Hydrogen generation from Red Sea water using CsSnI2 Cl lead-free perovskite/porous CuO nanomaterials: Coast of Jeddah, Saudi Arabia

doi:10.21203/rs.3.rs-2845482/v1

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Hydrogen generation from Red Sea water using CsSnI₂ Cl lead-free perovskite/porous CuO nanomaterials: Coast of Jeddah, Saudi Arabia

https://doi.org/10.21203/rs.3.rs-2845482/v1

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This study performed the preparation of inorganic CsSnI₂Cl Lead-free perovskite material with a great optical behavior that qualifies these materials for photoelectrode application. CsSnI2Cl is prepared through the casting adding the perovskite solution on porous CuO that previously prepared under the combustion of Cu-foil. Through short heating, the CsSnI₂Cl/CuO/Cu photoelectrode is prepared. This perovskite material is confirmed through the optical absorbance that has a great optical behavior with a band gap of 1.75 eV. The application of CsSnI₂Cl/CuO/Cu for hydrogen generation is performed using red sea water as an electrolyte, in which the hydrogen generation rate is estimated using the produced current density (J_ph) value. This J_ph value is 20 mA/cm² under a metal halide lamp. Moreover, this photoelectrode is estimated under various wavelengths, in which the optimum J_ph (10.8 mA.cm^-2) is achieved at 340 nm, in which the incident photon to electron conversion efficiency (IPCE) is 33 % at this wave lengths. This photoelectrode provides its qualified for hydrogen generation reaction under a wide optical range from 340 to 730 nm. Soon, our team is working on designing an electrochemical cell that can convert the red sea water into hydrogen gas directly.

Red sea water

perovskite

lead-free

porous materials

CuO

CsSnI2Cl.

The creation of safe and effective materials for photoelectrodes in hydrogen generation is a significant challenge for researchers. This technology can address the global energy crisis, particularly in developing nations, and promote a cleaner environment for improved health. By reducing the toxic oxides generated from the burning of fossil fuels each year, these deadly gases can be prevented from causing harm to lives[1–4].

Hydrogen generation reactions involve two aspects: the development of a suitable photoelectrode and achieving high efficiency in hydrogen generation. Researchers are focused on both aspects, with a particular emphasis on developing a material that is highly sensitive to photons. Oxides and halides are among the materials that exhibit good light-responsive behavior, and their stability makes them attractive for use in various applications[5–8]. By developing an efficient photoelectrode for hydrogen generation, scientists hope to provide a solution to the global energy crisis while also reducing the harmful effects of fossil fuel combustion on the environment and human health.

Improving the morphology of the materials is a strategy to enhance their efficiency, particularly through developing nanomaterials with different surface morphologies, such as sheets and wires, which can greatly impact their optical properties. However, these materials still face limitations, including low efficiency for hydrogen generation or high costs associated with complex preparation techniques[2, 9, 10].

Perovskite materials are an attractive option for photoelectrodes due to their excellent optical properties, particularly their high sensitivity to photons[11, 12]. Among these materials, lead-free perovskites are considered to be safe and highly sensitive to light, making them a promising option for use in various applications[13]. The second challenge in the hydrogen generation reaction is to develop an electrolyte that can serve as a source of hydrogen, and reducing the use of a sacrificing agent is a promising approach to reduce the costs of this process.

Rabia et al have conducted research on hydrogen generation through the splitting of sewage water, achieving good efficiency as measured by the Jph value, which represents the rate of the hydrogen generation reaction. In their work, they have obtained a J_ph of -1.6 mA/cm² using poly-3-matjyl aniline with wastewater as the electrolyte[14], -0.1 mA.cm-2 using TiN/TiO2/Alumina Membrane[15], and 0.13 mA.cm-2 using polyaniline/PbS for sewage water splitting[16]. Other studies by Rabia et al have also investigated hydrogen generation from sewage water, paraphrasing.

In this study, red-sea water is utilized as an electrolyte for the hydrogen generation reaction, as it contains a high concentration of ions which can act as a natural sacrificing agent. CsSnI₂Cl lead-free perovskite material is deposited on CuO/Cu, in which the produced CsSnI₂Cl/CuO/Cu photoelectrode is applied for the hydrogen generation using a three-electrode cell. The estimation of the IPCE and hydrogen moles are calculated under various optical conditions and wavelengths.

2.1. Materials and characterization

The chemicals used in the experiment include cesium chloride (CsCl, 99.9%), tin chloride (SnCl₂, 99.9%), and dimethyl formamide (DMF, 99.9%). These chemicals are obtained from Sigma Aldrich, USA, while potassium iodide (KI, 99.9%) are obtained from Pio-Chem Co., Egypt. Additionally, copper foil with a thickness of 1.0 mm and purity of 99.9% is used in the experiment.

