CuFeO<sub>2</sub>/Cu Photoelectrode Modified with SrTiO3 Perovskite for Efficient Hydrogen Generation from Sanitation Water

Ahmed, Aya; Ahmed, Ashour M.; Abdel-Khaliek, Ahmed A.; Shaban, Mohamed; Abdelazeez, Ahmed Adel A.; Rabia, Mohamed

doi:https://doi.org/10.1155/2023/4440117

International Journal of Energy Research

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Abstract Introduction Results and Discussion Conclusions Data Availability Conflicts of Interest Authors’ Contributions Acknowledgments References Copyright Related Articles

Research Article | Open Access

Volume 2023 | Article ID 4440117 | https://doi.org/10.1155/2023/4440117

CuFeO₂/Cu Photoelectrode Modified with SrTiO3 Perovskite for Efficient Hydrogen Generation from Sanitation Water

Aya Ahmed,^1,2Ashour M. Ahmed,³Ahmed A. Abdel-Khaliek,¹Mohamed Shaban,⁴Ahmed Adel A. Abdelazeez,⁵and Mohamed Rabia^2,6

Academic Editor: Tholkappiyan Ramachandran

Received15 Mar 2023

Revised27 May 2023

Accepted04 Jul 2023

Published28 Jul 2023

Abstract

We prepared a perovskite material, copper-doped strontium titanate (Cu-SrTiO₃), using the chemical bath deposition method and cast it on a CuFeO₂/Cu photoelectrode to generate hydrogen from sanitation water splitting. This preparation method considers a simple mass product and does not depend on complex techniques. The prepared perovskite materials had a compact nano-/microstructure. Both CuFeO₂ and Cu-SrTiO₃/CuFeO₂ exhibited excellent optical properties, with bandgap values of 1.4 and 1.26 eV, respectively. Here, the prepared CuFeO₂ and Cu-SrTiO₃ thin films are used as photoelectrodes for hydrogen generation, and their current-voltage relationship is analyzed under various conditions, such as different light intensities, wavelengths, and temperatures. This approach is promising for using wastewater as a source of hydrogen gas without requiring any additional electrolyte, making it a dual-purpose approach for both hydrogen generation and wastewater treatment. Through the electrochemical study, increasing the light intensity from 25 to 100 mW.cm^-2 resulted in a corresponding increase in the produced values from -1.02 to -1.292 mA.cm^-2. Similarly, the values increased from -1.25 to -1.91 mA.cm^-2 as the temperature increased from 30 to 70°C. We also calculated all thermodynamic parameters, the quantum efficiency (QE), and incident photon to current conversion efficiency (IPCE). For the Cu-SrTiO₃/CuFeO₂/Cu photoelectrode, the activation energy () value was 14.14 kJ mol^-1, while the and values were 11.46 kJ·mol^-1 and 34.9 kJ^-1·mol^-1, respectively. Additionally, the IPCE value was 3.31%. The prepared photoelectrode showed high stability and low cost, making it a potential candidate for industrial applications.

1. Introduction

Renewable energy sources are critical to human life’s actuality. The bulk of these sources are based on photocatalytic materials used in the fabrication of photodetectors, solar cells, and photocatalytic electrodes [1–4]. Hydrogen is one of the most ecofriendly and sustainable energy carriers available, and it may replace fossil fuels. Currently, most of the H₂ is generated from methane or fossil fuels with a significant carbon footprint. Extensive research is being performed to develop new technologies for economically producing hydrogen from renewable materials [5–7]. Photoelectrochemical (PEC) water splitting is regarded as one of the most promising methods for hydrogen production. The creation of H₂ gas by a water-splitting process is a vital energy source for aircraft, vehicles, and industries that utilize H₂ fuel. The synthesized photoelectrode must have high water-splitting efficiency and qualities that qualify it for numerous applications, such as low cost, simple preparation, easy operation, and stability [8]. The electrode can be utilized in sunlight or with another type of artificial light. Perovskite oxide substances are currently considered promising photocatalysts for a variety of potential photocatalytic applications due to their promising qualities, including compositional flexibility, excellent electronic, optical, and magnetic properties, overall resistance to photocorrosion, and excellent thermal stability properties [6, 9]. These characteristics are anticipated to improve their stability and desired photocatalytic activity. The single perovskite oxides can be represented as ABO₃, where A and B are metal cations. Alkaline-earth metal cations, transition metal cations, or alkali metal cations are the three options for A and B [10–12].

