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Effects of the hybrid plasmonic Ag/SrTiO3 nanocubes for efficient photo-catalytic of H2 generation and RhB decomposition






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Abstract

Introduction: Designing a novel photocatalyst toward the photo-catalytic degradation of dye molecules and hydrogen evolution reaction (HER) based on semiconductors has been drawn enormous attention as a potential strategy in the clean energy field and environmental treatment. Herein, a SrTiO3 (STO) nanocubes decorated with co-catalysts Ag nanoparticles (NPs) for H2 generation and organic dye Rhodamine B (RhB) photodegradation activity under UV and visible light irradiation was fabricated.


Method: The crystallinity, morphology, and chemical components of the photocatalyst were characterized through X-ray powder diffraction (XRD), scanning electron microscopy (SEM) equipped with energy-dispersive X-ray spectroscopy (EDX), respectively. The optical properties were evaluated through the UV-Visible absorbance spectra.


Results: As a result, the photo-catalytic performance of the obtained Ag/STO hybrid photocatalyst was higher than that of the pristine STO nanocubes due to i) the efficient charge separation and transfer of photogenerated electron-holes pairs; ii) the improvement of the light-harvesting efficacy in the visible light. The high photo-catalytic RhB decomposition of the achieved Ag/STO hybrid photo-catalytic was obtained compared to the pure SrTiO3 nanocubes under UV and visible light exposure. The H2 generation of Ag/STO photocatalyst was 2- and 12-time higher than that of the pure STO nanocubes under UV and visible light illumination, respectively.


Conclusion: This study gives a general strategy for photocatalyst design towards water splitting for photo-catalytic H2 evolution and environmental deterioration.

Keywords: SrTiO3 hybrid structures photo-catalytic activity Ag nanoparticles

INTRODUCTION

Achieving the global energy demand and environmental sustainability is an ideal approach for the growth of clean energy to address the global energy crisis and environmental concerns 1 , 2 . Therefore, many technologies have been proposed for a cleaner environment and fossil energy alternatives. Among these, the production of hydrogen from solar-driven water-splitting reactions employing semiconductor nanomaterials as photocatalyst has a huge potential for replacement from conventional fossil fuels to renewable energy sources since the work of Honda and Fujishima was reported in the 1970s 3 . In principle, the activity of the water-splitting process based on semiconductor nanomaterials is highly influenced by the appropriate alignment of the valence band (VB) and the conduction band (CB) edges, thigh mobility of the charge carriers, the stability in an aqueous environment, and harvesting solar light capability 4 , 5 , 6 . In this sense, the perovskite oxide family, with its ABO 3 stoichiometry, especially SrTiO 3 (STO), were extensively postulated as a potential photocatalyst to produce photo-catalytic H 2 from aqueous solutions due to the structural and compositional flexibility allowing A- and B-site replacement in the crystal structure 7 , 8 . Moreover, CB of STO has more negative potential than the H + /H 2 potential (0 V vs. NHE, at pH = 0), therefore supplies favorable redox potential for photo-catalytic water splitting into H 2 gas, leading to enhanced photo-catalytic efficiencies. From that time, many efforts based on perovskite materials have been explored 9 , 10 , 11 , 12 . However, the energy conversion efficiency of photo-catalytic water splitting into H 2 is still low due to i) STO can only be activated by UV light because of its wide forbidden energy of 3.2 eV; ii) the recombination rate of photogenerated electron-hole couples is rapid. Several effective strategies to address these intrinsic drawbacks of STO have been proposed, such as the use of co-catalysts 13 , 14 , doping metal into the bandgap 15 , 16 , incorporating with other oxide metal 17 , 18 . Among these approaches, the use of co-catalysts has been considered as one of the most promising approaches for enhanced photo-catalytic H 2 generation. Recently, plasmonic nanomaterials have attached considerable concerns in the field of photo-catalytic activity related to the localized surface plasmon resonance (LSPR) and the formation of the Schottky barrier at the interface between metal and semiconductor. In view of these characteristics, noble metals using as co-catalyst are expected to advantage photo-catalytic H 2 evolution as well. The vital role of the co-catalyst is to enable visible light absorption and prolong the lifetime of photoinduced charge carriers. Some previous studies reported that coupling plasmonic nanostructures such as Ag, Au for water splitting could achieve higher photo-catalytic rates. For example, Yan et al. reported that loading Au onto CaTiO 3 composites exhibit highly enhanced photo-catalytic performance compared to pristine CaTiO 3 due to an effective separation and transportation of photoinduced electron/hole pairs in CaTiO 3 and the LSPR effect of Au 19 . Guo et al. showcased that Al incorporated with BaTiO 3 exhibited excellent photo-catalytic water splitting and pollutant degradation based on the piezoelectric polarization of BaTiO 3 and plasmonic activities of Al nanoparticles 20 . Another work reported that Au x /BaTiO 3 plasmonic photocatalysts endowed a large light absorption from 300 to 600 nm. The results exhibited a high photo-catalytic performance for MO decomposition under solar light illumination of Au x /BaTiO 3 nanocubes 21 . Based on these phenomena, herein, we demonstrate that loading Ag nanoparticles on well-defined STO nanocubes (Ag/STO) can effectively improve the photo-catalytic H 2 evolution from water splitting under visible light-responsive photocatalyst. The obtained photocatalyst are prepared via a facile and cost-effective route, in which STO nanocubes are fabricated by hydrothermal approach and loaded Ag nanoparticles through chemical reduction method under UV light irradiation. The morphological and crystal characteristics, optical properties, compositions, and photo-catalytic activity of the achieved Ag/STO heterojunctions were evaluated in detail. The results reveal that the heterostructured photocatalyst shows a greatly enhanced photo-catalytic efficiency on H 2 generation and the degradation of organic dyes under the illumination of UV and visible light compared with bare STO due to an efficient separation and transfer of photogenerated charge carriers and an improvement in the optical absorption ability.

