Home Nanostructured p-PbS/p-CuO sulfide/oxide bilayer heterojunction as a promising photoelectrode for hydrogen gas generation
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Nanostructured p-PbS/p-CuO sulfide/oxide bilayer heterojunction as a promising photoelectrode for hydrogen gas generation

  • Mohamed Zayed , Mamduh J. Aljaafreh EMAIL logo , Mohamed Shaban , Mahmoud Hezam , Sodky H. Mohamed , Mohamed Rabia , Mohammad Marashdeh , M. Al-Hmoud and Ashour M. Ahmed EMAIL logo
Published/Copyright: December 31, 2023
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Open Chemistry
From the journal Open Chemistry Volume 21 Issue 1

Abstract

Recently, the photoelectrochemical (PEC) water-splitting reaction for hydrogen (H2) production has been a competitive research route to realize clean and sustainable electric power. In this work, copper oxide (CuO) and PbS thin films were fabricated on commercial glass, respectively, using the techniques of successive ionic-layer adsorption and reaction and chemical bath deposition. These nanostructured thin films served successfully as photoelectrodes for the photogeneration of H2. In addition, a p-PbS/p-CuO bilayer system was also fabricated, and a remarkable boost in PEC efficiency was observed compared to pure CuO and PbS thin films. Optical examinations showed excellent absorbance properties of the p-PbS/p-CuO bilayer in the visible range, with a bandgap of ∼1.28 eV. X-ray diffraction analysis indicated a monoclinic CuO/cubic PbS crystalline structure with a particle size of ∼18 nm. The photocurrent density (J ph) values were obtained using a three-electrode electrochemical cell in 0.3 M Na2S2O3 electrolyte. The p-PbS/p-CuO photoelectrode demonstrated a J ph value of −0.390 mA cm−2, which is significantly higher than the values of −0.120 and −0.008 mA cm−2 for the pure PbS and CuO photoelectrodes, respectively. This improvement is attributed to the p-PbS/p-CuO oxide/sulfide bilayer heterojunction, which improved the visible light absorption and reduced the electron–hole (e–h) recombination. The effects of pH value, temperature light intensity, and wavelength were all additionally studied. Remarkably, the photoelectrodes were stable under a pH of ∼7, which makes them promising for H2 production using normal drinking/seawater. These findings confirm the ability of the prepared photoelectrodes to facilitate water splitting and H2 generation under various environmental, chemical, and illumination conditions.

Graphical abstract

Keywords: CuO; PbS; p-PbS/p-CuO bilayer; photocatalyst; water splitting; H2 generation

1 Introduction

Fossil fuel combustion produces limited energy along with harmful gases such as NO X , SO X , and CO X , which contribute to the greenhouse effect and pose serious health risks to humans, animals, and plants even at low concentrations [1,2,3]. Hydrogen (H2) gas can be a promising solution to the energy crisis as its combustion produces a large amount of clean energy, and it can be produced from abundant compounds such as water [4,5,6]. H2 fuel has the potential to power a range of technological devices, from aircraft and rockets to homes, businesses, and factories. The production of H2 gas relies on the use of photocatalytic semiconductor materials, such as metal oxides, nitrides, and sulfides. Metal oxides are advantageous due to their low cost, availability, and high stability. The metal sulfides provide small bandgaps and high light absorption [7,8,9]. Bilayers of metal oxide and metal sulfide are expected to have high efficiency in H2 production.

Among nanomaterials, copper oxide (CuO) nanostructures have been investigated as a potential photocatalytic material due to their small bandgap [10,11]. This characteristic allows CuO to absorb sunlight in the ultraviolet (UV), visible, and near-IR regions. CuO is a non-toxic, p-type semiconductor. It is of low cost with relatively high conductivity, which makes it suitable for several applications. However, it is suffering from photo-corrosion and fast e–h pair recombination. There are many previous studies that have shown a limited success in enhancing the photocatalytic activity of CuO-based materials. For example, Ragupathi et al. [12] reported a small J ph value (1.0 µA at 1.2 V) for CuO/g-C3N4 composite as photocatalytic materials for water-splitting reaction. Other studies attempted to synthesize CuO-C/TiO2, but their J ph value was also low (0.012 mA cm−2) [13].

On the other hand, lead sulfide (PbS) is a promising p-type semiconductor with a narrow gap [14]. The bandgap energy of a PbS film can be tuned depending on the grain size, primarily due to the quantum confinement effect. It has high conductivity and a high dielectric constant. PbS possesses unique electronic characteristics that are governed by the interaction of the anions [15]. PbS is suitable for electric, optoelectric, and optoelectronic devices due to its relatively large Bohr radius of 18 nm. PbS has the feature of multiple exciton generation effects, which increase the quantum efficiency [16]. It has a high dielectric constant, excellent photosensitivity, high carrier mobility, and a long excitonic lifetime (200–800 ns). In addition, PbS is used as a window layer for heterojunction due to its superior visible light absorbance, good chemical stability, and easy ohmic contact. Likewise, PbS displayed a quick photogenerated carrier separation, which suppressed the e–h pair recombination efficiently [17]. Hsu et al. presented Al-doped ZnO nanorods coated with PbS nanoparticles as a photoelectrode for solar water splitting [18]. Halder et al. studied PbS/TiO2 for H2 production with an optimized efficiency of about 0.6% [19]. Unfortunately, the performance of photoelectrochemical (PEC) in these studies is poor and needs to be modified.

The synthesis of metal sulfide/metal oxide heterostructures has gained recognition due to their synergetic properties. However, research work on oxide/sulfide bilayer is limited. According to the literature, nanostructure synthesis of p-PbS/p-CuO double-layer thin film has not been reported yet for PEC activity. This study aims to address facile, low-cost, up-scalable techniques to provide a high J ph value as a measure of the H2 generation rate. The CuO, PbS, and p-PbS/p-CuO films were prepared using successive ionic-layer adsorption and reaction (SILAR) and chemical bath deposition (CBD) techniques on normal glass. The resulting p-PbS/p-CuO photoelectrode was used as a working electrode in a three-electrode cell for the H2 generation process through water splitting. This study investigated the impact of various factors, such as light wavelengths and intensities, pH of the medium, and scan rate, on the process.

2 Experimental part

2.1 Materials

Sigma-Aldrich provided sulfuric acid (H2SO4), copper chloride (CuCl2·2H2O), ammonia (NH3), lead nitrate (Pb(NO3)2), thiourea (CS(NH2)2), sodium hydroxide (NaOH), isopropanol (C3H8O), and sodium thiosulfate (Na2S2O3).

2.2 Synthesis of CuO thin film

A pure CuO thin film was created using the SILAR technique. First, a commercial glass substrate was cleaned by being immersed in H2SO4 for 25 min, then in C3H8O for 20 min, and finally in distilled water (DW) for 15 min. The SILAR process involved using 0.06 M CuCl2·2H2O as the cationic precursor. It was dissolved in 100 mL of DW and adjusted to pH ∼9 by adding a diluted NH3 solution (33%). Hot DW (80°C) was used as the anionic precursor.

The process involved four steps. In the first step, the cleaned substrate was immersed in the cationic precursor for 20 s, allowing complex copper NH3 [(Cu(NH3)4)2+] to adsorb onto the glass substrate. In the second step, the substrate was rinsed in DW at room temperature for 30 s, converting the adsorbed copper NH3 complex to copper hydroxide (Cu(OH)2). In the third step, ultrasonic agitation was used to remove any loosely bonded Cu(OH)2 molecules. In the final step, the Cu(OH)2-coated substrate was immersed in hot DW (80°C) for 20 s, converting the Cu(OH)2 to a solid CuO film. To obtain high-quality homogenous CuO thin films, 40 SILAR cycles were repeated. Finally, the films were annealed at 450°C for 2 h. The following equations represent the preparation steps:

(1) Cu Cl 2 + 2 H 2 O + 6 N H 3 → [ Cu ( N H 3 ) 4 ] 2 + + 2 N H 4 Cl + 2 O H − ,

(2) [ Cu ( N H 3 ) 4 ] 2 + + 4 H 2 O → Cu 2 + + 4 N H 4 + + 4 O H − ,

(3) Cu 2 + + 2 O H − → Cu ( OH ) 2 ,

(4) Cu ( OH ) 2 → 450 ° C CuO ( s ) + H 2 O .

