microscopy (SEM), transmission electron microscopy (TEM), photocurrent density test, degradation of RhB, magnetic recycling, and radical trapping experiments. Furthermore, the mechanism of improving the photocatalytic performance of samples by Ag-loading was studied.

2 Experimental

2.1 Preparation of sample

2.1.1 Preparation of phenolic formaldehyde microspheres (PFS)

PFS were synthesized by using resorcinol and formaldehyde solution as precursors [16]. Ammonia aqueous solution (NH4OH, 0.1 mL, 25 wt.%) was mixed with a solution containing absolute ethanol (EtOH, 8 mL) and deionized water (H2O, 20 mL), then stirred for more than 1 h. Subsequently, resorcinol (0.2 g) was added and continually stirred for 30 min. The formaldehyde solution (0.28 mL) was then added to the reaction solution and stirred for 12 h at 30 °C, and subsequently heated for 24 h at 100 °C under a static condition in a Teflon-lined autoclave. The solid product was recovered by centrifugation and air-dried at 100 °C for 48 h.

2.1.2 Preparation of ZnFe2O4 hollow nanospheres

ZnFe2O4 hollow nanospheres were synthesized via a template-assisted calcination. Put 20 mL of the mixture with 2 mg L−1 Fe(NO3)3 and 0.1 mg L−1 Zn(NO3)2 into a 100 mL beaker and stir strongly to dissolve forming a transparent solution. 0.5 g of the as-prepared PFS was added to the above mixture solution and dispersed evenly with ultrasonic treatment. After ultrasonic treatment for 15 min, then aged for 3 h, filtered, washed and dried at 80 °C for 48 h. The PFS adsorbed metal ions were heated to 700 °C at a warming rate of 0.5 K min−1, then held for 3 h, cooled naturally to room temperature. The preparation method of bulk ZnFe2O4 is the same as that of nano ZnFe2O4, except that no PFS is added, and then crush it with a mortar.

2.1.3 Preparation of Ag–ZnFe2O4 hollow nanospheres

Ag–ZnFe2O4 was prepared by the process of photoreduction. Under dark conditions, 0.5 g ZnFe2O4 was added to 50 mL AgNO3 solution, followed by irradiation under a 500 W xenon lamp for 0.5 h, accompanied by magnetic agitation. Then filtered, washed, and dried at 80 °C for 48 h. Finally, Ag–ZnFe2O4 powders were obtained. When the amount of AgNO3 was added with 0.1 mmol, 0.15 mmol, 0.2 mmol and 0.25 mmol, corresponding Ag–ZnFe2O4 were denoted as AZ-1, AZ-2, AZ-3 and AZ-4.

2.2 Characterization

The crystal phase and crystallinity of the photocatalyst samples were characterized by X-ray diffractometry (D/max2200pc, Japan). Scanning electron microscopy (S-4800, Japan) was used to observe the morphology of the prepared samples. The structure of the samples was observed by transmission electron tunneling microscopy (JEM-3010, Japan).

2.3 Determination of photocatalytic and photoelectric properties

2.3.1 Determination of photocatalytic properties

In this study, rhodamine B (RhB) was used as the standard pollutant for degradation, and different photocatalysts was characterized by the degradation of RhB solution under 500 W xenon lamp irradiation.

The detailed experimental process is as follows. 300 mL RhB solution with a concentration of 10 mg L−1 was prepared. 20 mL as-prepared RhB solution and 20 mg photocatalyst were added to each quartz tube and stirred for 30 min under dark conditions to ensure that the RhB solution and photocatalyst reached the adsorption–desorption balance. Subsequently the mixture was then magnetically stirred and irradiated with a 500 W xenon lamp. After every 30 min interval, a quartz tube was taken out and the photocatalyst in the solution was removed by centrifugation. The content of RhB in the solution was detected by UV–vis spectrometry.