The characterization is performed using different devices and models; XRD (PANalytical) FTIR (Jasco spectrophotometer), XPS (Kratos Analytical Ltd, UK), SEM (ZEISS, Germany), TEM (JEOL JEM-2100), and UV (spectrophotometer, Perkin Elmer).

2.2. Preparation of CsSnI₂Cl/CuO and electrochemical testing

CuO is synthesized using a hydrothermal method by oxidizing Cu foil at 400°C in air. CsSnI₂Cl is synthesized by drop-casting a solution containing KI, CsCl, and SnCl2 dissolved in DMF (3:1:1) onto the CuO foil. After drop-casting, the layer is dried at 150°C for 5 minutes, resulting in the formation of a perovskite layer on top of the CuO material.

The CsSnI₂Cl/CuO photoelectrode is used as the working electrode in a three-electrode cell, where the produced current density (J_ph) from the workstation (CHI608) is used to determine the hydrogen generation rate. A calomel electrode and graphite are used as reference and counter electrodes, respectively. The photocurrent, which represents the rate of hydrogen gas produced under light illumination from a metal halide lamp (400 W), is determined through this electrochemical testing. It should be noted that J_ph depends on the light wavelengths or conditions.

3.1. Analyses

The analyses describe morphological and topographic conducted on two materials: CuO nanomaterials and CsSnI₂Cl perovskite. For CuO nanomaterials, Fig. 1(a), SEM analysis shows that the material has a great porous structure with pore diameter ranging from 150 to 250 nm. These pores can work as a trap for other materials, allowing the growth of additional material inside it. For CsSnI₂Cl perovskite materials, Fig. 2(b), the morphological behavior appears like pyramid-shapes with large crystals that confirm their great behavior and compact surface. This behavior confirms the perovskite materials' ability for the light reaction and production of electrons under the light incidence[17]. The pyramid side is about 400 nm above the surface.

The theoretical modeling of CsSnI₂Cl perovskite surface roughness is represented in Fig. 2(c), where a 3D pyramid structure appears for the perovskite materials. These particles are surrounded by other smaller particles that prevent the formation of pores. Finally, the TEM analyses for CsSnI₂Cl perovskite material are shown in Fig. 2(d), where the 2D pyramid structure are confirmed again with a dark color, in which there ia additional small particles surrounding it.

The XRD pattern shown in Fig. 2(a) is related to CuO/Cu, it is evident that the peaks correspond to the formation of CuO monoclinic structure, which is indicated by the peaks located at 35° and 38.5° (JCPDS #41–0254) [18]. In addition, sharp peaks observed at 43°, 50°, and 62° indicate the presence of Cu-foil (JCPDS #02–1225) [19].

The XRD pattern of the CsSnI2Cl perovskite materials is presented in Fig. 2(b). The pattern shows several sharp peaks, which indicate the successful formation of the perovskite materials. The peaks correspond to the crystallographic planes (101), (240), (131), (240), (320), (301), (210), (112), (321), (004), (322), (430), (362), and (323), with diffraction angles of 21.5°, 24.9°, 26.4°, 27.6°, 28.5°, 30.9°, 35.4°, 41.8°, 43.9°, 48.8°, 50.0°, 57.9°, 62.3°, and 66.2°, respectively. The presence of a large number of peaks is consistent with the characteristics of inorganic perovskite tin halide materials [11].

The XPS analysis of CsSnI₂Cl is presented in Fig. 2(c), which shows the survey of the perovskite material. All the elements are observed, confirming the formation of the perovskite material. The Cl and I spectra are observed at 201 and 635 eV, respectively, related to the 2p and 3d orbital spectra. N and O are detected at 404 and 534 eV, respectively, related to the 1s spectra for both. The Sn atom is observed at 490 eV for the 3D orbital spectra, while the Cs spectra are observed at 719 eV. Additionally, a very small peak related to the K spectra is observed at 297 eV.