2.3 Fabrication of PbS thin film

A PbS thin film was successfully fabricated on a commercial glass substrate using a simple CBD technique in a strongly alkaline medium. The deposition bath solution consisted of a mixture of 90 mL (0.010 M) of Pb(NO3)2, 90 mL (0.057 M) of CS(NH2)2, and 90 mL (0.146 M) of NaOH. The glass substrate was vertically immersed in the solution at room temperature and allowed to keep undisturbed for 1 h. As the deposition proceeded, the color of the bath solution gradually transitioned from colorless to brown and eventually to dark gray, indicating the successful formation of the PbS thin film. The reaction process for forming PbS film is considered as following equations [20]:

(5) Pb ( N O 3 ) 2 + 2 NaOH → Pb ( OH ) 2 + 2 NaN O 3 ,

(6) Pb ( OH ) 2 + 4 NaOH → Na 4 Pb ( OH ) 6 ,

(7) Na 4 Pb ( OH ) 6 → 4 N a + + HPb O 2 − + 3 O H − + H 2 O ,

(8) SC ( N H 2 ) 2 + 2 O H − → CH 2 N 2 + H 2 O + S H − ,

(9) HPb O 2 − + S H − → PbS + 2 O H − .

2.4 Fabrication of PbS/CuO bilayer

To fabricate PbS/CuO thin films, the same CBD technique is used for depositing the PbS layer onto the CuO/glass thin film. The CuO film, prepared earlier, was vertically placed into the deposition bath solution at room temperature and left undisturbed for 1 h, mirroring the procedure used for the PbS fabrication. Finally, the PbS/CuO thin films were thoroughly washed multiple times with deionized water (DW) and subsequently dried at room temperature.

2.5 Examination of samples

The crystal structures of the CuO, PbS, and p-PbS/p-CuO films were studied using an X-ray Empyrean Alpha diffractometer. To accurately analyze the chemical elements in the samples, energy-dispersive X-ray spectroscopy (EDAX; Oxford Link ISIS 300) was used. The structural morphology of the samples, including particle shape and diameter, was investigated using field emission scanning electron microscopy (FE-SEM; ZEISS SUPRA 55 VP and ZEISS LEO). The spectral absorbance of the samples was measured using a double-beam spectrophotometer (PerkinElmer, Lambda 950).

2.6 PEC measurements

The PEC measurements are taken using an OrigaFlex potentiostat in a three-electrode system. The working electrode was prepared using the PbS, CuO, and p-PbS/p-CuO films. The silver paste was used as an ohmic electrical contact. The counter electrode was made of platinum, and the reference electrode used was silver chloride (Ag/AgCl). The PEC measurements were taken using a three-electrode cell. The prepared film was used as the working electrode, a Pt electrode was used as the counter electrode, and an Ag/AgCl electrode was used as the reference electrode. The PEC measurements are taken in a 0.3 M Na2S2O3 solution under a solar simulator xenon lamp (100 mW cm−2). The selection of a xenon lamp is based on its ability to maintain a consistent intensity across the entire spectrum of wavelengths from 200 to 2,400 nm, encompassing UV to near-infrared (NIR) light. The spectrum for the xenon arc lamp is shown in Figure S1 (Supplementary Data).

The measurements included studying the effects of electrolyte pH, white light intensity, and temperature. The pH value was adjusted by adding a few drops of 0.1 M NaOH and HCl solutions to the electrolyte. Temperature control was achieved using a water bath during measurements. Additionally, the response of the p-PbS/p-CuO photoelectrode was measured under different monochromatic lights within the range of 390–636 nm. Monochromatic optical filters (Oriel) covering the range of 470–636 nm were placed in front of the xenon lamp to illuminate the electrochemical cell with various wavelengths.

The electrochemical measurements were taken by applying a voltage range of −1 V to +1 V vs Ag/AgCl with a sweep rate of 100 mV s−1, as illustrated in Figure 1. The measured potentials relative to Ag/AgCl were subsequently converted to the reversible hydrogen electrode (RHE) scale using the Nernst equation as follows:

(10) V RHE = V Ag / Agcl o + V Ag / AgCl + 0.059 × pH ,

where V Ag / Agcl o = 0.1976 V at 25°C and V Ag / AgCl is the applied potential.

Figure 1 Schematic diagram for the PEC H2 generation process, which was measured using a three-electrode cell.
Figure 1

Schematic diagram for the PEC H2 generation process, which was measured using a three-electrode cell.

3 Results and discussion

3.1 Optical, morphological, and structural properties

The optical properties of CuO, PbS, and p-PbS/p-CuO films were investigated. The absorbance of CuO and PbS films covered the UV and visible regions, while the absorbance of p-PbS/p-CuO nanomaterials was the sum of both absorbance behaviors as shown in Figure 2(a). The excellent absorbance for the p-PbS/p-CuO bilayer was due to the high optical properties of CuO and PbS, their black color, and narrow size distribution, which allowed for the collection of photons in both UV and visible regions [21].

Figure 2 Optical (a) absorbance and (b) bandgap values for CuO, PbS, and p-PbS/p-CuO films.
Figure 2

Optical (a) absorbance and (b) bandgap values for CuO, PbS, and p-PbS/p-CuO films.

Using film thickness (d), material absorption (A), and absorption coefficient (α), bandgap (E g) value was calculated based on Tauc equations (11) and (12) [22,23]:

(11) ( α h ν ) 2 = K ( h ν − E g ) ,

(12) α ( cm 2 ) = 2.303 d A ,

where K, h, and ν are constant, Planck constant (eV s), and photon frequency (Hz), respectively.

The p-PbS/p-CuO bilayer thin film exhibits a reduced bandgap (Eg) value of 1.28 eV, compared to the individual PbS (1.36 eV) and CuO (1.45 eV) films as shown in Figure 2(b). The reduced bandgap of the p-PbS/p-CuO bilayer thin film can be attributed to several reasons. The presence of interfaces and interfacial interactions between the PbS and CuO layers can modify the band structure and the electronic properties, leading to a lower bandgap in the bilayer thin film. Additionally, the junctions formed at the interface in the bilayer structure have an impact on the band alignment and electronic states. Furthermore, the reduced crystallite size of the bilayer thin film plays a role in lowering the bandgap according to quantum confinement effects.

Figure 3 (SEM images) displays the morphology of the prepared PbS, CuO, and p-PbS/p-CuO films. The PbS film contains a continuous layer of multi-shaped nano-stones that are coalescent and intergrown with each other. These nano-stones have a random distribution with irregular shapes and sizes. The CuO nanoparticles are agglomerated and have appendages extending over the particles. The particle size of CuO ranged between 50 and 70 nm. However, after the deposition of PbS, the particle size increases to an average of 150 nm. The coverage of PbS on CuO results in the formation of a non-uniform hexagonal shape with a more crystalline nature.

Figure 3 SEM images of (a) PbS, (b) CuO, and (c) p-PbS/p-CuO films.
Figure 3

SEM images of (a) PbS, (b) CuO, and (c) p-PbS/p-CuO films.

X-ray diffraction (XRD) analysis was used to examine the structural properties of the prepared films (CuO, PbS, and p-PbS/p-CuO), and the XRD patterns of the as-deposited films are shown in Figure 4. The XRD analysis revealed that all of the samples were poly-oriented. Eight peaks in the XRD lines indicate the monoclinic phase of CuO according to standard card #03-056-2309. CuO film shows a strong (002) diffraction peak located at 2θ = 39.89°. Seven distinct peaks for the cubic phase of PbS were observed based on standard cards # 04-002-0034 and 00-005-0592. Two main peaks are assigned to the (111) and (200) planes located at 125.98 and 29.67, respectively, with good crystallinity. PbS film shows a strong (111) diffraction peak located at 2θ = 25.89° with good crystallinity. There are eleven distinct peaks for the mixed phases of p-PbS/p-CuO as shown in Figure 4. The absence of any other XRD lines indicated the good quality of the fabricated films with no impurities.

Figure 4 XRD patterns of CuO, PbS, and p-PbS/p-CuO films.
Figure 4

XRD patterns of CuO, PbS, and p-PbS/p-CuO films.

The Williamson-Hall (W-H) model was used to calculate the average values of crystallite size (D) and microstrain (ɛ) for the films prepared using XRD data, as shown in Figure 5 and Table 1. This was done using the following equation [24,25,26]:

(13) β cos θ = 0.95 λ D + 4 ε sin θ ,

where 0.95 is the shape factor for a thin film sample, λ is the wavelength of the XRD (0.15418 nm), and β is the broadening of the diffraction lines in radian. The assumption was made that the materials studied have an isotropic character and that the micro-strain is uniform in all (hkl) possible orientations. The values of βcos θ on the y-axis were plotted against 4sin θ on the x-axis for each diffraction pattern. A linear regression analysis was conducted to determine the intercept and slope of the line (Figure 5). The intercept and slope of this line were used to calculate the crystallite size and micro-strain.

