Recepción: 22 Julio 2021
Aprobación: 01 Septiembre 2021
Publicación: 11 Abril 2022
DOI: https://doi.org/10.26850/1678-4618eqj.v47.1SI.2022.p20-27
Abstract: In this work, the W-doped Ag3PO4 was prepared by the chemical coprecipitation method and irradiated with a femtosecond laser (FL). The successful formation of the Ag/Ag3PO4:W heterostructure was confirmed by XRD analysis. A higher structural disorder in the [PO4] clusters was observed for the FL irradiated sample (Ag3PO4:W-FL), indicating the formation of Ag metallic from the Ag3PO4 structure. The photocatalytic activity of the samples was studied by photodegradation of rhodamine B under visible light irradiation. The formation of Ag nanoparticles on the surface of Ag3PO4:W led to a degradation rate constant 3.54 times higher than the nonirradiated sample. This higher photocatalytic activity was related to the surface plasmon resonance effect of the Ag metallic, which acts by capturing photoexcited electrons from the Ag3PO4:W, avoiding the recombination of electron-hole pairs, and thus improving the photocatalytic activity.
Keywords: Ag3PO4, doping, heterostructure, photocatalytic property.
1. Introduction
Water sources contain various types of contaminants (Sousa et al., 2018), with industrial waste being the contaminants that draw the major attention in environmental pollution, thus requiring a suitable treatment (Karimi-Maleh et al., 2020). Among industrial wastes, organic dyes are the main concern due to their high generated content and toxicity, being of fundamental importance the proper treatment. Rhodamine B (RhB) is an organic dye that can cause damage to humans, leading to skin and eye irritations and respiratory problems (Aljerf, 2018; Dong et al., 2010). Several treatment methods have been studied, such as heterogeneous photocatalysis, which has been considered promising for the treatment of organic dyes because of its green and clean aspects, simplicity and low cost (Zangeneh et al., 2015). Silver phosphate (Ag3PO4) has been receiving attention from researchers since its discovery for presenting photocatalytic properties such as the extremely high photooxidative capacity for the evolution of O2 from water and the decomposition of efficient organic dyes using sunlight (Chen et al., 2015; He et al., 2019; Trench et al., 2018; Zwara et al., 2018). Furthermore, Ag3PO4 presents advantages in relation to other well-known photocatalysts, such as TiO2, due to its ability to absorb light in the visible region (Fujishima and Honda, 1972). However, Ag3PO4 has the disadvantage of photocorrosion and fast recombination of electron-hole pairs, decreasing its stability as a photocatalyst, making its use unfeasible (Chen et al., 2015). Therefore, studies that aim to modify to improve the Ag3PO4 photocatalytic activity are of great interest (R. Santos et al., 2020; Shaveisi and Sharafnia, 2020; Shi et al., 2019).
Among the modification methods, the doping process was applied to overcome these disadvantages of Ag3PO4. Our research group has showed a significant improvement of the photocatalytic performance of Mo- and W-doped Ag3PO4 (Trench et al., 2018; 2020), while very recently ultra-active Ag3PO4 with different W doping rates were successfully synthesized by Trench et al., 2020. Moreover, the deposition of noble nanoparticles, such as Ag, Au, Pt and Pd, onto the surface of Ag3PO4 is an important approach to produce a metal semiconductor composite with enhanced photocatalytic performance (Y. Liu et al., 2012; Yan et al., 2014; Z. Liu et al., 2017). This behavior mainly stems from the surface plasmon resonance (SPR) effect of metal nanoparticles, which are related to the collective oscillations of free electrons that can lead to improved visible light absorption, the superior separation of electron-hole pairs in the composite material, and by the inhibition of photocorrosion mechanisms due to the accumulation of electrons in the Ag nanoparticles instead of Ag3PO4 surface (Li et al., 2019).