MATERIALS - METHODS

Materials

Titanium dioxide (TiO 2 , Merck, 99%), strontium nitrate (Sr(NO 3 ) 2 , Sigma-Aldrich <99%), hydrochloric acid fuming (HCl, Merck, <37%), sodium hydroxide (NaOH, Merck, 99%), methanol (Merck, CH 3 OH, <99.9%), rhodamine B (RhB, C 28 H 31 ClN 2 O 3 , >98% purity, Merck) and silver nitrate (AgNO 3 , Merck, >=99). The chemical reagents were employed without any further purification. Double distilled water was used overall in the experiment.

Synthesis of SrTiO3 (STO) nanocubes

STO nanocubes have been fabricated by hydrothermal approach as described in our study 22 . The schematic for the fabrication of STO is presented in Schematic 1. In a typical synthesis, 20 mL of a 0.5 M TiCl 4 aqueous solution was dissolved in 60 mL of DI and vigorously stirred for 30 min. After that, a suitable amount of Sr(NO 3 ) 2 was put into the above solution and continually stirred. Then, 10 ml of 2M KOH solution was dropped into the above reaction mixture and stirred for 30 minutes. The achieved suspension was transferred in a closed Teflon-lined autoclave at 210 °C for 4 h. The precipitates were collected using the centrifugation process and washed several times with double-distilled water. In the end, the sample was dried at 100 °C to obtain the final specimen.

Synthesis of Ag loaded onto the STO photocatalyst (Ag/STO)

Ag/STO photocatalyst was achieved by the photoreduction method. In detail, STO (30mg) was dispersed into the AgNO 3 aqueous solution under stirring. The reaction mixture was irradiated under a 300 W Xe lamp at room temperature for 1 hour. After the irradiation process, the grey products were gathered using the centrifugation process, washed with double water several times, and dried at 60 °C overnight.

Materials characterization

Powder X-ray diffraction (XRD) patterns of the as-obtained photocatalyst were acquired using X-ray diffractometry (Bruker D8 ADVANCE) equipped with Cu Kα radiation (α = 1.54056 Å). Morphological characterization of the samples was evaluated using a transmission electron microscope (TEM), field-emission scanning electron microscopy (FESEM) equipped with energy disperse X-ray spectrometer (EDX). The optical absorption of the photocatalyst was assessed by UV−visible diffuse reflectance spectroscopy (V-650, JASCO) at room temperature. Raman scattering spectra of the as-prepared was recorded by a Horiba XploRA PLUS Raman System at an excitation wavelength of 532 nm.