Figure 5 W-H plots of the investigated (a) CuO, (b) PbS, and (c) p-PbS/p-CuO films.
Figure 5

W-H plots of the investigated (a) CuO, (b) PbS, and (c) p-PbS/p-CuO films.

Table 1

XRD calculated parameters for the CuO, PbS, and p-PbS/p-CuO films

Sample Crystallite size (D) (nm) Micro-strain (ε) (10−3) Dislocation density (ρ) (1011 cm−2)
CuO 25.88 3.7 1.49
PbS 53.68 6.5 0.34
p-PbS/p-CuO 18.34 0.24 2.97

From Table 1, the crystallite size of the PbS, CuO, and p-PbS/p-CuO films is 53.68, 25.88, and 18.34 nm, respectively. The smaller crystallite size of the p-PbS/p-CuO double-layer thin film may also be due to the heteroepitaxial growth of PbS on CuO, which can cause lattice mismatch and strain. Lower crystallite size indicates high surface area for p-PbS/p-CuO film, which is very useful in the PEC application. The micro-strain is the root mean square of the variations in the lattice parameters across the sample. It depends on factors such as antiphase domain boundaries, non-uniform lattice distortions, grain surface relaxation, and faulting. These microstructural effects contribute to the shape profile of the diffraction peaks, resulting in line broadening and shift. In Table 1, it can be observed that the p-PbS/p-CuO double-layer thin film exhibits a lower micro-strain compared to individual CuO and PbS films.

Dislocation density (ρ) is defined as the number of dislocations in a crystalline thin film. Since dislocations are line defects, this is expressed as a ratio of the total length of the dislocation line to the volume of the crystal (L/L 3) in line centimeters squared (cm2). There is an opposite relationship between crystallite size and dislocation density. The dislocation density (ρ) of the prepared films was calculated using the following equation:

(14) ρ = 1 D 2 .

The presence of a higher dislocation density in the p-PbS/p-CuO structure, attributed to a reduced crystallite size, indicates an increased concentration of defects and a decrease in the crystallization quality when compared to individual PbS and CuO films.

Figure 6 shows the EDX spectrum of the PbS and CuO films. The EDX patterns showed the existence of Pb and S signals as the components of the synthetic PbS film as presented in Figure 6(a). The atomic ratio is approximately 44.43 and 55.57%, respectively. For CuO film, the EDX patterns indicated that there are only signals for Cu and O with atomic ratios of 37.35 and 62.65%, respectively. The peaks Cu and O are positioned around 0.93 and 0.52 keV, as illustrated in Figure 6(b). No impurities of elements were found within the detection limit of the EDX. This confirms the high purity of the deposited thin films, which is a coincidence with the XRD data.

Figure 6 EDX spectra for (a) PbS and (b) CuO films.
Figure 6

EDX spectra for (a) PbS and (b) CuO films.

3.2 Photoelectrode evaluation with the electrochemical tests

Figure 7 displays the PEC activity by measuring the voltage–current of CuO, PbS, and p-PbS/p-CuO photoelectrodes in dark and light conditions. The J ph values (photocurrent density) produced by the photoelectrodes are higher under light conditions than under dark conditions. The rate of H2 generation during water splitting is directly proportional to J ph. The value of the dark current (J o) of CuO is very small (6 µA cm−2) and is neglected because it is related to the semiconductor nature of the prepared nanomaterials [27]. The p-PbS/p-CuO photoelectrode had a J ph value of −0.39 mA cm−2, which is much higher than the values of −0.12 and −0.008 mA cm−2 for the PbS and CuO photoelectrodes, respectively.

Figure 7 Photocurrent–voltage characteristics (J ph–V) of CuO, PbS, and p-PbS/p-CuO photoelectrodes measured in dark and light conditions using a three-electrode system with a 0.3 M Na2S2O3 solution at pH 7 and 25°C, under a solar simulator xenon lamp (100 mW cm−2), with an applied voltage range of −0.35 to 0 V vs RHE and a sweep rate of 100 mV s−1.
Figure 7

Photocurrent–voltage characteristics (J ph–V) of CuO, PbS, and p-PbS/p-CuO photoelectrodes measured in dark and light conditions using a three-electrode system with a 0.3 M Na2S2O3 solution at pH 7 and 25°C, under a solar simulator xenon lamp (100 mW cm−2), with an applied voltage range of −0.35 to 0 V vs RHE and a sweep rate of 100 mV s−1.

The p-PbS/p-CuO bilayer photoelectrode exhibits enhanced PEC performance for H2 gas generation due to several advantages offered by the sulfide/oxide bilayer heterojunction. Optical data confirm that the p-PbS/p-CuO bilayer has higher light absorption than individual PbS and CuO layers. This enables efficient light absorption across a wide range of wavelengths, improving overall photoconversion efficiency. When illuminated, the bilayer structure facilitates the formation of electron–hole pairs with high density [28]. The energy-level difference between PbS and CuO within the bilayer allows these hot electrons to reach the water solution, promoting the H2 generation reaction. The p-p heterojunction formation between PbS and CuO aids in separating the electrons and holes, minimizing recombination, and enhancing charge transport [29,30]. This leads to increased photocurrent generation and improved H2 gas production. Furthermore, the heterojunction structure enhances the chemical stability of the photoelectrode surface, passivates surface recombination centers, and improves the catalytic activity. Additionally, the p-PbS/p-CuO bilayer is composed of low-cost materials and can be easily fabricated at low temperatures with various morphologies.

The effect of Na2S2O3 electrolyte pH on the water-splitting reaction was investigated at room temperature as presented in Figure 8(a). NaOH and HCl were used to adjust the pH from 3 to 12. The optimum J ph value of −0.39 mA cm−2 for the p-PbS/p-CuO photoelectrode was obtained at pH 7 (neutral). When the pH was increased to 12 or decreased to 3, the J ph values decreased to −0.14 and −0.06 mA cm−2, respectively. The decrease in J ph at pH 12 was due to electrode corrosion at this high pH, while the low J ph value at pH 3.5 was related to the dissolution of PbS or CuO in the acidic medium [31].

Figure 8 Effect of (a) pH of Na2S2O3 electrolyte and (b) temperature on the H2 generation reaction using a p-PbS/p-CuO photoelectrode in a three-electrode system under a solar simulator xenon lamp (100 mW cm−2), with an applied voltage range of −0.35 to 0 V vs RHE and a sweep rate of 100 mV s−1.
Figure 8

Effect of (a) pH of Na2S2O3 electrolyte and (b) temperature on the H2 generation reaction using a p-PbS/p-CuO photoelectrode in a three-electrode system under a solar simulator xenon lamp (100 mW cm−2), with an applied voltage range of −0.35 to 0 V vs RHE and a sweep rate of 100 mV s−1.

Figure 8(b) displays the effect of temperature on the water-splitting reaction for p-PbS/p-CuO bilayer photoelectrode in 0.3 M Na2S2O3 electrolyte at pH = 7. As the temperature increases, the produced J ph values increase, which confirms that the rate of H2 gas evolution increases. At an applied voltage of −0.39 V, the J ph values increase from 0.42 to 2.06 mA cm−2 with the increase in the temperature from 25 to 60°C, respectively. This behavior is related to increasing ion mobility with an increase in temperature.

Figure 9(a) shows the impact of light intensity (ranging from 25 to 100 mW cm−2) on the p-PbS/p-CuO photoelectrode. The value of J ph increases with an increase in light flux incidence. The values of J ph increased from −0.26 to −0.39 mA cm−2 under applied −0.34 V as the light power intensity increased from 25 to 100 mW cm−2, respectively. Based on equation (15), the number of photons (N) increases from 1.25 × 1021 to 8 × 1021 photon s−1 as the light intensity (P) increases from 12 to 100 mW cm−2, respectively. This equation relies on certain constants, such as Planck’s constant (h), light wavelength (λ), and velocity of light (c):

(15) N ( photon s − 1 ) = λ ( m ) P ( j s − 1 m − 2 ) h ( J s − 1 ) c ( m s − 1 ) .

Figure 9 Effect of (a) white light intensity and (b) different monochromatic wavelengths of intensity of 75 mW cm−2 on the H2 generation reaction using a p-PbS/p-CuO photoelectrode with a three-electrode system with a 0.3 M Na2S2O3 solution at pH 7 and 25°C under an applied voltage range of −0.35 to 0 V vs RHE and a sweep rate of 100 mV s−1.
Figure 9

Effect of (a) white light intensity and (b) different monochromatic wavelengths of intensity of 75 mW cm−2 on the H2 generation reaction using a p-PbS/p-CuO photoelectrode with a three-electrode system with a 0.3 M Na2S2O3 solution at pH 7 and 25°C under an applied voltage range of −0.35 to 0 V vs RHE and a sweep rate of 100 mV s−1.