The decoration of semiconductors with metal nanoparticles is mainly conducted by the adsorption of metal precursors on their surface followed by the chemical reduction in solution (Kochuveedu et al., 2013). Alternatively, the femtosecond laser (FL) irradiation is attracting attention as a cost-effective, fast and clean method for the fabrication of metal-semiconductor heterostructure in which the requirement of organic solvents or chemical reducing agents are minimized (Tan et al., 2013; Vorobyev and Guo, 2013). The short pulses of the laser can induce the nanoparticles formation from distinct bulk targets, as the migration of Ag atoms to the surface of complex oxides followed by their reduction into metallic species (Machado et al., 2018). Our research group reported the formation of Ag nanoparticles on α-Ag2WO4 with superior bactericidal activity (Assis et al., 2018), the laser-induced formation of Ag/Cr particles on AgCrO4 (Lemos et al., 2019), and the synthesis of Ag−Bi nanoalloys from Ag2WO4 and NaBiO3 targets (Machado et al., 2018). In special, we reported the nucleation and growth of Ag nanoparticles on Ag3PO4 surface mediated by FL irradiation (C. Santos et al., 2019). As a step forward, in the present study we demonstrate the formation of Ag/Ag3PO4:W heterostructure by FL irradiation and its superior photocatalytic activity in compare to Ag4PO3:W, as evidenced by RhB visible light-driven photodegradation process.
2. Materials and methods
2.1 Synthesis of Ag3PO4:W and preparation of Ag3PO4:W-FL samples
The Ag3PO4:W sample was synthesized using the coprecipitation method and doped with 1% mol Na2WO4·2H2O, as previously reported by Trench et al. (2020).
Ag3PO4:W was irradiated with a Ti:sapphire laser (Femtopower Compact Pro, Femto Lasers) using 30 fs full width at half maximum (FWHM) pulses at the central wavelength of 800 nm, and a repetition rate of 1 kHz. A laser beam of 6 mm diameter and mean power of 185 mW was focused onto the surface of Ag3PO4:W with a 75 mm lens. To obtain the Ag3PO4:W-FL heterostructure, the Ag3PO4:W was placed at the bottom of a quartz cuvette attached to a two-dimensional motion-controlled stage moving in a raster scanning at a constant speed of 0.5 mm s–1 in the focus plane perpendicular to the laser beam.
2.2 Characterization techniques
The structural features at long-range of the samples were investigated by X-ray diffraction (XRD) performed in a D/Max-2500PC diffractometer (Rigaku, Japan) using Cu Kα radiation (λ = 1.54056 Å), at a scan rate of 0.5° min–1. The structural features at short-range of the samples were investigated by micro-Raman scattering spectroscopy measurements performed in a LabRAM iHR550 Horiba Jobin Yvon spectrometer coupled with a charge-coupled device (CCD, Synapse) as a signal detector, and an ion argon laser with 514.5 nm of wavelength (Melles Griot). The optical absorption spectroscopy measurements in the ultraviolet and visible region were performed in the diffuse reflectance mode in a Varian spectrophotometer model Cary 5G (USA) in the range of 250–800 nm. Field emission scanning electron microscopy (FE-SEM) was performed using a FEI microscope (Model Inspect F50) operating at 5 kV.
2.3 Photocatalytic experiments
The photocatalytic activity of Ag3PO4:W and Ag3PO4:W-FL samples were tested for degradation of RhB (95%, Aldrich) under visible light irradiation. For this experiment, 50 mg of each sample and 50 mL of RhB (10 mg L–1) were used, which were submitted to an ultrasonic bath (Branson, model 1510; frequency 42 kHz) for 5 min and 30 min of constant agitation, in order to reach the adsorption-desorption balance and later exposed to irradiation of six lamps (Philips TL-D, 15 W). Aliquots were taken at 1 min intervals, centrifuged and their degradation monitored by measuring the peak of maximum RhB absorption (λmax = 554 nm) using an ultraviolet-visible (UV-Vis) spectrophotometer (V-660, JASCO). A test under the same conditions without the presence of catalysts was also carried out.