The morphologies and surface properties of several perovskite oxides, including SrTiO₃, KTaO₃, NaTaO₃, KNbO₃, Zn_1-xBa_xFe₂O₄, ZnFe_1.96La_0.04O₄, BiFeO₃, and NaNbO₃, were observed to have a significant impact on the photocatalytic activities in this context [13–15]. The main characteristics of perovskite oxide-based photocatalysts in solar-driven photocatalytic hydrogen evolution reaction (HER) have been particularly emphasized in several great academic studies over the past few years. Recent studies have proven the insertion of transition metal causes additional enhancement in these perovskite materials that appear as enhancements in the optical and electrical properties [16–20].

Recent advances in single perovskite oxide ABO₃-based photocatalysts, perovskite materials, and SrTiO3-based photocatalysts for use in HER via water splitting were also discussed [21]. Certainly, photocatalysts based on perovskite oxide will play a vital role in solar-driven HER during the next years. It is found that the current H₂ evolution rate is still low and will require further enhancement in the future. This has motivated the scientific community to focus on understanding the existing state of affairs and ideas for improving the overall quality, productivity, and efficiency of perovskite material or oxide catalysts for HER [22–24].

The main goal of this study was to develop a SrTiO₃/CuFeO₂/Cu photoelectrode for hydrogen generation through water splitting. To achieve this, the CuFeO₂ and Cu-SrTiO₃ layers were fabricated using combustion and chemical bath deposition methods, respectively. The efficiency of the photoelectrode for H₂ production was evaluated by analyzing its current-voltage relationship under various light intensities, wavelengths, and temperatures. Additionally, various thermodynamic parameters were calculated along with quantum efficiency (QE) and incident photon-to-current conversion efficiency (IPCE). The photoelectrode showed high stability and has promising potential for utilization in the industrial sector.

2. Experimental Methodology

2.1. Preparing of CuFeO₂ Perovskite Layer

Cu foil with a dimension was immersed in 3 ml of Conc. H₂SO₄ for 15 min on each side, then washed with deionized water. Then, the copper substrate was immersed in 0.1 FeCl₃, dissolved in 50 ml of deionized water for 20 min on each side, left hanging to dry in the air for 15 min, then heated over a hot plate at 50°C for 10 min, and then annealed inside a tube at 500°C for 10 min using a CVD furnace.

2.2. Preparation of Cu-SrTiO₃ Perovskite Layer

0.1 M of strontium chloride (SrCl₂, 99.6%) and 0.02 M of copper chloride (CuCl₂, 99.7%) were dissolved in 10 ml of isopropanol (99.0%) using ultrasonic for 1 min. Then 5 ml of this solution was added to 0.1 M of titanium isopropoxide (99.9%). Cast 100 μl of Cu-SrTiO₃ solution over the CuFeO₂ layer, then let it dry in the air and then over a hot plate at 50°C for 15min, and then anneal inside a tube at 500°C for 10 min using a CVD furnace. Ag paste is diluted by adding a couple of drops of acetone (98.9%), then deposited on one side of the cell drop using cotton bud and then dried it over a hot plate at 70°C for 2 min.

2.3. Samples Characterization

The prepared perovskite layers were characterized using different devices. The chemical structure was confirmed using an X-ray diffractometer (XRD, Bruker/Siemens D5000, Aubrey, TX, USA) by Kα radiation of Cu (λ = 1.5405 Å) at 30 mA and 40 kV. Moreover, the chemical structure was confirmed using X-ray photoelectron spectroscopy (XPS) models (advance diffractometer, Bruker D8) and K-ALPHA, USA. Besides, the elements inside the materials and morphologies were determined using a scanning electron microscope (SEM, Auriga Zeiss FIB, Zeiss Company, Oberkochen, Germany). Also, the morphologies were confirmed using transmitted electron microscope (TEM) models Hitachi, S-4800, and JEOL JEM-2100, respectively. The optical properties were characterized using a double-beam spectrophotometer (Perkin Elmer Lambda 950, Perkin Elmer Company, Waltham, MA 02451, USA).

2.4. Water-Splitting Test

The water splitting reaction happened under a solar simulator from a three-electrode cell, in which the Cu-SrTiO₃/CuFeO₂/Cu represented the working electrode as a cathode, whereas graphite and calomel electrodes were worked as counter and reference electrodes, respectively. These electrodes are partially immersed in 30 ml of filtered sanitation water (third-stage treated, company of drinking water and wastewater, Beni-Suef City, Egypt). The measurements were carried out using an electrochemical workstation (CHI660E) at a scan rate of 100 mV.s^-1. The effects of light intensity (100 to 400 mW.cm^-2), incident wavelength (390 to 636 nm), temperature reaction (30 to 70°C), and time stability were studied for water splitting for H₂ generation (Figure 1).