The J ph values produced varied based on the light intensity, which indicates that the photoelectrode is responsive to photons. The high response of the p-PbS/p-CuO photoelectrode to light incidence can be attributed to the multi-electron transition properties of PbS nanomaterials [32]. With an increase in photon flux, more e–h pairs increase [33]. Consequently, this enhances the activation of surface sites on photoelectrode [34]. These results confirm that the rate of water splitting and H2 generation increases with increasing photon flux [35,36].

The impact of monochromatic light on the response of the p-PbS/p-CuO photoelectrode is explored within the 390–636 nm range as presented in Figure 9(b). The J ph values are observed to change from −0.290 to −0.248 mA cm−2 at 470 and 508 nm, respectively, then increasing to −0.258 mA cm−2 at 636 nm. The optimal J ph value is observed at 470 nm, which is attributed to the effect of high-energy light on the photoelectrode, capable of triggering electron transition within the prepared p-PbS/p-CuO photoelectrode. The excellent performance of the p-PbS/p-CuO photoelectrode lies in its ability to respond to a broad range of solar wavelengths, ranging from 470 to 636 nm, with high J ph values. The near-IR light at 636 nm is particularly effective at causing electron vibrations within the electrode materials. This wide range of light coverage ensures that the photoelectrode can facilitate water-splitting and H2 generation reactions across a broad spectrum of optical wavelengths.

To fully examine the PEC performance of the p-PbS/p-CuO photoelectrode, the incident photon-to-current (IPCE%) and applied-bias-to-photon (ABPE%) conversion efficiencies were estimated [37,38]. The IPCE and ABPE can be calculated using the illuminating light power density (P, mW cm−2), the wavelength (λ, nm) of the monochromatic light, the applied potential (V app, V), and photocurrent density (J ph, mA cm−2) according to the following equations:

(16) IPCE ( % ) = J ph ( mA cm − 2 ) 1 , 240 λ ( nm ) P ( mW cm − 2 ) × 100 ,

(17) ABPE ( % ) = J ph ( mA cm − 2 ) . ( 1.23 − V app ) P ( mW cm − 2 ) × 100 .

The p-PbS/p-CuO electrode has optimum IPCE and ABPE values of 2.1 and 0.46%, respectively. These results indicate good performance PEC activity of the p-PbS/p-CuO bilayer film.

Figure 10(a) displays the chronoamperometry J ph–t response of p-PbS/p-CuO photoelectrode. Initially, the photocurrent densities rapidly decline. Then, the current density value becomes stable at 0.270 mA cm−2 because of the increase in the accumulation of the ionic charges. From the J ph–t curve, the produced H2 moles is revealed by the following equation [39]:

(18) H 2 ( moles ) = 1 F ∫ 0 t J ph d t ,

where F = 96,500 C mol−1 is the Faraday constant. The H2 generation increased sharply with time reaction as seen in Figure 10(b). The H2 output rate of approximately p-PbS/p-CuO photoelectrode versus the production time was calculated per unit active area to be 40.23 μmol s−1 cm−2.

Figure 10 (a) Chronoamperometry J ph–t response of p-PbS/p-CuO photoelectrode and (b) calculated number of H2 moles through p-PbS/p-CuO photoelectrode using a three-electrode system with a 0.3 M Na2S2O3 solution at pH 7 under a solar simulator xenon lamp (100 mW cm−2) with a sweep rate of 100 mV s−1.
Figure 10

(a) Chronoamperometry J ph–t response of p-PbS/p-CuO photoelectrode and (b) calculated number of H2 moles through p-PbS/p-CuO photoelectrode using a three-electrode system with a 0.3 M Na2S2O3 solution at pH 7 under a solar simulator xenon lamp (100 mW cm−2) with a sweep rate of 100 mV s−1.

Table 2 compares the amount of H2 gas produced by the p-PbS/p-CuO photoelectrode in this study with previous literature. The results show that the photoelectrode prepared in this study has a high efficiency in producing H2 gas compared to many other reported materials. This confirms the great potential of the p-PbS/p-CuO photoelectrode in the field of photocatalysis and renewable energy production.

Table 2

Comparison of this study results with the previous literature

Photoelectrode Electrolyte J ph (mA cm−2) Efficiency Reference
g-C3N4/CuO NaOH 0.01 — [12]
CuO-C/TiO2 Glycerol 0.012 — [13]
TiN/TiO2 NaOH 3.0 × 10−4 IPCE = 0.03% [40]
BiFeO3 NaOH 0.1 — [41]
Au/Pb(Zr, Ti)O3 NaOH 0.06 IPCE = 0.50% [42]
Si/ZnO Na2SO4 0.5 ABPE = 0.035% [43]
ZnO/Au/Al2O3 Na2SO4 0.55 IPCE = 0.70% [44]
CdSe/TiO2 NaOH 0.13 IPCE = 0.45 [45]
Fe-ZnO Na2S2O3 0.56 IPCE = 1.45%, ABPE = 0.20% [46]
p-PbS/p-CuO Na2S2O3 −0.39 IPCE = 2.1% and ABPE = 0.46% Present work

3.3 Mechanism of p-PbS/p-CuO heterojunction

The photocatalytic technique is reliant on the creation of photocarrier e–h pairs under light excitation. The quantity of light absorbed determines the PEC’s activity, which confirms the existence of e–h pairs and the separation of the charge carriers. Figure 11 illustrates the schematic diagram of the p-PbS/p-CuO structure according to the Anderson model. From Figure 2(b), the energy gaps of PbS and CuO are 1.36 and 1.45 eV, respectively. The electron affinities (χ) of PbS and CuO are 3.5 and 4.07 eV, respectively, [47,48]. The work functions (φ) of PbS and CuO are 4.34 and 5.20 eV, respectively [49,50]. The conduction band (CB) discontinuity and the valence band (VB) discontinuity are calculated according to the following relations [51]:

(19) Δ E c = χ PbS − χ CuO = 3.5 − 4.07 = − 0.57 eV ,

(20) Δ E v = E gpbs − E g Cuo + Δ E c = 1.36 − 1.45 − 0.57 = − 0.66 eV .

Figure 11 Energy band diagram of (a) isolated PbS and CuO and (b) p-PbS/p-CuO heterojunction.
Figure 11

Energy band diagram of (a) isolated PbS and CuO and (b) p-PbS/p-CuO heterojunction.

After photon absorption of the semiconductor (PbS or CuO), the electrons jumped to the CB from the VB, leaving positive holes in the VB. For the p-PbS/p-CuO bilayer, high absorbance in the visible range of the solar spectrum helps in the creation of a large number of e−/h+ pairs under light more than in pristine PbS or CuO thin films. Both the PbS and CuO films were p-type semiconductors and possess different energy levels from their corresponding VB and CB, which create heterojunction systems. The valence (E v) and conduction (E c) bands of CuO are lower than those of PbS. Thus, the charge transfer is formed at the interface between PbS and CuO, leading to the formation of heterojunction at the interface of p-PbS/p-CuO bilayer. A heterojunction is an interface between two layers of dissimilar semiconductors. The heterojunction layers offer many advantages such as fast photo-generated carrier separation, holding multiple bandgaps for better matching the solar spectrum, enhancing the chemical stability, passivating the surface recombination centers, and improving the catalytic activity of the photoelectrode surface [52]. It is useful in applications, including solar cells, photocatalytic, transistors, and lasers. The photoexcited electrons in PbS may migrate to the CB of CuO, while the photo-generated holes are left in the VB of PbS [53,54].

This way prevents the e–h recombination, which helps in the continuous electron flow and leads to photocurrent generation. Consequently, the band disposition of the p-PbS/p-CuO bilayer film facilitates the separation and transportation of photo-induced charged carriers, leading to its elevated photocatalytic activity. The photogenerated electron–hole moved to the surface of the semiconductor, to react with the electrolyte and generate H2 gas as described in equations (21)–(23). The oxygen evolution reaction (equation (22)) occurs at the anode, while the H2 evolution reaction (equation (23)) takes place at the cathode [55]:

(21) PbS / CuO + h ν → PbS / CuO ( e − CB + h + VB ) ,

(22) h + + H 2 O → 1 2 O 2 + 2 H + ,

(23) 2 e − + 2 H + → H 2 .

4 Conclusion

This study demonstrates the potential of p-PbS/p-CuO bilayer films as a photoelectrode for H2 generation through water splitting. The film’s structure was characterized using various analytical techniques, confirming its high crystallinity and an average particle size of 18.2 nm. The photoelectrode exhibited a small bandgap of 1.28 eV and demonstrated effective performance in a wide range of optical wavelengths, including UV, visible, and near-IR. The particle size of the p-PbS/p-CuO bilayer was non-uniform and had an average size of 150 nm with a hexagonal shape. The J ph values were observed to increase with increasing light power intensity, and the electrode exhibited a high response to a wide range of optical wavelengths in the UV, visible, and IR regions.