3. Results and discussion
Figure 1a shows the XRD patterns of Ag3PO4:W and Ag3PO4:W-FL samples. The diffraction peaks for both samples indicated the cubic phase of Ag3PO4 with P-43n space group, according to the Inorganic Crystal Structure Database (ICSD) code 14000 (Masse et al., 1976). No secondary or any dopant related phases were observed for Ag3PO4:W sample, indicating the successfully of insertion of W as dopant into the Ag3PO4 structure. However, for the sample irradiated with the FL, it was observed the emergence of a peak at approximately 37.8° (2θ), as can be seen in Fig. 1b. The as-mentioned peak is assigned to the (111) diffraction plane of cubic phase of Ag with Fm-3m space group, which is the most intense diffraction peak for this structure, according to the ICSD code 604630 (Jette and Foote, 1935). It is well-known that the FL irradiation in Ag-containing materials, such as Ag3PO4, induces the reduction of Ag+ cations in the structure for the formation of Ag nanoparticles on the semiconductor surface (Assis et al., 2018; 2019; C. Santos et al., 2019). Herewith, the FL irradiation effectively allowed the formation of Ag/Ag3PO4:W heterostructure in the Ag3PO4:W-FL samples.
Figure 1.
XRD patterns of Ag3PO4:W and Ag3PO4:W-FL samples in the range of 10–100° (a) and in the range of 33–50° (b).
Figure 2 shows the Raman spectra of Ag3PO4:W and Ag3PO4:W-FL samples. According to the group theory analysis, the cubic phase of Ag3PO4 structure presents 18 Raman active modes (Γ = 2 A1 + 4 E + 12 T2) (Trench et al., 2018; Botelho et al., 2015). The observed Raman bands for the prepared samples are located at approximately 100, 237, 539, 700, 904, and 997 cm–1. All these modes are related to the cubic phase of Ag3PO4 and no Raman bands related to any secondary or W dopant phases were observed. The bands located at 100 and 237 cm–1 have been assigned to the translational and/or rotational modes with T2 symmetry of [PO4] clusters. The band located at 539 cm–1 is assigned to the bending mode with T2 symmetry of [PO4] clusters. The band located at 700 cm–1 is attributed to the symmetric stretching mode of the [PO4] clusters. The most intense band located at 904 cm–1 is related to the symmetric stretching (A1) mode, whereas the band located at 997 cm–1 is related to the asymmetric stretching mode (T2) mode of [PO4] clusters.
Figure 2.
Raman spectra of Ag3PO4:W and Ag3PO4:W-FL samples.
It can be observed that the Ag3PO4:W-FL sample presented a remarkable decrease of the relative intensity of the band at 904 cm–1 compared to the Ag3PO4:W sample. As observed in XRD results, the FL irradiation in Ag3PO4:W sample induced the formation of metallic Ag that arises from the reduction of Ag+ cations in the Ag3PO4 structure. This process generates Ag vacancies in the structure, which induce a local structural rearrangement of the adjacent [PO4] clusters. This rearrangement causes variations in the coordination parameters of the clusters, i.e., bond angles and lengths, thus increasing the structural disorder in the [PO4] clusters. The structural disorder in the clusters leads to a break of local symmetry that decreases the freedom degree of vibrational modes the [PO4] clusters, hence decreasing the intensity of Raman scattering.