The photo-catalytic activity for H2 evolution reaction (HER)

The photo-catalytic HER activity of samples was carried out in a Pyrex cell closed gas-circulation system. A Xe lamp (Cermax, 300 W) was utilized as the light source. In a typical process, 10 mg of the photocatalyst was dispersed in 40 mL of the aqueous solution containing 25 vol % methanol as the sacrificial agent and the reaction mixture was sonicated for 30 min to achieve a well-dispersed particle suspension. Before the light irradiation, the suspension was sealed and vacuumed for 30 min to ensure an inert environment. Then, the suspension was exposed under a 300 W xenon lamp equipped with a band-cutoff filter (420 nm). The H 2 evolution was monitored by gas chromatography with a thermal conductivity detector (TCD).

Photo-catalytic decomposition of the RhB molecules Dye

The photo-catalytic activity of the as-achieved photocatalyst was controlled under UV light (365 nm) and visible light irradiation for 150 min (Xe lamp, 300 W). Prior to light illumination, the mixture of aqueous RhB solution and the photocatalyst was placed in a dark. The remaining RhB concentration was investigated through a UV−vis spectrophotometer at the wavelength of 554 nm. The % decomposition of RhB dye was evaluated using the equation:

RhB decomposition (%) = [(C 0 -C t )/C 0 ] ´ 100

Where, C o and C t are the RhB concentration at the initial time and after irradiation for time “t”, respectively.

RESULTS

The detailed morphological characteristics of the as-prepared STO and Ag/STO nanocubes were investigated via SEM and TEM analyses. As shown in Figure 1 (a), the pristine STO exhibits 3D nanostructures with an average particle size of ca.300 nm and an almost perfect cubic structure with six isotropic {100} facets. As mirrored in Figure 1 (b), structures of Ag/STO are analogous to those of STO. Moreover, after photo-deposition of the Ag NPs on STO, a large number of Ag nanoparticles with the particle size of ca.30 nm was assembled on the whole STO surface, as marked by the yellow arrows ( Figure 1 (b)). As shown in Figure 1 (b), the Ag atoms were not easily discovered as separate particles on the surface of STO, implying the Ag atoms were homogeneously deposited on the STO. The TEM image in Figure 1 (c) reveals the nanocubes of Ag/STO with almost the same size as STO, indicating that Ag assembly did not change the morphological features of STO structures, which is consistent with SEM images. The EDX mapping images show the presence of Sr, Ti, O, and Ag elements of Ag/STO photocatalyst as presented in Figure 1 (d-h), suggesting that Ag nanoparticles were deposited successfully on STO nanocubes via photoreduction method under UV light irradiation.

Figure 1 . The morphological features and chemical elements of the pristine STO and the Ag/STO photocatalyst (a, b) SEM image of the pristine STO, and Ag/STO photocatalyst, respectively, (c) TEM image of the Ag/STO specimen, and (d-g) elemental mapping of Sr, Ti, O, and Ag, respectively, (h) EDX spectrum of the Ag/STO heterostructures.

Figure 1

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The crystal information of the pristine STO and Ag/STO photocatalyst was assessed through XRD analyses, as displayed in Figure 2 . The XRD patterns of the samples exhibit typical diffraction peaks of cubic perovskite STO, in which the characteristic peaks at 2θ of 24.807, 26.507, 28.182, 36.620, 43.681, and 47.839 are assigned to (100), (002), (101), (102), (110), and (103) crystal planes respectively (JCPDS no. 74-1296). Furthermore, the peak appearing at 2θ = 38° is produced in STO/Ag nanocubes belonging to the Ag phase about the JCPDS card no. 04-0783. This demonstrated that the AgNPs were deposited successfully on the surface area of STO, which is consistent with the results of the TEM image in Figure 1 .

Figure 2 . The crystallinity using XRD patterns of the obtained Ag/STO and pristine STO photocatalyst.