Acknowledgments

This work was supported and funded by the Deanship of Scientific Research at Imam Mohammad Ibn Saud Islamic University (IMSIU) (grant number IMSIU-RG23130).

  1. Author contributions: Mohamed Zayed: conceptualization, methodology, formal analysis, investigation, and writing. Ashour M. Ahmed, Mamduh J. Aljaafreh, and Mohamed Rabia: conceptualization, methodology, formal analysis, investigation, and writing – review and editing. Mohamed Shaban: methodology, investigation, formal analysis. Sodky H. Mohamed, Mahmoud Hezam, Mohammad Marashdeh, and M. Al-Hmoud: validation and formal analysis.

  2. Conflict of interest: The authors declare that they have no conflict of interest.

  3. Ethical approval: The conducted research is not related to either human or animal use.

  4. Data availability statement: The datasets generated during and/or analyzed during this study are available from the corresponding author on a reasonable request.

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Received: 2023-10-17
Revised: 2023-11-25
Accepted: 2023-12-11
Published Online: 2023-12-31

© 2023 the author(s), published by De Gruyter

This work is licensed under the Creative Commons Attribution 4.0 International License.

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  71. Exploring the antimicrobial potential of biologically synthesized zero valent iron nanoparticles
  72. NaCl regulates goldfish growth and survival at three food supply levels under hypoxia
  73. An exploration of the physical, optical, mechanical, and radiation shielding properties of PbO–MgO–ZnO–B2O3 glasses
  74. A novel statistical modeling of air pollution and the COVID-19 pandemic mortality data by Poisson, geometric, and negative binomial regression models with fixed and random effects
  75. Treatment activity of the injectable hydrogels loaded with dexamethasone In(iii) complex on glioma by inhibiting the VEGF signaling pathway
  76. An alternative approach for the excess lifetime cancer risk and prediction of radiological parameters
  77. Panax ginseng leaf aqueous extract mediated green synthesis of AgNPs under ultrasound condition and investigation of its anti-lung adenocarcinoma effects
  78. Study of hydrolysis and production of instant ginger (Zingiber officinale) tea
  79. Novel green synthesis of zinc oxide nanoparticles using Salvia rosmarinus extract for treatment of human lung cancer
  80. Evaluation of second trimester plasma lipoxin A4, VEGFR-1, IL-6, and TNF-α levels in pregnant women with gestational diabetes mellitus
  81. Antidiabetic, antioxidant and cytotoxicity activities of ortho- and para-substituted Schiff bases derived from metformin hydrochloride: Validation by molecular docking and in silico ADME studies
  82. Antioxidant, antidiabetic, antiglaucoma, and anticholinergic effects of Tayfi grape (Vitis vinifera): A phytochemical screening by LC-MS/MS analysis
  83. Identification of genetic polymorphisms in the stearoyl CoA desaturase gene and its association with milk quality traits in Najdi sheep
  84. Cold-acclimation effect on cadmium absorption and biosynthesis of polyphenolics, and free proline and photosynthetic pigments in Spirogyra aequinoctialis
  85. Analysis of secondary metabolites in Xinjiang Morus nigra leaves using different extraction methods with UPLC-Q/TOF-MS/MS technology
  86. Nanoarchitectonics and performance evaluation of a Fe3O4-stabilized Pickering emulsion-type differential pressure plugging agent
  87. Investigating pyrolysis characteristics of Shengdong coal through Py-GC/MS
  88. Extraction, phytochemical characterization, and antifungal activity of Salvia rosmarinus extract
  89. Introducing a novel and natural antibiotic for the treatment of oral pathogens: Abelmoschus esculentus green-formulated silver nanoparticles
  90. Optimization of gallic acid-enriched ultrasonic-assisted extraction from mango peels
  91. Effect of gamma rays irradiation in the structure, optical, and electrical properties of samarium doped bismuth titanate ceramics
  92. Combinatory in silico investigation for potential inhibitors from Curcuma sahuynhensis Škorničk. & N.S. Lý volatile phytoconstituents against influenza A hemagglutinin, SARS-CoV-2 main protease, and Omicron-variant spike protein
  93. Physical, mechanical, and gamma ray shielding properties of the Bi2O3–BaO–B2O3–ZnO–As2O3–MgO–Na2O glass system
  94. Twofold interpenetrated 3D Cd(ii) complex: Crystal structure and luminescent property
  95. Study on the microstructure and soil quality variation of composite soil with soft rock and sand
  96. Ancient spring waters still emerging and accessible in the Roman Forum area: Chemical–physical and microbiological characterization
  97. Extraction and characterization of type I collagen from scales of Mexican Biajaiba fish
  98. Finding small molecular compounds to decrease trimethylamine oxide levels in atherosclerosis by virtual screening
  99. Prefatory in silico studies and in vitro insecticidal effect of Nigella sativa (L.) essential oil and its active compound (carvacrol) against the Callosobruchus maculatus adults (Fab), a major pest of chickpea
  100. Polymerized methyl imidazole silver bromide (CH3C6H5AgBr)6: Synthesis, crystal structures, and catalytic activity
  101. Using calcined waste fish bones as a green solid catalyst for biodiesel production from date seed oil
  102. Influence of the addition of WO3 on TeO2–Na2O glass systems in view of the feature of mechanical, optical, and photon attenuation
  103. Naringin ameliorates 5-fluorouracil elicited neurotoxicity by curtailing oxidative stress and iNOS/NF-ĸB/caspase-3 pathway
  104. GC-MS profile of extracts of an endophytic fungus Alternaria and evaluation of its anticancer and antibacterial potentialities
  105. Green synthesis, chemical characterization, and antioxidant and anti-colorectal cancer effects of vanadium nanoparticles
  106. Determination of caffeine content in coffee drinks prepared in some coffee shops in the local market in Jeddah City, Saudi Arabia
  107. A new 3D supramolecular Cu(ii) framework: Crystal structure and photocatalytic characteristics
  108. Bordeaux mixture accelerates ripening, delays senescence, and promotes metabolite accumulation in jujube fruit
  109. Important application value of injectable hydrogels loaded with omeprazole Schiff base complex in the treatment of pancreatitis
  110. Color tunable benzothiadiazole-based small molecules for lightening applications
  111. Investigation of structural, dielectric, impedance, and mechanical properties of hydroxyapatite-modified barium titanate composites for biomedical applications
  112. Metal gel particles loaded with epidermal cell growth factor promote skin wound repair mechanism by regulating miRNA
  113. In vitro exploration of Hypsizygus ulmarius (Bull.) mushroom fruiting bodies: Potential antidiabetic and anti-inflammatory agent
  114. Alteration in the molecular structure of the adenine base exposed to gamma irradiation: An ESR study
  115. Comprehensive study of optical, thermal, and gamma-ray shielding properties of Bi2O3–ZnO–PbO–B2O3 glasses
  116. Lewis acids as co-catalysts in Pd-based catalyzed systems of the octene-1 hydroethoxycarbonylation reaction
  117. Synthesis, Hirshfeld surface analysis, thermal, and selective α-glucosidase inhibitory studies of Schiff base transition metal complexes
  118. Protective properties of AgNPs green-synthesized by Abelmoschus esculentus on retinal damage on the virtue of its anti-inflammatory and antioxidant effects in diabetic rat
  119. Effects of green decorated AgNPs on lignin-modified magnetic nanoparticles mediated by Cydonia on cecal ligation and puncture-induced sepsis
  120. Treatment of gastric cancer by green mediated silver nanoparticles using Pistacia atlantica bark aqueous extract
  121. Preparation of newly developed porcelain ceramics containing WO3 nanoparticles for radiation shielding applications
  122. Utilization of computational methods for the identification of new natural inhibitors of human neutrophil elastase in inflammation therapy