3. Results and Discussion

3.1. Analyses

3.1.1. XRD and XPS Analyses

The XRD of the delafossite, CuFeO₂, materials are shown in Figure 2 (black line). From this figure, all characteristic peaks related to CuFeO₂ are confirmed; this is related to the peaks located at 34.1°, 35.5°, 38.5°, 53°, 61.2°, and 68°. These peaks are matched with the analysis for the hexagonal and rhombohedral structures (JCPDS No. 75-2146) [25]. These peaks confirm the highly crystalline nature of the prepared CuFeO₂ materials. The XRD for the STO is shown in Figure 2 (red curve). The characteristic peaks located at 22.09^o, 31.88^o, 41^o, 45.83^o, and 53.83^o matched with the growth directions (100), (110), (111), (200), and (211), respectively. These characteristic peaks confirm the highly crystalline nature of the prepared perovskite materials, STO. Moreover, these peaks are matched with the previous studies. There are additional peaks for Cu_xSrTi_1-xO₃; these peaks are related to the formation of these materials under the incorporation of Cu inside the chemical structure of STO. These additional peaks are matched with the previous studies.

The oxidation states and chemical environment of components in Cu-SrTiO3 were determined using XPS. The XPS survey spectrum of Cu-SrTiO₃ is featured in Figure 3(a), which displays the different elements and their BE. The XPS plot comprises Cu 2p, O1s, Ti 2p, C 1s, and Sr 3d5 at 932.71, 531.26, 459.17, 283.25, and 135.83 eV, respectively. The above findings suggest forming Cu-SrTiO₃ thin films through the solvothermal method. Figures 3(b)–3(e) show elements of a Cu-SrTiO3 sample for O1s, Cu 2p, Sr3d, and Ti 2p, respectively. Binding energy peaks for O1s were observed at 531.26, 531.8, and 528.4 eV, which correlate to various chemical states of oxygen. Due to the existence of Sr-O and Ti-O bonds in the SrTiO₃ crystal lattice, the O1s XPS signal attributed to the oxygen crystal lattice was detected at 528.4 eV. Surface oxygen was assigned a peak position of 531.8 eV due to hydroxyl groups [26, 27]. On the other hand, the peak at 531.26 eV was attributable to a surface-coordinated water molecule. Figure 3(c) exhibits two significant peaks at around 932.6 and 952.4 eV that may be attributed to Cu2p3/2 and Cu 2p1/2, respectively, indicating that the synthesized material has a monovalent copper cation (Cu+). From Figure 3(d), the Sr 3d5/2 peaks at 134.04 eV and the Sr3d 3/2 peaks at 135.65 eV. As well, Ti2p peaks at 458.17 eV and 464.19 eV are illustrated in Figure 3(e).

(a)

(b)

(c)

(d)

(e)

(f)

The surface types of Fe, Cu, O, and C atoms in CuFeO₂/Cu are shown in the survey X-ray photoelectron spectrum in Figure 3(f), which displays the different elements and their corresponding binding energies (BE). The XPS plot comprises Cu2p, Fe2p, O1s, and C1s at 932.61, 711.25, 530.98, and 285.0 eV, respectively. The above findings suggest that the CuFeO₂/Cu thin film is produced through the combustion approach.

3.1.2. SEM and TEM Studies

In Figure 4(a), the design of a homogenous highly crystalline surface is seen. The crystals are compacted and connected high together on one surface. The formed nano-/microparticle for the perovskite materials is expected to have high optical properties. The significant roughness and minimum porousness of the Cu-SrTiO₃/CuFeO₂/Cu surface qualify it for absorbing light in many directions in an area of nm, as drawn with the ImageJ program (Figure 4(b)). The SEM of the CuFeO₂/Cu thin film is presented in Figure 4(c). It could be seen that the highly crystalline polyhedral CuFeO₂/Cu delafossite thin film is free of cracks with a smooth surface. This surface is used as a substrate for the deposition of the Cu-SrTiO₃ materials.

The TEM image of Cu-SrTiO₃/CuFeO₂/Cu is shown in Figure 4(d). This figure reveals the nano-/microstructured morphology of Cu-SrTiO₃/CuFeO₂ with an average crystalline particle size of 200 nm.