UV-Vis diffuse reflectance measurements were employed to determine the optical band gap energies of the prepared samples. Considering that the absorption spectrum of the Ag3PO4 is governed by indirect electronic transitions (Botelho et al., 2016), Fig. 3a and b show the Tauc plot (Wood and Tauc, 1972) for the Ag3PO4:W and Ag3PO4:W-FL samples, respectively. It can be observed a slight decrease in the band gap energy for the Ag3PO4:W-FL compared to the Ag3PO4:W sample, being the values of 2.53 and 2.43 eV, respectively. As previous mentioned in Raman analysis, the FL irradiation in the Ag3PO4:W sample induced structural disorder in the [PO4] clusters due to the formation of Ag vacancies in the Ag3PO4 structure. These structural distortions induce the formation of intermediate energy levels within the band gap, which can act as electron traps, thus decreasing the band gap energy of the FL irradiated sample.
Figure 3.
Tauc plot for the Ag3PO4:W (a) and Ag3PO4:W-FL (b) samples.
The morphological aspects of the Ag3PO4:W and Ag3PO4:W-FL samples were investigated by FE-SEM analysis. Figure 4a and b shows the FE-SEM images of the Ag3PO4:W and Ag3PO4:W-FL samples, respectively, with their corresponding insets with magnified regions of the images. For the Ag3PO4:W sample, it can be observed nano- and microparticles with quasi-spherical shape. These morphologies are similar to those previously reported (Trench et al., 2018; 2020). However, the FE-SEM image of the Ag3PO4:W-FL sample presents smaller and agglomerated particles compared to the Ag3PO4:W sample. These aspects arise from the high local energy of the pulsed FL in the sample, thus inducing the fragmentation and coalescence of the particles. Moreover, according to reported works (Assis et al., 2018; C. Santos et al., 2019) and the XRD results, the presence of nanoparticles on the surface of larger particles can be assigned to the Ag metallic nanoparticles.
Figure 4.
FE-SEM images of Ag3PO4:W (a) and Ag3PO4:W-FL (b) samples.
The photocatalytic activity of the Ag3PO4:W and Ag3PO4:W-FL samples were investigated by the degradation of RhB under visible light irradiation. Figure 5a shows the degradation efficiency of both prepared samples and the control experiment without photocatalyst. As can be seen, no significant degradation was observed in the absence of photocatalyst. As previously reported, the Ag3PO4:W sample presents a highly photocatalytic activity for RhB degradation under visible light irradiation, allowing approximately 82.5% of RhB degradation in only 3 min of reaction (Trench et al., 2020). However, it was observed a remarkable improvement of the photocatalytic activity of the FL irradiated sample, allowing 100% of RhB degradation in 3 min of reaction. To further compare, the Ag3PO4:W and Ag3PO4:W-FL samples promoted 60.5% and 97.2% of RhB in only 2 min of reaction. Figure 5b shows the Langmuir-Hinshelwood plot for the pseudo first-order kinetics model (B. Liu et al., 2014) for both prepared samples and the control experiment. It was observed that the Ag3PO4:W-FL sample presented a rate constant (k) 3.54 times higher than the Ag3PO4:W sample.
Figure 5.
Relative concentration of RhB against reaction time in photocatalytic experiments (a) and pseudo first-order kinetics plot (b) of Ag3PO4:W and Ag3PO4:W-FL samples.
It has been demonstrated that the FL irradiation in Ag-containing materials induces the formation of Ag nanoparticles, as observed by XRD results and inferred by FE-SEM analysis. The formation of Ag nanoparticles on the surface of Ag3PO4 particles results in a semiconductor/metal interface. This interface has an important role in the photocatalytic performance of the Ag3PO4:W-FL sample due to the charge carrier transport (Koyappayil et al., 2020; Nubla and Sandhyarani, 2020; Silva et al., 2019; Sofi and Majid, 2019). The visible light irradiation photoexcites electrons from the valence band to the conduction band. The photoexcited electrons can participate in reduction reactions with the reaction media, but also recombine with the holes in the valence band. The presence of the Ag nanoparticles on the Ag3PO4 surface under visible light irradiation can act as electron traps due to the SPR effect. Thus, the photoexcited electrons in the conduction band of AgPO4 can be transferred to the Ag nanoparticles. These electrons in the Ag nanoparticles can perform the reduction reactions with the reaction media, whereas the holes in the valence band of Ag3PO4 can perform the oxidation reactions. Herewith, the electron transfer from the conduction band of Ag3PO4 to Ag nanoparticles decreases the recombination rate of the electron-hole pairs, hence increasing their availability to perform the redox reactions. These reactions can be performed directly with the RhB adsorbed on the particle surface and also indirectly by the formation of radical species.