2.3.2 Determination of photoelectrochemical properties

The samples were used as the working electrode [17, 18]. Ag/AgCl (3 M, KCl) was used as the reference electrode, and platinum wire was used as the counter electrode. 1 M NaOH solution was used as the electrolyte solution and 300 W xenon lamp was used as the excitation light source.

2.3.3 Cyclic photocatalytic experiments

Five cyclic photocatalytic experiments were conducted: After the first photocatalytic reaction, the photocatalyst obtained after sampling and centrifugation was collected together with the remaining catalysts in the reactor. Then the samples were washed three times in anhydrous ethanol and deionized water, and dried at 80 °C for 6 h. Subsequently, four more cyclic photocatalytic experiments were carried out under the same experimental conditions.

3 Results and discussion

3.1 XRD analysis

The XRD pattern of ZnFe2O4 based photocatalysts are presented in Figure 1. It can be clearly seen that there are diffraction peaks at 18.16°, 29.96°, 35.34°, 42.86°, 53.26°, 56.7° and 62.34° in curves a and b, which are indexed to the (111), (220), (311), (400), (422), (511), and (440) face-centered cubic structure of ZnFe2O4 (JCPDS No. 77-0011), respectively. In curve b, the peaks at 38.02°, 44.24° and 64.62° are in good agreement with (111), (200) and (222) crystal planes of Ag (JCPDS No. 04-0783). Therefore, the material of b is Ag–ZnFe2O4. In addition, no other miscellaneous peaks were found in Figure 1, and the diffraction peak was sharp and had high intensity, indicating that the prepared sample had high purity and good crystallinity.

Figure 1: XRD patterns of ZnFe2O4 based photocatalyst: (a) ZnFe2O4, (b) Ag–ZnFe2O4.
Figure 1:

XRD patterns of ZnFe2O4 based photocatalyst: (a) ZnFe2O4, (b) Ag–ZnFe2O4.

3.2 Morphology analysis

It is universally acknowledged that the structure of a photocatalyst has great influence on the performance of photodegradation of pollutants. As shown in Figure 2a, the narrow size distribution of PFS is demonstrated by SEM, which verifies that PFS possess a mean diameter of 510 nm and smooth surface. In Figure 2a, it is easy to think that PFS have a narrow particle size distribution and uniform size, which is conducive to the construction of ZnFe2O4 hollow nano-shell structure in the next step. The SEM image of Ag–ZnFe2O4 in Figure 2b clearly shows spherical morphology and narrow size distribution. The particle size distribution of Ag–ZnFe2O4 is about 280 nm. Meanwhile, we find that the surface of the sample is rough, which can increase the absorption of sunlight. Figure 2c is a TEM image of Ag–ZnFe2O4. It can be clearly seen that the edge of the sample is darker and the inner region is lighter, and the thickness of the shell is about 24 nm, which fully indicates that the prepared sample has a hollow nano-structure. Moreover, TEM shows that there are a large number of small white areas in the spherical shell, indicating that there are many holes in the shell. This phenomenon is attributed to the thin thickness, and the sunlight can easily pass through the surface of the spherical shell.

Figure 2: SEM and TEM of samples: (a) SEM of PFS, (b) SEM of Ag–ZnFe2O4, and (c) TEM of Ag–ZnFe2O4.
Figure 2:

SEM and TEM of samples: (a) SEM of PFS, (b) SEM of Ag–ZnFe2O4, and (c) TEM of Ag–ZnFe2O4.

Figure 2 shows that the sample has a hollow nanostructure, and thin shell, indicating that the large specific surface area of the sample is conducive to the absorption of sunlight and increases the contact frequency with pollutants, which will greatly promote the performance of photocatalytic degradation of pollutants by the sample.