Figure 2

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The optical properties of as-prepared specimens are important processes for photo-catalytic reactions. Therefore, the UV−vis spectra were used to investigate the optical characteristic of the photocatalysts ( Figure 3 ). As reflected by Figure 3 , the pristine STO photocatalyst shows absorption edges at 388 nm related to a charge transfer from the valence band (VB) to the conduction band (CB), which corresponds to a bandgap energy of 3.2 eV for pristine STO ( Figure 3 (b)). For the Ag/STO sample case, the Ag/STO photocatalyst exhibits visible-light absorption with an absorption edge at ∼ 450 nm due to the LSPR of Ag NPs, which is beneficial for enhancing the photo-catalytic HER activity in the visible light.

Figure 3 . The optical characteristics of the photocatalyst using the UV–Vis diffuse reflectance spectra (a) and plot of (ah ) 1/2 vs. photon energy (b) of the pure STO and the Ag/STO specimen.

Figure 3

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To evaluate the effect of decorating with Ag on the surface of the SrTiO 3 nanocubes for photo-catalytic H 2 evolution activities. The photo-catalytic H 2 evolution performance of photocatalyst was accomplished using water/methanol solution under UV light and visible light, as shown in Figure 4 . As observed, the H 2 production of the Ag/SrTiO 3 sample exhibited significantly higher than that of the pure STO under experimental conditions. Under UV light, the Ag/STO sample achieved the H 2 evolution of ~ 414 mol.h −1 .g −1 , which is ~ 2 times that photocatalyst with the pure STO nanocubes due to efficient charge separation. Interestingly, the amount of H 2 produced by the Ag/STO photocatalyst was ~ 316 mol.h −1 .g −1 , roughly 12-times that of the pure STO under visible light, whereas, no appreciable H 2 production was observed under visible light irradiation of the pure STO nanocubes. This could be attributed to the larger bandgap energy of the single STO that cannot be reached under visible light, leading to low H 2 . On the other hand, compared with that of the pure STO, the Ag/STO photocatalyst exhibited outstanding H 2 photo-catalytic activity. Additionally, the reusability of a photocatalyst is also a critical factor for practical applications. The heterostructure of Ag/STO was thus employed for H 2 production under UV light ( Figure 5 ). The H 2 performance of the Ag/STO remained unchanged after 4 cycles, implying that the high durability of the as-obtained photocatalyst.

Figure 4 . The photo-catalytic H 2 evolution of the obtained photocatalyst under the different irradiation (a) under UV light, (b) visible light of the STO and Ag/STO photocatalyst.

Figure 4

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Figure 5 . The recyclability performance for H 2 activity under visible light illumination after 4 cycles of the Ag/STO photocatalyst.

Figure 5

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The photo-catalytic performance of the single STO and Ag/STO photocatalyst was evaluated under photodecomposition of RhB aqueous solution with the existence of UV light and visible light irradiation after 120 min, as shown in Figure 6 . It could be clearly observed that no decomposition of the RhB was achieved without the photocatalyst under UV and visible light irradiation, which may be assigned to the low self-degradation of RhB. In contrast, the effective decomposition of RhB in the presence of photocatalyst and light energy source was obtained, thereby indicating that the photocatalyst and light irradiation plays a significant role in the photodegradation activity of RhB solution. Compared with the pure STO, the Ag/STO photocatalyst showed a higher photodegradation of the RhB dye under both UV and visible light exposure. As presented in Figure 6 , the Ag/STO photocatalyst exhibited outstanding RhB decomposition with degradation rates of RhB of approximately ~80 % and ~70 % under exposure to UV light and visible light, respectively.

Figure 6 . The photo-catalytic performance of the photocatalyst through decomposition of RhB organic dyes.