Moreover, as observed by Raman and UV-Vis results, the FL irradiation in Ag3PO4:W induced structural disorder in the [PO4] clusters, which generated intermediate energy levels within the band gap. These energy levels can also act as traps for photoexcited electrons in the recombination process, thus decreasing the recombination rate of the electron-hole pairs. Therefore, the FL irradiation in Ag3PO4:W sample induced the formation of Ag nanoparticles and intermediate energy levels that can act as electron traps, promoting a significant improvement of the photocatalytic performance of the Ag3PO4:W.
4. Conclusions
The FL irradiation in Ag3PO4:W sample induced the formation of metallic Ag and also structural disorder in [PO4] clusters, as observed by XRD and Raman results. The FE-SEM indicated the fragmentation and agglomeration of Ag3PO4 particles due to the high local energy of the pulsed laser. Further, it was observed the emergence of nanoparticles in the Ag3PO4 surface, which can be assigned to the Ag nanoparticles. The structural disorder in the [PO4] clusters induced the formation of intermediate energy levels within band gap, as observed by the decrease in its energy. The FL irradiation promoted a significant improvement of the photocatalytic activity of the Ag3PO4:W sample, being 3.54 times higher than the non-irradiated sample. This improvement can be attributed to the SPR effect by the formation of Ag nanoparticles and the intermediate energy levels. Both can act as traps for the photoexcited electrons, which increase the availability of the electron-hole pairs to perform the redox reactions with the reaction medium. Therefore, the FL irradiation has proved to be an effective method for the development of metal-semiconductor heterostructure and for the enhancement of photocatalytic properties.
Authors’ contribution
Conceptualization: Trench, A. B.; Longo, E.
Data curation: Trench, A. B.; Teodoro, V.; Trindade, L. G.; Machado, T. R.
Formal Analysis: Trench, A. B.; Teodoro, V.; Trindade, L. G.; Machado, T. R.
Funding acquisition: Not applicable.
Investigation: Trench, A. B.
Methodology: Trench, A. B.; Longo, E.; Minguez-Veja, G.; Cordoncillo, E.; Doñate-Buendía, C.; Andrés, J.
Project administration: Trench, A. B.; Longo, E.
Resources: Longo, E.
Software: Not applicable.
Supervision: Longo, E.
Validation: Trench, A. B.
Visualization: Trench, A. B.
Writing – original draft: Trench, A. B.; Teodoro, V.; Trindade, L. G.; Machado, T. R.; Longo, E.
Writing – review & editing: Trench, A. B.; Longo, E.; Minguez-Veja, G.; Cordoncillo, E.; Doñate-Buendía, C.; Andrés, J.
Data availability statement
All data sets were generated or analyzed in the current study.
Funding
Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP). Grant No: 2013/07296-2.
Coordenação de Aperfeiçoamento de Pessoal de Nível Superior - Brasil (CAPES). Finance Code: 001.
Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq). Grant No: 142035/2017-3.
Universitat Jaume I. Project: UJI-B2019-30; UJI-B2019-37; UJI-B2019-41.
Ministerio de Ciencia, Innovación y Universidades (Spain). Project: PGC2018094417-B-I00.
Ministerio de Ciencia e Innovación. PID2019-110927RB-I00.
Generalitat Valenciana. PROMETEO/2020/029.
Acknowledgments
The authors are very grateful to the “Serveis Centrals d’Instrumentación Científica” (SCIC) of the University Jaume I for the use of the femtosecond laser.
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