3.1.3. Optical Analyses

The optical characteristics of the prepared Cu-SrTiO₃/CuFeO₂ and CuFeO₂ are shown in Figure 5(a). The refraction of CuFeO₂ is higher than that of Cu-SrTiO₃/CuFeO₂, indicating that the absorption intensity is increasing, in which the electron transition is the main factor for peak formation in the UV, Vis, and near IR regions [28–31].

(a)

(b)

The CuFeO₂ and Cu-SrTiO₃/CuFeO₂ bandgap () values of 1.4 and 1.26 eV, respectively, show an improvement in optical characteristics (Figure 5(b)). The Kubelka-Munk equation was used to obtain the value, where and are the scattering and absorption coefficients, respectively; is the diffuse reflectance; and is the Kubelka-Munk function [32].

3.2. Photoelectrochemical Activity

In the presence of a Xenon lamp (Newport, 66926-500HX-R07), the photoelectrochemical performance of the constructed electrode Cu-SrTiO₃/CuFeO₂/Cu for hydrogen generation is measured. The electrochemical workstation used for the measurements is CHI660E. The relationship between voltage and current density is revealed in Figure 6(a). It appears that the Cu-SrTiO₃/CuFeO₂/Cu electrode served as a photocathode for the formation of H₂ gas. Figure 6(a) shows that when exposed to light, the resultant current density () is 1.292 mA.cm^-2 at 0.5 V. The result of light intensity on the prepared photoelectrode is shown in Figures 6(a) and 6(b). When the light intensity is increased from 25 to 100 mW.cm^-2, the produced values increase from -1.02 to -1.292 mA.cm^-2. The rises with increasing light intensity owing to enhanced electron-hole pair production [33, 34]. The generated current is directly proportional to the amount of light absorbed. Because indicates the current density generated in the cell as a result of water splitting, it can also measure the rate of hydrogen generation from sanitation water.

(a)

(b)

As seen in Equation (2), the number of photons () is directly proportional to the intensity of light (P) [35]. This equation is also affected by other parameters including wavelength (), Planck constant (), and light velocity (). Applying this equation, the per second is changed from photon/s under light intensity from 25 to 100, and mW·cm⁻² is changed from to photon/s, respectively.

The stability of the prepared Cu-SrTiO₃/CuFeO₂/Cu photoelectrode was investigated, as shown in Figure 7(a). The relationship between time and the generated value is discussed, and the produced value under light and dark chopping is steady with time (500 s) at around -0.11 mA.cm^-2. According to the figure, the electrode has good stability and high light sensitivity. The variation in values across on- and off-chopped light is clearly visible. The remarkable influence of light on the electrode confirms the electrode’s high sensitivity to light. Figure 7(b) depicts the repeatability of the electrode over two runs, with the voltage-current relationship exhibiting similar performance through four runs. This repeatability has been tested at 25°C and under natural light.

(a)

(b)

The temperature effect on the Cu-SrTiO₃/CuFeO₂/Cu photoelectrode for hydrogen generation because of water splitting is revealed in Figure 8(a), where the rises from -1.25 to -1.91 mA.cm^-2 as the temperature increases from 30 to 70°C, correspondingly. The overall rise in values represents the rate of the reaction, which correlates to the rate of hydrogen generation [2, 36]. The produced values at various temperatures are mentioned in Figure 8(b). Relying on particle collision and the rate of water splitting, the activation energy (Ea) could be determined using the Arrhenius equation, Equation (3), where , , , and are the rate, universal gas, absolute temperature, and Arrhenius constants, respectively [34]. The value defines the degree of reaction occurrence [37–39].

(a)

(b)

(c)

(d)

Figure 8(c) shows that the slope values of the relationship and 1/T yield the value. For the Cu-SrTiO₃/CuFeO₂/Cu photoelectrode, the value is 14.144 kJ mol^-1. When analyzed with previously published results for different photocatalysts, the value for this electrode is exceptionally low. As a result of the water-splitting reaction, the synthesized electrode is effective for H₂ evolution. Similarly, utilizing the Boltzmann constant (kB) and the Planck constant (), the Eyring equation (4), maybe get the enthalpy () and entropy ()

To determine the and values, slope and intercept from Figure 8(d), respectively, are used. The value of Cu-SrTiO₃/CuFeO₂/Cu photoelectrode is 11.46 kJ·mol^-1, while value is 34.9 kJ^-1·mol^-1.