  123. Some anticancer agents as effective glutathione S-transferase (GST) inhibitors
  124. Clay-based bricks’ rich illite mineral for gamma-ray shielding applications: An experimental evaluation of the effect of pressure rates on gamma-ray attenuation parameters
  125. Stability kinetics of orevactaene pigments produced by Epicoccum nigrum in solid-state fermentation
  126. Treatment of denture stomatitis using iron nanoparticles green-synthesized by Silybum marianum extract
  127. Characterization and antioxidant potential of white mustard (Brassica hirta) leaf extract and stabilization of sunflower oil
  128. Characteristics of Langmuir monomolecular monolayers formed by the novel oil blends
  129. Strategies for optimizing the single GdSrFeO4 phase synthesis
  130. Oleic acid and linoleic acid nanosomes boost immunity and provoke cell death via the upregulation of beta-defensin-4 at genetic and epigenetic levels
  131. Unraveling the therapeutic potential of Bombax ceiba roots: A comprehensive study of chemical composition, heavy metal content, antibacterial activity, and in silico analysis
  132. Green synthesis of AgNPs using plant extract and investigation of its anti-human colorectal cancer application
  133. The adsorption of naproxen on adsorbents obtained from pepper stalk extract by green synthesis
  134. Treatment of gastric cancer by silver nanoparticles encapsulated by chitosan polymers mediated by Pistacia atlantica extract under ultrasound condition
  135. In vitro protective and anti-inflammatory effects of Capparis spinosa and its flavonoids profile
  136. Wear and corrosion behavior of TiC and WC coatings deposited on high-speed steels by electro-spark deposition
  137. Therapeutic effects of green-formulated gold nanoparticles by Origanum majorana on spinal cord injury in rats
  138. Melanin antibacterial activity of two new strains, SN1 and SN2, of Exophiala phaeomuriformis against five human pathogens
  139. Evaluation of the analgesic and anesthetic properties of silver nanoparticles supported over biodegradable acacia gum-modified magnetic nanoparticles
  140. Review Articles
  141. Role and mechanism of fruit waste polyphenols in diabetes management
  142. A comprehensive review of non-alkaloidal metabolites from the subfamily Amaryllidoideae (Amaryllidaceae)
  143. Discovery of the chemical constituents, structural characteristics, and pharmacological functions of Chinese caterpillar fungus
  144. Eco-friendly green approach of nickel oxide nanoparticles for biomedical applications
  145. Advances in the pharmaceutical research of curcumin for oral administration
  146. Rapid Communication
  147. Determination of the contents of bioactive compounds in St. John’s wort (Hypericum perforatum): Comparison of commercial and wild samples
  148. Retraction
  149. Retraction of “Two mixed-ligand coordination polymers based on 2,5-thiophenedicarboxylic acid and flexible N-donor ligands: The protective effect on periodontitis via reducing the release of IL-1β and TNF-α”
  150. Topical Issue on Phytochemicals, biological and toxicological analysis of aromatic medicinal plants
  151. Anti-plasmodial potential of selected medicinal plants and a compound Atropine isolated from Eucalyptus obliqua
  152. Anthocyanin extract from black rice attenuates chronic inflammation in DSS-induced colitis mouse model by modulating the gut microbiota
  153. Evaluation of antibiofilm and cytotoxicity effect of Rumex vesicarius methanol extract
  154. Chemical compositions of Litsea umbellata and inhibition activities
  155. Green synthesis, characterization of silver nanoparticles using Rhynchosia capitata leaf extract and their biological activities
  156. GC-MS analysis and antibacterial activities of some plants belonging to the genus Euphorbia on selected bacterial isolates
  157. The abrogative effect of propolis on acrylamide-induced toxicity in male albino rats: Histological study
  158. A phytoconstituent 6-aminoflavone ameliorates lipopolysaccharide-induced oxidative stress mediated synapse and memory dysfunction via p-Akt/NF-kB pathway in albino mice
  159. Anti-diabetic potentials of Sorbaria tomentosa Lindl. Rehder: Phytochemistry (GC-MS analysis), α-amylase, α-glucosidase inhibitory, in vivo hypoglycemic, and biochemical analysis
  160. Assessment of cytotoxic and apoptotic activities of the Cassia angustifolia aqueous extract against SW480 colon cancer
  161. Biochemical analysis, antioxidant, and antibacterial efficacy of the bee propolis extract (Hymenoptera: Apis mellifera) against Staphylococcus aureus-induced infection in BALB/c mice: In vitro and in vivo study
  162. Assessment of essential elements and heavy metals in Saudi Arabian rice samples underwent various processing methods
  163. Two new compounds from leaves of Capparis dongvanensis (Sy, B. H. Quang & D. V. Hai) and inhibition activities
  164. Hydroxyquinoline sulfanilamide ameliorates STZ-induced hyperglycemia-mediated amyleoid beta burden and memory impairment in adult mice
  165. An automated reading of semi-quantitative hemagglutination results in microplates: Micro-assay for plant lectins
  166. Inductively coupled plasma mass spectrometry assessment of essential and toxic trace elements in traditional spices consumed by the population of the Middle Eastern region in their recipes
  167. Phytochemical analysis and anticancer activity of the Pithecellobium dulce seed extract in colorectal cancer cells
  168. Impact of climatic disturbances on the chemical compositions and metabolites of Salvia officinalis
  169. Physicochemical characterization, antioxidant and antifungal activities of essential oils of Urginea maritima and Allium sativum
  170. Phytochemical analysis and antifungal efficiency of Origanum majorana extracts against some phytopathogenic fungi causing tomato damping-off diseases
  171. Special Issue on 4th IC3PE
  172. Graphene quantum dots: A comprehensive overview
  173. Studies on the intercalation of calcium–aluminium layered double hydroxide-MCPA and its controlled release mechanism as a potential green herbicide
  174. Synergetic effect of adsorption and photocatalysis by zinc ferrite-anchored graphitic carbon nitride nanosheet for the removal of ciprofloxacin under visible light irradiation
  175. Exploring anticancer activity of the Indonesian guava leaf (Psidium guajava L.) fraction on various human cancer cell lines in an in vitro cell-based approach
  176. The comparison of gold extraction methods from the rock using thiourea and thiosulfate
  177. Special Issue on Marine environmental sciences and significance of the multidisciplinary approaches
  178. Sorption of alkylphenols and estrogens on microplastics in marine conditions
  179. Cytotoxic ketosteroids from the Red Sea soft coral Dendronephthya sp.
  180. Antibacterial and biofilm prevention metabolites from Acanthophora spicifera
  181. Characteristics, source, and health risk assessment of aerosol polyaromatic hydrocarbons in the rural and urban regions of western Saudi Arabia
  182. Special Issue on Advanced Nanomaterials for Energy, Environmental and Biological Applications - Part II
  183. Green synthesis, characterization, and evaluation of antibacterial activities of cobalt nanoparticles produced by marine fungal species Periconia prolifica
  184. Combustion-mediated sol–gel preparation of cobalt-doped ZnO nanohybrids for the degradation of acid red and antibacterial performance
  185. Perinatal supplementation with selenium nanoparticles modified with ascorbic acid improves hepatotoxicity in rat gestational diabetes
  186. Evaluation and chemical characterization of bioactive secondary metabolites from endophytic fungi associated with the ethnomedicinal plant Bergenia ciliata
  187. Enhancing photovoltaic efficiency with SQI-Br and SQI-I sensitizers: A comparative analysis
  188. Nanostructured p-PbS/p-CuO sulfide/oxide bilayer heterojunction as a promising photoelectrode for hydrogen gas generation
https://doi.org/10.1515/chem-2023-0177
Keywords for this article
CuO; PbS; p-PbS/p-CuO bilayer; photocatalyst; water splitting; H2 generation
Creative Commons
BY 4.0