3.3 Formation mechanism of ZnFe2O4 hollow nano shell-structure

PFS is a polymer compound with a large number of active functional groups on the surface, such as C–OH, C=H, C=C and C–H, and has strong adsorption capacity for ions. As can be seen from Figure 3, when PFS is immersed in a mixed solution of zinc salt and iron salt, the functional groups on the surface of PFS will strongly adsorb Zn2+ and Fe3+. With slow calcination in an aerobic environment, PFS adsorbed ions on the surface, shrank and carbonized, and the Zn2+ and Fe3+ particles adsorbed on the surface of PFS were solidified and compacted. Zn2+ and Fe3+ react to form ZnFe2O4 with the increase of temperature, and the carbonized PFS will eventually oxidize into CO2 and H2O. In the end, the hollow nanostructure of ZnFe2O4 can be formed, and the thickness of the shell can be controlled by adjusting the amount of PFS, sintering temperature and sintering rate.

Figure 3: Formation mechanism of ZnFe2O4 hollow nano shell-structure.
Figure 3:

Formation mechanism of ZnFe2O4 hollow nano shell-structure.

3.4 Transient photocurrent–time performance of the catalysts

The photoelectric conversion efficiency of a photocatalyst plays a crucial role in the degradation of pollutants. The higher the photoelectric conversion efficiency, the higher the photocurrent intensity, which will be more beneficial to the degradation of pollutants. In order to investigate the photocurrent response of the photocatalyst under visible light, Figure 4 shows the photocurrent response curve of ZnFe2O4 based photocatalyst under a 300 W xenon lamp light source. As can be seen from the curves in the figure, the photocurrent densities of bulk ZnFe2O4, ZnFe2O4, AZ-1, AZ-2, AZ-3, and AZ-4 are 0.4 μA cm−2, 1.2 μA cm−2, 4.9 μA cm−2, 6.4 μA cm−2, 7.3 μA cm−2 and 8.1 μA cm−2 respectively. The photocurrent density of Ag–ZnFe2O4 is higher than that of bulk ZnFe2O4 and ZnFe2O4, which further proves that Ag loaded ZnFe2O4 is beneficial to improve the photoconversion efficiency of photocatalysts.

Figure 4: Photocurrent response curves of ZnFe2O4 based photocatalysts: (a) bulk ZnFe2O4, (b) ZnFe2O4, (c) AZ-1, (d) AZ-2, (e) AZ-3, and (f) AZ-4.
Figure 4:

Photocurrent response curves of ZnFe2O4 based photocatalysts: (a) bulk ZnFe2O4, (b) ZnFe2O4, (c) AZ-1, (d) AZ-2, (e) AZ-3, and (f) AZ-4.

In order to investigate the effect of Ag modified content on the Ag–ZnFe2O4 composite system, with the increase of Ag loading, the photocurrent intensity of AZ-1, AZ-2, AZ-3 and AZ-4 samples first increased and then decreased. When the concentration of AgNO3 solution was 0.2 mmol, the photocurrent intensity of the complex was the highest, indicating that appropriate Ag loaded ZnFe2O4 was conducive to improving the photoelectric conversion efficiency. Since Ag is loaded on the surface of ZnFe2O4, it facilitates electron transfer from ZnFe2O4 to Ag and reduces electron–hole pair recombination. However, with the high Ag loading, the absorption of visible light by ZnFe2O4 is reduced, the recombination rate of electron–hole pairs is increased, the effective photogenerated electron density is reduced, and the photodegradation efficiency is further decreased. The higher photocatalytic activity of Ag–ZnFe2O4 may be attributed to the presence of plasmonic metallic Ag [19]. Modification of ZnFe2O4 with silver nanoparticles having surface plasmon resonance characteristics is a potential candidate for enhanced solar light harvesting as well as effective charge transfer.