Figure 2(d) shows the optical absorbance of CsSnI2Cl perovskite material, indicating its absorption band in the UV, Vis, and near-IR region up to 680 nm. The incorporation of Cl and I atoms in the perovskite material leads to this enhancement in optical behavior, covering most of the optical region. To evaluate the superiority of this material, its bandgap is calculated using Tauc's Eqs. 1 and 2 [20]. These equations utilize the density (d) and absorption coefficient of the material (α) to estimate the bandgap (Eg), which is found to be 1.75 eV.

$${{\alpha }\text{h}{\nu } = \text{A}(\text{h}{\nu }-{\text{E}}_{\text{g}})}^{1/2}$$

$${\alpha }=\left(\frac{\text{2,303}}{\text{d}}\right)\text{A}$$

3.2. Red Sea water as a source of hydrogen gas: electrochemical testing

This study used Red Sea water as a source of hydrogen gas. Table 1 provides the chemical composition of this water, which is a promising choice for generating hydrogen gas through electrochemical means. The heavy metals present in this water act as a sacrificing agent for the hydrogen gas production process, eliminating the need for an external electrolyte. This approach is cost-effective since the water is abundant and freely available. A three-electrode cell is used for their experiments, where the CsSnI₂Cl/CuO/Cu photoelectrode was used as the working electrode, and the reference and auxiliary electrodes were connected to the cell to facilitate the electrochemical reactions. The researchers applied photon illumination to the cell using the CHI608E instrument and a metal halide lamp with a power of 400 W.

Figure 3(a) shows the photosensitivity of the prepared CsSnI₂Cl/CuO/Cu photoelectrode under light illumination. This photoelectrode receives photons that excite the surface of the semiconductor materials (CsSnI₂Cl and CuO) for electron transition, and the resulting electrons are collected on the surface of the photoelectrode. These electrons are then transferred to the neighboring electrolyte for the hydrogen generation process through the J_ph value. The J_ph value produced by this photoelectrode is 20 mA/cm² in light, which indicates its high photosensitivity for the hydrogen generation reaction.

The small current density (J_o) observed in the dark indicates the semiconductive nature of the prepared material, which is significantly smaller than the J_ph value produced under light illumination. This demonstrates the significant effect of incident photons on the photoelectrode for the hydrogen generation reaction. The curve is non-linear, indicating the generation of a Schottky barrier [21] during the electron transition from CuO to CsSnI₂Cl. This is due to the difference in energy levels between the two materials. After the electrons are generated by the photoelectrode, they reach the surface of the perovskite material and combine with the electrons produced by the material itself. These electrons then move towards the seawater where they participate in the splitting reaction, leading to the production of hydrogen gas.

Figure 3(b) further supports this observation by testing the photoelectrode under both dark and light conditions. The significant increase in Jph value (by -2.5 mA.cm^− 2) and the decrease in Jo value (by -0.93 mA.cm^− 2) in light compared to dark confirm the high sensitivity of the prepared CsSnI₂Cl/CuO/Cu photoelectrode to light.

Table 1

The concentration of metals in red sea water.
Material or element	Concentration (mg/L)
Zn	0.044
Pb	0.008
Ni	0.001
Mn	0.009
Fe	0.012
Cu	0.10
Cr	0.005
Cd	0.001
Co	0.032
B	0.132

The response of the CsSnI₂Cl/CuO/Cu photoelectrode to light is shown in Fig. 4(a) through the produced J_ph values under different monochromatic lights. The J_ph value at -0.8 V is shown in Fig. 4(b). As seen in Fig. 4(a), there are significant enhancements in the J_ph values as the light wavelength decreases from 730 to 440 nm, with the J_ph value decreasing from − 10.8 to -4.9 mA.cm^− 2, respectively. This behavior is typical in the effect of light on a photoelectrode, where the high effect of light under low wavelength is due to the high frequency of light, which promotes electron transition from low to high energy levels[22, 23]. These electrons are collected on the upper level and transferred to the electrolyte solution for further reactions. In contrast, the J_ph under low frequency (near IR) is related to bond vibrations that cause electron vibration. At V = 0, the high photocurrent value represents the efficiency of these materials for electron production, in this case, J_ph = J_SC.

The efficiency of the hydrogen generation reaction was estimated using Eq. 3 and is shown in Fig. 5(a). The CsSnI₂Cl/CuO/Cu photoelectrode achieved a high and broad efficiency across most of the optical region, with an optimal value of 33% at 340 nm. The efficiency decreased to 13% at 730 nm, indicating that the optimal generation of electrons occurred under photon incidence at 340 nm. Figure 5(b) presents the calculation of the number of H₂ moles produced from the CsSnI₂Cl/CuO/Cu photoelectrode based on the Faraday law [7] and using the constant Faraday constant (F, 9.65×104 C mol-1). The estimated H2 mole is 30 µmole/h.cm2. This means that using a 10 cm² surface of this photoelectrode would result in the production of 0.3 m.mol/h. Moreover, The efficiency of CsSnI₂Cl/CuO/Cu photoelectrode in compared to the previous studies is mentioned in Table 2.