Articles in the same Issue

  1. Characteristics, source, and health risk assessment of aerosol polyaromatic hydrocarbons in the rural and urban regions of western Saudi Arabia
  2. Regular Articles
  3. A network-based correlation research between element electronegativity and node importance
  4. Pomegranate attenuates kidney injury in cyclosporine-induced nephrotoxicity in rats by suppressing oxidative stress
  5. Ab initio study of fundamental properties of XInO3 (X = K, Rb, Cs) perovskites
  6. Responses of feldspathic sandstone and sand-reconstituted soil C and N to freeze–thaw cycles
  7. Robust fractional control based on high gain observers design (RNFC) for a Spirulina maxima culture interfaced with an advanced oxidation process
  8. Study on arsenic speciation and redistribution mechanism in Lonicera japonica plants via synchrotron techniques
  9. Optimization of machining Nilo 36 superalloy parameters in turning operation
  10. Vacuum impregnation pre-treatment: A novel method for incorporating mono- and divalent cations into potato strips to reduce the acrylamide formation in French fries
  11. Characterization of effective constituents in Acanthopanax senticosus fruit for blood deficiency syndrome based on the chinmedomics strategy
  12. Comparative analysis of the metabolites in Pinellia ternata from two producing regions using ultra-high-performance liquid chromatography–electrospray ionization–tandem mass spectrometry
  13. The assessment of environmental parameter along the desalination plants in the Kingdom of Saudi Arabia
  14. Effects of harpin and carbendazim on antioxidant accumulation in young jujube leaves
  15. The effects of in ovo injected with sodium borate on hatching performance and small intestine morphology in broiler chicks
  16. Optimization of cutting forces and surface roughness via ANOVA and grey relational analysis in machining of In718
  17. Essential oils of Origanum compactum Benth: Chemical characterization, in vitro, in silico, antioxidant, and antibacterial activities
  18. Translocation of tungsten(vi) oxide/gadolinium(iii) fluoride in tellurite glasses towards improvement of gamma-ray attenuation features in high-density glass shields
  19. Mechanical properties, elastic moduli, and gamma ray attenuation competencies of some TeO2–WO3–GdF3 glasses: Tailoring WO3–GdF3 substitution toward optimum behavioral state range
  20. Comparison between the CIDR or sponge with hormone injection to induce estrus synchronization for twining and sex preselection in Naimi sheep
  21. Exergetic performance analyses of three different cogeneration plants
  22. Psoralea corylifolia (babchi) seeds enhance proliferation of normal human cultured melanocytes: GC–MS profiling and biological investigation
  23. A novel electrochemical micro-titration method for quantitative evaluation of the DPPH free radical scavenging capacity of caffeic acid
  24. Comparative study between supported bimetallic catalysts for nitrate remediation in water
  25. Persicaline, an alkaloid from Salvadora persica, inhibits proliferation and induces apoptosis and cell-cycle arrest in MCF-7 cells
  26. Determination of nicotine content in locally produced smokeless tobacco (Shammah) samples from Jazan region of Saudi Arabia using a convenient HPLC-MS/MS method
  27. Changes in oxidative stress markers in pediatric burn injury over a 1-week period
  28. Integrated geophysical techniques applied for petroleum basins structural characterization in the central part of the Western Desert, Egypt
  29. The impact of chemical modifications on gamma-ray attenuation properties of some WO3-reinforced tellurite glasses
  30. Microwave and Cs+-assisted chemo selective reaction protocol for synthesizing 2-styryl quinoline biorelevant molecules
  31. Structural, physical, and radiation absorption properties of a significant nuclear power plant component: A comparison between REX-734 and 316L SS austenitic stainless steels
  32. Effect of Moringa oleifera on serum YKL-40 level: In vivo rat periodontitis model
  33. Investigating the impact of CO2 emissions on the COVID-19 pandemic by generalized linear mixed model approach with inverse Gaussian and gamma distributions
  34. Influence of WO3 content on gamma rays attenuation characteristics of phosphate glasses at low energy range
  35. Study on CO2 absorption performance of ternary DES formed based on DEA as promoting factor
  36. Performance analyses of detonation engine cogeneration cycles
  37. Sterols from Centaurea pumilio L. with cell proliferative activity: In vitro and in silico studies
  38. Untargeted metabolomics revealing changes in aroma substances in flue-cured tobacco
  39. Effect of pumpkin enriched with calcium lactate on iron status in an animal model of postmenopausal osteoporosis
  40. Energy consumption, mechanical and metallographic properties of cryogenically treated tool steels
  41. Optimization of ultra-high pressure-assisted extraction of total phenols from Eucommia ulmoides leaves by response surface methodology
  42. Harpin enhances antioxidant nutrient accumulation and decreases enzymatic browning in stored soybean sprouts
  43. Physicochemical and biological properties of carvacrol
  44. Radix puerariae in the treatment of diabetic nephropathy: A network pharmacology analysis and experimental validation
  45. Anti-Alzheimer, antioxidants, glucose-6-phosphate dehydrogenase effects of Taverniera glabra mediated ZnO and Fe2O3 nanoparticles in alloxan-induced diabetic rats
  46. Experimental study on photocatalytic CO2 reduction performance of ZnS/CdS-TiO2 nanotube array thin films
  47. Epoxy-reinforced heavy metal oxides for gamma ray shielding purposes
  48. Black mulberry (Morus nigra L.) fruits: As a medicinal plant rich in human health-promoting compounds
  49. Promising antioxidant and antimicrobial effects of essential oils extracted from fruits of Juniperus thurifera: In vitro and in silico investigations
  50. Chloramine-T-induced oxidation of Rizatriptan Benzoate: An integral chemical and spectroscopic study of products, mechanisms and kinetics
  51. Study on antioxidant and antimicrobial potential of chemically profiled essential oils extracted from Juniperus phoenicea (L.) by use of in vitro and in silico approaches
  52. Screening and characterization of fungal taxol-producing endophytic fungi for evaluation of antimicrobial and anticancer activities
  53. Mineral composition, principal polyphenolic components, and evaluation of the anti-inflammatory, analgesic, and antioxidant properties of Cytisus villosus Pourr leaf extracts
  54. In vitro antiproliferative efficacy of Annona muricata seed and fruit extracts on several cancer cell lines
  55. An experimental study for chemical characterization of artificial anterior cruciate ligament with coated chitosan as biomaterial
  56. Prevalence of residual risks of the transfusion-transmitted infections in Riyadh hospitals: A two-year retrospective study
  57. Computational and experimental investigation of antibacterial and antifungal properties of Nicotiana tabacum extracts
  58. Reinforcement of cementitious mortars with hemp fibers and shives
  59. X-ray shielding properties of bismuth-borate glass doped with rare earth ions
  60. Green supported silver nanoparticles over modified reduced graphene oxide: Investigation of its antioxidant and anti-ovarian cancer effects
  61. Orthogonal synthesis of a versatile building block for dual functionalization of targeting vectors
  62. Thymbra spicata leaf extract driven biogenic synthesis of Au/Fe3O4 nanocomposite and its bio-application in the treatment of different types of leukemia
  63. The role of Ag2O incorporation in nuclear radiation shielding behaviors of the Li2O–Pb3O4–SiO2 glass system: A multi-step characterization study
  64. A stimuli-responsive in situ spray hydrogel co-loaded with naringenin and gentamicin for chronic wounds
  65. Assessment of the impact of γ-irradiation on the piperine content and microbial quality of black pepper
  66. Antioxidant, sensory, and functional properties of low-alcoholic IPA beer with Pinus sylvestris L. shoots addition fermented using unconventional yeast
  67. Screening and optimization of extracellular pectinase produced by Bacillus thuringiensis SH7
  68. Determination of polyphenols in Chinese jujube using ultra-performance liquid chromatography–mass spectrometry
  69. Synergistic effects of harpin and NaCl in determining soybean sprout quality under non-sterile conditions
  70. Field evaluation of different eco-friendly alternative control methods against Panonychus citri [Acari: Tetranychidae] spider mite and its predators in citrus orchards
  71. Exploring the antimicrobial potential of biologically synthesized zero valent iron nanoparticles
  72. NaCl regulates goldfish growth and survival at three food supply levels under hypoxia
  73. An exploration of the physical, optical, mechanical, and radiation shielding properties of PbO–MgO–ZnO–B2O3 glasses
  74. A novel statistical modeling of air pollution and the COVID-19 pandemic mortality data by Poisson, geometric, and negative binomial regression models with fixed and random effects
  75. Treatment activity of the injectable hydrogels loaded with dexamethasone In(iii) complex on glioma by inhibiting the VEGF signaling pathway
  76. An alternative approach for the excess lifetime cancer risk and prediction of radiological parameters
  77. Panax ginseng leaf aqueous extract mediated green synthesis of AgNPs under ultrasound condition and investigation of its anti-lung adenocarcinoma effects
  78. Study of hydrolysis and production of instant ginger (Zingiber officinale) tea
  79. Novel green synthesis of zinc oxide nanoparticles using Salvia rosmarinus extract for treatment of human lung cancer
  80. Evaluation of second trimester plasma lipoxin A4, VEGFR-1, IL-6, and TNF-α levels in pregnant women with gestational diabetes mellitus