3.5 Photocatalytic performance test

Figure 5 shows the experimental data of degradation of RhB solution by ZnFe2O4 based photocatalyst under visible light irradiation. After 30 min of dark treatment, bulk ZnFe2O4, ZnFe2O4, AZ-1, AZ-2, AZ-3, and AZ-4 all reached adsorption–desorption equilibrium. The adsorption rate of RhB solution for the bulk ZnFe2O4 was about 4 %, however ZnFe2O4 based hollow nano-photocatalysts were about 17 %, indicating that the hollow nano-samples prepared by this process have a large specific surface area, which is beneficial to the photocatalytic reaction. After all samples were irradiated with the 500 W xenon lamp for 180 min, respectively, the degradation rates of RhB solution in blank experiment were almost 0, and the degradation rate of RhB solution by bulk ZnFe2O4, nano ZnFe2O4 were almost 12 % and 39 %, while the degradation rates of RhB solution by AZ-1, AZ-2, AZ-3, and AZ-4 can reach 79 %, 86 %, 97 % and 91 %, respectively. We can clearly see in Figure 5, as the silver loaded increases, the photocurrent intensity and photocatalytic activity of AZ-1, AZ-2, AZ-3 and AZ-4 corresponding samples first increased and then decreased. When the concentration of AgNO3 solution was 0.2 mmol, Ag–ZnFe2O4 has the strongest photodegradation efficiency.

Figure 5: Photodegradation curve of ZnFe2O4 based photocatalysts: (a) blank, (b) bulk ZnFe2O4, (c) ZnFe2O4, (d) AZ-1, (e) AZ-2, (f) AZ-3, and (g) AZ-4.
Figure 5:

Photodegradation curve of ZnFe2O4 based photocatalysts: (a) blank, (b) bulk ZnFe2O4, (c) ZnFe2O4, (d) AZ-1, (e) AZ-2, (f) AZ-3, and (g) AZ-4.

3.6 Stability and recovery test

Photocatalyst can only be used for some cycles to degrade pollutants and maintain stable catalytic performance. Figure 6a shows the cyclic degradation of RhB solution by Ag–ZnFe2O4 photocatalyst. It can be seen that after five cyclic photodegradation experiments, the catalytic performance of Ag–ZnFe2O4 is only decreased by 2.8 %, which further proves that the physical and chemical properties of Ag–ZnFe2O4 are stable. Figure 6b shows the Ag–ZnFe2O4 magnetic separation and recovery experiment. A is a picture of Ag–ZnFe2O4 uniformly dispersed into water, B is a picture of A gathering under magnetic force, which proves that the photocatalyst of Ag–ZnFe2O4 is easy to recover in a magnetic environment. Figures 5 and 6 further demonstrate the practicability of Ag–ZnFe2O4.

Figure 6: (a) Stability experiments of Ag–ZnFe2O4, and (b) recovery test experiments: (A) Ag–ZnFe2O4 uniformly dispersed into water, (B) Ag–ZnFe2O4 gathering under magnetic force.
Figure 6:

(a) Stability experiments of Ag–ZnFe2O4, and (b) recovery test experiments: (A) Ag–ZnFe2O4 uniformly dispersed into water, (B) Ag–ZnFe2O4 gathering under magnetic force.

3.7 Photocatalytic mechanism analysis

As shown in Figure 7a, the active species experiment was conducted to decompose RhB by Ag–ZnFe2O4; p-benzoquinone (BQ), isopropanol (IPA), ammonium oxalate (AO) were applied for •O2−, •OH, h+ scavenging, respectively. After 180 min of excitation by visible light, the photodegradation efficiency in the presence of AO was 62 %, with IPA to 54 %, and with BQ to 32 %. As observed, ·O2− was the key active species in the catalytic reaction, and ·OH and h+ also played a role to some extent.

Figure 7: Ag–ZnFe2O4: (a) radical trapping experiments, and (b) photodegradation mechanism.
Figure 7:

Ag–ZnFe2O4: (a) radical trapping experiments, and (b) photodegradation mechanism.