Figure 6

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DISCUSSION

The morphological and crystal characteristics of STO did not significantly change after the introduction to Ag nanoparticles by hydrothermal pathway and photo-reduction method as shown in Figure 1 and Figure 2 . The photocatalytic degradation of dye molecules and hydrogen evolution reaction (HER) of the Ag/STO photocatalyst was higher than that of the pristine STO under both UV and visible light exposure. This could be explained by i) improvement of absorption ability in the visible light region based on the LSPR effect of AgNP, which efficiently prompted the absorption and separation of the photoinduced electron-hole pairs; ii) the effective separation and transport of the photogenerated charge carriers based on the formation of a Schottky barrier between the Ag and STO, leading to an enhanced photo-catalytic H 2 generation and photodegradation of the RhB dye. Under irradiation with an photon energy equal or greater than the bandgap energy of semiconductor, the photoinduced electron–hole pairs are generated. These photoinduced electrons can reduce organic pollutants or water to form H 2 production. Meanwhile, the photoinduced holes react with dye molecules to generate a strong oxidizing agents, which improve the decomposition of dye molecules into nontoxic products 22 . Based on the above results, to better understand the photo-catalytic improvement of the hybrid photocatalyst compared with the pure photocatalyst, a mechanism of their photo-catalytic activity was discussed. Upon exposure to UV light, STO is excited and generated the photoinduced electron-hole pairs. These electrons jump to the CB and transfer to Ag NPs. They reduce protons (H + ) to generate H 2 . Meanwhile, the photogenerated holes on the VB of STO can oxidize the absorbed H 2 O molecules into hydroxyl radicals (OH • ) 23 . Under visible light irradiation, STO cannot be activated because of its large energy gap. Meanwhile, the AgNPs can strongly absorb under the visible light based on the effect of LSPR to form the hot electrons 24 . These hot electrons move to the CB of STO and reduce H + to produce H 2 gas. The holes on the Ag surface can react with H 2 O to form OH • in a successive reaction route. These formed reactive species decompose RhB molecule dyes into nontoxic products. These outcomes from this work provide new insight into the water-splitting performance and photo-catalytic RhB degradation in practical applications based on the incorporation of perovskite and noble metal.

CONCLUSION

In summary, Ag/STO heterostructures were successfully synthesized by the hydrothermal method and photo-reduction under assisted-UV light. An outstanding photo-catalytic and yield in H 2 evolution reaction of the Ag/STO photocatalyst in comparison with the pristine STO was observed. This could be attributed to the synergetic effect between STO and Ag and the LSPR effect of Ag that was responsible for the effective separation and transportation of the charge carriers and inhibition of the rapid recombination of the photoinduced charge carriers on the Ag/STO hybrid. As a result, the recombination of the photogenerated electron-hole pairs on the photocatalyst was eliminated through the establishment of the Schottky channel, and the strong absorption in the visible light was enhanced via the LSPR effect of AgNPs, providing an efficient charge separation and transfer of the hybrid photocatalyst. Thus, the photo-catalytic activity for the RhB photodegradation efficiency of Ag/STO was ~ 80% and ~ 70% under UV and visible light, respectively. Furthermore, the H 2 evolution rate of the achieved Ag/STO nanocubes was approximately 414 and 316 mol.h −1 .g −1 under UV and visible light illumination, respectively. This study can give an efficient pathway for designing the photo-catalytic system for environmental treatment and renewable energy production.

ABBREVIATIONS

Ag : Silver

SrTiO 3 : Strontium titanate

COMPETING INTERESTS

The authors declare that there is no conflict of interest regarding the publication of this article.

AUTHORS’ CONTRIBUTIONS

Ton Nu Quynh Trang has conceived of the present idea, carried out and written the manuscript with support from Vu Thi Hanh Thu.

Le Thị Ngoc Tu and Le Lam Anh Phi has supported the analytical techniques.

ACKNOWLEDGEMENTS

Ton Nu Quynh Trang was funded by Vingroup Joint Stock Company and supported by the Domestic Master/PhD Scholarship Programme of Vingroup Innovation Foundation (VINIF), Vingroup Big Data Institute (VINBIGDATA), code [VINIF.2020.TS.08].

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Article Details

Issue: Vol 24 No 3 (2021)
Page No.: 2011-2018
Published: Aug 2, 2021
Section: Section: NATURAL SCIENCES
DOI: https://doi.org/10.32508/stdj.v24i3.2568

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Copyright: The Authors. This is an open access article distributed under the terms of the Creative Commons Attribution License CC-BY 4.0., which permits unrestricted use, distribution, and reproduction in any medium, provided the original author and source are credited.

 How to Cite
Trang, T. N. Q., Phi, L., Thi Ngoc Tu, L., & Thi Hanh Thu, V. (2021). Effects of the hybrid plasmonic Ag/SrTiO3 nanocubes for efficient photo-catalytic of H2 generation and RhB decomposition. Science and Technology Development Journal, 24(3), 2011-2018. https://doi.org/https://doi.org/10.32508/stdj.v24i3.2568


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