  81. Antidiabetic, antioxidant and cytotoxicity activities of ortho- and para-substituted Schiff bases derived from metformin hydrochloride: Validation by molecular docking and in silico ADME studies
  82. Antioxidant, antidiabetic, antiglaucoma, and anticholinergic effects of Tayfi grape (Vitis vinifera): A phytochemical screening by LC-MS/MS analysis
  83. Identification of genetic polymorphisms in the stearoyl CoA desaturase gene and its association with milk quality traits in Najdi sheep
  84. Cold-acclimation effect on cadmium absorption and biosynthesis of polyphenolics, and free proline and photosynthetic pigments in Spirogyra aequinoctialis
  85. Analysis of secondary metabolites in Xinjiang Morus nigra leaves using different extraction methods with UPLC-Q/TOF-MS/MS technology
  86. Nanoarchitectonics and performance evaluation of a Fe3O4-stabilized Pickering emulsion-type differential pressure plugging agent
  87. Investigating pyrolysis characteristics of Shengdong coal through Py-GC/MS
  88. Extraction, phytochemical characterization, and antifungal activity of Salvia rosmarinus extract
  89. Introducing a novel and natural antibiotic for the treatment of oral pathogens: Abelmoschus esculentus green-formulated silver nanoparticles
  90. Optimization of gallic acid-enriched ultrasonic-assisted extraction from mango peels
  91. Effect of gamma rays irradiation in the structure, optical, and electrical properties of samarium doped bismuth titanate ceramics
  92. Combinatory in silico investigation for potential inhibitors from Curcuma sahuynhensis Škorničk. & N.S. Lý volatile phytoconstituents against influenza A hemagglutinin, SARS-CoV-2 main protease, and Omicron-variant spike protein
  93. Physical, mechanical, and gamma ray shielding properties of the Bi2O3–BaO–B2O3–ZnO–As2O3–MgO–Na2O glass system
  94. Twofold interpenetrated 3D Cd(ii) complex: Crystal structure and luminescent property
  95. Study on the microstructure and soil quality variation of composite soil with soft rock and sand
  96. Ancient spring waters still emerging and accessible in the Roman Forum area: Chemical–physical and microbiological characterization
  97. Extraction and characterization of type I collagen from scales of Mexican Biajaiba fish
  98. Finding small molecular compounds to decrease trimethylamine oxide levels in atherosclerosis by virtual screening
  99. Prefatory in silico studies and in vitro insecticidal effect of Nigella sativa (L.) essential oil and its active compound (carvacrol) against the Callosobruchus maculatus adults (Fab), a major pest of chickpea
  100. Polymerized methyl imidazole silver bromide (CH3C6H5AgBr)6: Synthesis, crystal structures, and catalytic activity
  101. Using calcined waste fish bones as a green solid catalyst for biodiesel production from date seed oil
  102. Influence of the addition of WO3 on TeO2–Na2O glass systems in view of the feature of mechanical, optical, and photon attenuation
  103. Naringin ameliorates 5-fluorouracil elicited neurotoxicity by curtailing oxidative stress and iNOS/NF-ĸB/caspase-3 pathway
  104. GC-MS profile of extracts of an endophytic fungus Alternaria and evaluation of its anticancer and antibacterial potentialities
  105. Green synthesis, chemical characterization, and antioxidant and anti-colorectal cancer effects of vanadium nanoparticles
  106. Determination of caffeine content in coffee drinks prepared in some coffee shops in the local market in Jeddah City, Saudi Arabia
  107. A new 3D supramolecular Cu(ii) framework: Crystal structure and photocatalytic characteristics
  108. Bordeaux mixture accelerates ripening, delays senescence, and promotes metabolite accumulation in jujube fruit
  109. Important application value of injectable hydrogels loaded with omeprazole Schiff base complex in the treatment of pancreatitis
  110. Color tunable benzothiadiazole-based small molecules for lightening applications
  111. Investigation of structural, dielectric, impedance, and mechanical properties of hydroxyapatite-modified barium titanate composites for biomedical applications
  112. Metal gel particles loaded with epidermal cell growth factor promote skin wound repair mechanism by regulating miRNA
  113. In vitro exploration of Hypsizygus ulmarius (Bull.) mushroom fruiting bodies: Potential antidiabetic and anti-inflammatory agent
  114. Alteration in the molecular structure of the adenine base exposed to gamma irradiation: An ESR study
  115. Comprehensive study of optical, thermal, and gamma-ray shielding properties of Bi2O3–ZnO–PbO–B2O3 glasses
  116. Lewis acids as co-catalysts in Pd-based catalyzed systems of the octene-1 hydroethoxycarbonylation reaction
  117. Synthesis, Hirshfeld surface analysis, thermal, and selective α-glucosidase inhibitory studies of Schiff base transition metal complexes
  118. Protective properties of AgNPs green-synthesized by Abelmoschus esculentus on retinal damage on the virtue of its anti-inflammatory and antioxidant effects in diabetic rat
  119. Effects of green decorated AgNPs on lignin-modified magnetic nanoparticles mediated by Cydonia on cecal ligation and puncture-induced sepsis
  120. Treatment of gastric cancer by green mediated silver nanoparticles using Pistacia atlantica bark aqueous extract
  121. Preparation of newly developed porcelain ceramics containing WO3 nanoparticles for radiation shielding applications
  122. Utilization of computational methods for the identification of new natural inhibitors of human neutrophil elastase in inflammation therapy
  123. Some anticancer agents as effective glutathione S-transferase (GST) inhibitors
  124. Clay-based bricks’ rich illite mineral for gamma-ray shielding applications: An experimental evaluation of the effect of pressure rates on gamma-ray attenuation parameters
  125. Stability kinetics of orevactaene pigments produced by Epicoccum nigrum in solid-state fermentation
  126. Treatment of denture stomatitis using iron nanoparticles green-synthesized by Silybum marianum extract
  127. Characterization and antioxidant potential of white mustard (Brassica hirta) leaf extract and stabilization of sunflower oil
  128. Characteristics of Langmuir monomolecular monolayers formed by the novel oil blends
  129. Strategies for optimizing the single GdSrFeO4 phase synthesis
  130. Oleic acid and linoleic acid nanosomes boost immunity and provoke cell death via the upregulation of beta-defensin-4 at genetic and epigenetic levels
  131. Unraveling the therapeutic potential of Bombax ceiba roots: A comprehensive study of chemical composition, heavy metal content, antibacterial activity, and in silico analysis
  132. Green synthesis of AgNPs using plant extract and investigation of its anti-human colorectal cancer application
  133. The adsorption of naproxen on adsorbents obtained from pepper stalk extract by green synthesis
  134. Treatment of gastric cancer by silver nanoparticles encapsulated by chitosan polymers mediated by Pistacia atlantica extract under ultrasound condition
  135. In vitro protective and anti-inflammatory effects of Capparis spinosa and its flavonoids profile
  136. Wear and corrosion behavior of TiC and WC coatings deposited on high-speed steels by electro-spark deposition
  137. Therapeutic effects of green-formulated gold nanoparticles by Origanum majorana on spinal cord injury in rats
  138. Melanin antibacterial activity of two new strains, SN1 and SN2, of Exophiala phaeomuriformis against five human pathogens
  139. Evaluation of the analgesic and anesthetic properties of silver nanoparticles supported over biodegradable acacia gum-modified magnetic nanoparticles
  140. Review Articles
  141. Role and mechanism of fruit waste polyphenols in diabetes management
  142. A comprehensive review of non-alkaloidal metabolites from the subfamily Amaryllidoideae (Amaryllidaceae)
  143. Discovery of the chemical constituents, structural characteristics, and pharmacological functions of Chinese caterpillar fungus
  144. Eco-friendly green approach of nickel oxide nanoparticles for biomedical applications
  145. Advances in the pharmaceutical research of curcumin for oral administration
  146. Rapid Communication
  147. Determination of the contents of bioactive compounds in St. John’s wort (Hypericum perforatum): Comparison of commercial and wild samples
  148. Retraction
  149. Retraction of “Two mixed-ligand coordination polymers based on 2,5-thiophenedicarboxylic acid and flexible N-donor ligands: The protective effect on periodontitis via reducing the release of IL-1β and TNF-α”
  150. Topical Issue on Phytochemicals, biological and toxicological analysis of aromatic medicinal plants
  151. Anti-plasmodial potential of selected medicinal plants and a compound Atropine isolated from Eucalyptus obliqua
  152. Anthocyanin extract from black rice attenuates chronic inflammation in DSS-induced colitis mouse model by modulating the gut microbiota
  153. Evaluation of antibiofilm and cytotoxicity effect of Rumex vesicarius methanol extract
  154. Chemical compositions of Litsea umbellata and inhibition activities
  155. Green synthesis, characterization of silver nanoparticles using Rhynchosia capitata leaf extract and their biological activities
  156. GC-MS analysis and antibacterial activities of some plants belonging to the genus Euphorbia on selected bacterial isolates
  157. The abrogative effect of propolis on acrylamide-induced toxicity in male albino rats: Histological study
  158. A phytoconstituent 6-aminoflavone ameliorates lipopolysaccharide-induced oxidative stress mediated synapse and memory dysfunction via p-Akt/NF-kB pathway in albino mice
  159. Anti-diabetic potentials of Sorbaria tomentosa Lindl. Rehder: Phytochemistry (GC-MS analysis), α-amylase, α-glucosidase inhibitory, in vivo hypoglycemic, and biochemical analysis
  160. Assessment of cytotoxic and apoptotic activities of the Cassia angustifolia aqueous extract against SW480 colon cancer
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