Based on the above test data and outcome analysis, a possible photocatalytic mechanism of Ag–ZnFe2O4 hollow nano-photocatalysts is shown in Figure 7b. It can be attributed to the Schottky barrier. When Ag is loaded on ZnFe2O4, the electron migration mode at the interface between ZnFe2O4 and Ag will change. The work function of Ag is larger than that of ZnFe2O4, thus the minimum energy needed for electrons to move from the interior of Ag to the surface is more than that of ZnFe2O4. When ZnFe2O4 and Ag are in contact, electrons migrate from ZnFe2O4 to Ag until their Fermi energy levels are equal. As a result of electron migration, Ag gains excessive negative charge and ZnFe2O4 gains excessive holes, forming a Schottky barrier at the interface. Hence, O2 receives electron on the surface of Ag nanoparticles and reduced to O2−. Since the potential of OH−/·OH (+1.99 V vs. NHE) and H2O/·OH (+2.38 V vs. NHE) was more positive than the VB potential of ZnFe2O4 (+1.65 V vs. NHE), the photo-generated holes (h+) couldn’t oxidize OH− and H2O to ·OH directly [20, 21]. Moreover, Ag nanoparticles can give rise to surface plasmonic resonance effects (SPR) under visible light excitation, which also can enhance the photodegradation efficiency of Ag–ZnFe2O4 [22, 23].

4 Conclusions

In this study, Ag–ZnFe2O4 hollow nanospheres loaded with different cotent of Ag were successfully prepared by a template-assisted calcination and photoreduction process. The samples have a hollow nano shell-structure with a particle size distribution of about 280 nm and a shell thickness of about 24 nm, which can increase the absorption of sunlight and the frequency of contact with pollutants. The results of the photocurrent density and photocatalytic activity of rhodamine B under visible light irradiation reveal the sequence: Ag–ZnFe2O4 > ZnFe2O4 > bulk ZnFe2O4. As the silver loading increases, the photocurrent intensity and photocatalytic activity of AZ-1, AZ-2, AZ-3 and AZ-4 first increases, and then decreases. When the concentration of AgNO3 solution was 0.2 mmol, Ag–ZnFe2O4 had the strongest photodegradation efficiency. Ag–ZnFe2O4 can be conveniently separated from water in a magnetic environment. After several photodegradation experiments, the photodegradation efficiency was only decreased by 2.8 %, further proving that Ag–ZnFe2O4 possess good application value in wastewater treatment.

Corresponding author: Zhenxing Liu, School of Chemical Engineering, Shaanxi Institute of Technology, Xi’an 710300, P.R. China, E-mail:

  1. Research ethics: All procedures performed in studies involving human participants were in accordance with the ethical standards of the institutional research committee.

  2. Author contributions: Zhenxing Liu completed all the work of the study. The author has accepted responsibilityfor the entire content of this manuscript and approved its submission.

  3. Competing interest: The author states no conflict of interest.

  4. Research funding: We are grateful for the financial support of the natural Science Program of the Shaanxi Institute of Technology (grant No. Gfy2024).

  5. Data availability: The data that support the findings of this study are available from the corresponding author upon reasonable request.

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Received: 2022-11-10
Accepted: 2024-02-08
Published Online: 2024-03-05
Published in Print: 2024-04-25

© 2024 Walter de Gruyter GmbH, Berlin/Boston

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  11. DGM – Deutsche Gesellschaft für Materialkunde
https://doi.org/10.1515/ijmr-2022-0459
Keywords for this article
Ag–ZnFe2O4; Photocatalysis; Magnetic recovery; Nanometric materials

Articles in the same Issue

  1. Frontmatter
  2. Original Papers
  3. Fabrication of magnetically separable Ag–ZnFe2O4 hollow nanospheres with efficient photocatalytic activity
  4. Optimization of magnetic properties of MnFe2O4 by modulating molarity of NaOH as precipitating agent
  5. Effect of synthesis method on structural and magnetic properties of La0.7Ca0.2Ba0.1MnO3
  6. Exploring the functional abilities of PVA–combeite composites as potential candidates for bone substitutes
  7. Study of optical, structural and radiation shielding properties of (55 − x)TeO2–20ZnO–25B2O3–xEr2O3 glass matrix
  8. Effect of post-weld heat treatment on corrosion resistance of X90 pipeline steel joints
  9. Microstructure and residual stress distribution of electron beam-welded joints of a 50 mm-thick TA15 titanium alloy plate
  10. News
  11. DGM – Deutsche Gesellschaft für Materialkunde
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