IPCE = 1240.${J}_{ph}$/λ. P .100 (3)

Table 2

The efficiency of CsSnI₂Cl/CuO/Cu photoelectrode in compared to the previous studies.
Photoelectrode	Electrolyte	J_ph (mA/cm²)	Applied Voltage (V)	IPCE% (390 nm)	Light Source
CuO-C/TiO₂ [24]	glycerol	0.001	−0.5	-	300 W xenon lamp
g-C₃N4-CuO [25]	NaOH	0.01	1.6	-	300 W xenon lamp
CuO thin films [26]	Na₂SO₄	2.5	0	3.1	Solar simulator 1.5 global (AM 1.5G)
TiO₂/CdS/PbS [27]	Na₂S/Na₂S₂O₃	2	0.2	4	AM 1.5G illumination
CuO nanowire [28]	Na₂SO₄	1.5	−0.5	-	simulated AM1.5 illumination
GaN [29]	HBr	0.6	+ 1	8	Sunlight
CuO [30]	KOH	1	−1.2	-	White light
SnO₂/TiO₂ [31]	Na₂S₂O₃	0.4	0.6	-	1 Sun (100 mW cm^− 2)
BiFeO₃ [32]	NaOH	0.1	1.6	0.21	1 sun (AM 1.5G solar spec)
PrFeO [33]	Na₂SO₄	0.130	−0.6	-	Simulated sunlight
CuO nanocrystals [34]	Na₂SO₄	1.1	−0.5	8.7	Xenon lamp light
Poly(3-aminobenzoic acid) frame [35]	H₂SO₄	1.2	1.6	-	150 W xenon lamp
ZnO/TiO₂/FeOOH [36]	Na₂S₂O₃	1.59	0.8	-	A 150 W xenon lamp
TiN-TiO₂ [22]	NaOH	3.0 × 10^− 4	0.2	0.03	Solar simulator (150 mW cm^− 2)
ITO/VO2 [37]	Na₂S₂O₃	1.5	+ 1	4	400 W metal halid
Au/PbS/Ro-GO/PANI [38]	Na₂S₂O₃	1.1	+ 1	10	400 W xenon lamp
CsSnI₂Cl/CuO/Cu (Present work)	Red sea water	20	-0.8	33	Simulated sunlight

In summary, this study focused on the preparation and characterization of CsSnI₂Cl/CuO/Cu photoelectrode for hydrogen generation. The perovskite material was prepared using a casting method on porous CuO, and the optical behavior of CsSnI₂Cl was confirmed to have a bandgap of 1.75 eV. The photoelectrode showed a high J_ph value of 20 mA/cm² under a metal halide lamp, and an optimum J_ph value of 10.8 mA/cm² was achieved at 340 nm. The IPCE efficiency was estimated to be 33% at this wavelength. The photoelectrode showed a wide optical range for hydrogen generation from 340 to 730 nm, with an estimated hydrogen generation rate of 30 µmole/h.cm². The results demonstrate the potential of CsSnI₂Cl/CuO/Cu photoelectrode as a promising candidate for hydrogen generation using seawater as an electrolyte.

Acknowledgments

The Deanship of Scientific Research (DSR) at King Abdulaziz University (KAU), Jeddah, Saudi Arabia has funded this Project under grant no (G: 026-130-1443).

Authors contributions

All the authors have shared well in this manuscript. All authors approve this submission.

The authors have no conflict of interest

Research Data Policy and Data Availability Statements

All data generated or analysed during this study are included in this article

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Hydrogen generation from Red Sea water using CsSnI₂ Cl lead-free perovskite/porous CuO nanomaterials: Coast of Jeddah, Saudi Arabia

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Abstract

Figures

1. Introduction

2. Experimental section

2.1. Materials and characterization

2.2. Preparation of CsSnI₂Cl/CuO and electrochemical testing

3. Results and discussion

3.1. Analyses

3.2. Red Sea water as a source of hydrogen gas: electrochemical testing

4. Conclusions

Declarations

References

Additional Declarations

Status:

Version 1

Hydrogen generation from Red Sea water using CsSnI2 Cl lead-free perovskite/porous CuO nanomaterials: Coast of Jeddah, Saudi Arabia

Status:

Version 1

Abstract

Figures

1. Introduction

2. Experimental section

2.1. Materials and characterization

2.2. Preparation of CsSnI2Cl/CuO and electrochemical testing

3. Results and discussion

3.1. Analyses

3.2. Red Sea water as a source of hydrogen gas: electrochemical testing

4. Conclusions

Declarations

References

Additional Declarations

Status:

Version 1

Hydrogen generation from Red Sea water using CsSnI₂ Cl lead-free perovskite/porous CuO nanomaterials: Coast of Jeddah, Saudi Arabia

2.2. Preparation of CsSnI₂Cl/CuO and electrochemical testing