The photocurrent produced as a result of photon energy is defined as the incident photon-to-current conversion efficiency (IPCE). The wavelength value can be used to determine it. Equation (5) is used to compute the IPCE [18, 40–42].

In Figure 9, the IPCE is calculated at a light intensity of 100 mW.cm² and a temperature of 30°C. At 390 nm, the electrode has the optimum IPCE of 3.31%. This value is reduced by raising the wavelength to 500 nm, then rising until it reaches 636 nm. The IPCE value is obtained from the impact of the electrode’s photocatalytic ability for sanitation water splitting without the presence of an additional electrolyte. As a result, the device converts sanitation water to H₂ with more efficiency than earlier studies have shown.

Equation (6) was used to determine the amount of H₂ moles [43], where is the Faraday constant and is the time change. Production of H₂ increases with time, corresponding to 10 ml/h for the sample with a dimension of 20 cm² for hydrogen production from a photoelectrode. Moreover, Table 1 illustrates a comparison of our study with previous literature.

4. Conclusions

A photodetector made of Cu-SrTiO₃/CuFeO₂/Cu was used to produce hydrogen gas from sanitation water. XRD analysis confirmed the formation of perovskite materials, including SrTiO₃ and Cu_xSrTi_1-xO₃, as well as CuFeO₂ and CuO. SEM analysis confirmed that the materials were highly crystalline with small surface pores. The materials’ excellent optical properties were confirmed by their small bandgap values of 1.4 and 1.26 eV for CuFeO₂ and Cu-SrTiO₃/CuFeO₂, respectively. During hydrogen generation, values were significantly enhanced under light compared to dark conditions. Moreover, increasing the light intensity from 25 to 100 mW/cm² increased the produced values from -1.02 to -1.292 mA/cm². Temperature also had a significant effect, with the rising from -1.25 to -1.91 mA/cm² as the temperature increased from 30 to 70°C. The study measured various thermodynamic parameters related to the rate of hydrogen gas evolution, including an value of 14.14 kJ mol^-1 and and values of 11.46 kJ mol^-1 and 34.9 kJ mol^-1, respectively. These findings are promising for H₂ gas fuel production, and the team plans to design a prototype of cells that can directly convert wastewater into H₂ gas fuel.

Data Availability

The authors confirm that the data supporting the findings of this study are available within the article.

Conflicts of Interest

The authors declare that they have no conflicts of interest.

Authors’ Contributions

The methodology was prepared by Aya Ahmed. Formal analysis was done by Ashour M. Ahmed, Ahmed A. Abdel-Khaliek, Mohamed Shaban, Ahmed Adel A. Abdelazeez, and Mohamed Rabia. The investigation was performed by Ahmed Adel A. Abdelazeez and Mohamed Rabia. Supervision was implemented by Ahmed A. Abdel-Khaliek, Mohamed Shaban, and Mohamed Rabia. Writing—original draft preparation—was done by Aya Ahmed and Mohamed Rabia. Writing, which includes review and editing, was performed by Ahmed A. Abdel-Khaliek, Ahmed Adel A. Abdelazeez, and Mohamed Rabia. Open Access funding is enabled and organized by Carolinas 2023.

Acknowledgments

This paper is based on work supported by the Science, Technology & Innovation Funding Authority (STDF) under a grant given to Aya Ahmed, with the project number 44746.

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Copyright © 2023 Aya Ahmed et al. This is an open access article distributed under the Creative Commons Attribution License, which permits unrestricted use, distribution, and reproduction in any medium, provided the original work is properly cited.

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International Journal of Energy Research

CuFeO2/Cu Photoelectrode Modified with SrTiO3 Perovskite for Efficient Hydrogen Generation from Sanitation Water

Abstract

1. Introduction

2. Experimental Methodology

2.1. Preparing of CuFeO2 Perovskite Layer

2.2. Preparation of Cu-SrTiO3 Perovskite Layer

2.3. Samples Characterization

2.4. Water-Splitting Test

3. Results and Discussion

3.1. Analyses

3.1.1. XRD and XPS Analyses

3.1.2. SEM and TEM Studies

3.1.3. Optical Analyses

3.2. Photoelectrochemical Activity

4. Conclusions

Data Availability

Conflicts of Interest

Authors’ Contributions

Acknowledgments

References

Copyright

CuFeO₂/Cu Photoelectrode Modified with SrTiO3 Perovskite for Efficient Hydrogen Generation from Sanitation Water

2.1. Preparing of CuFeO₂ Perovskite Layer

2.2. Preparation of Cu-SrTiO₃ Perovskite Layer