Photoelectrochemical Response Research Articles

Boosting visible-light photoelectrochemical water splitting response of WO3–MoS2 nanocomposites by transition metal doping: Experimental and first-principles studies

The current study employs both theoretical and experimental methods to investigate the effect of Ti and Co doping on the WO3 nanocomposite with MoS2 photoanode's photoelectrochemical (PEC) water-splitting reaction. A simple hydrothermal and sol-gel method was adopted for the preparation of samples. The Ti-doped WO3–MoS2 (1.96 at %) sample showed the maximum optical absorption with a photocurrent density of 1.15 mA/cm2 at 1.6 V vs Ag/AgCl. The improvement in photocurrent density may be ascribed to the upward shifting of the conduction band edge towards the H+/H2 redox potential as well as the presence of a large number of active sites in MoS2. A high value of flat band potential of −0.3 V vs Ag/AgCl was achieved in Ti-doped WO3–MoS2, which was confirmed by Mott-Schottky measurements with the corresponding lowest charge transfer resistance at the semiconducting electrode/electrolyte interface. Furthermore, density functional theory calculations have also indicated that on doping WO3 with Ti and Co, there is a slight upward shift in the conduction band minimum, without any significant change in the valence band maximum, with respect to the Fermi level. This study provides new insight into the impact of transition metal doping and nanocomposite of chalcogenide materials for WO3-based PEC electrodes.

Synthesis of CuO nanosheets on Cu foil via one-step wet chemical process at different reaction temperatures and their photoelectrochemical performance

Cupric oxide (CuO) nanostructures were directly grown on copper substrate via a simple one step solution-immersion process. The films were formed by the direct oxidation of copper in aqueous solution containing sodium hydroxide (NaOH) and ammonium persulfate (NH4)2S2O8. The influence of the reaction temperature on the structural, morphological, optical and photoelectrochemical (PEC) properties of the formed copper compounds nanostructures was investigated. The XRD and Raman spectroscopy results revealed the formation of Cu(OH)2/CuO composite for the samples prepared at 3 and 25 °C, and pure CuO was obtained for the samples prepared at 45 and 55 °C. The SEM micrographs showed that the formed Cu(OH)2 and CuO present a nanowire bundles and nanosheet morphology, respectively. The increase of the reaction temperature enhanced the absorbance of the CuO samples in the entire visible region. According to the photoelectrochemical measurements, the increase of the reaction temperature resulted in an improvement of the PEC response. The CuO nanosheets synthesized at 55 °C presents the highest and the most stable PEC response. A reasonable mechanism describing the formation of nanostructured copper compounds at different reaction temperatures is discussed in this paper.

Photoelectrochemical sensor consisting of sulfhydryl-borate ester modified A1/B1 type Pillar[5]arene-functionalized gold NPs

Recognition of mitochondrial reactive oxygen species (ROS) in cells is essential for understanding the critical roles of different ROS in biology reaction processes. In this study, an ultrasensitive and specific photoelectrochemical (PEC) sensor is constructed and applied for the capture and identification of H2O2 in cells. For the targeted detection of H2O2 in cells containing similar groups, such as •OH and O2•-, a new sulfhydryl-borate ester modified A1/B1 type pillar[5]arene (BP5) with a specific borate group is designed as a specific recognition molecule, and Au nanoparticles (Au NPs) are synthesized as the photoactive material. Specifically, the localized surface plasmon resonance (LSPR) of the Au NPs and host-guest interaction between BP5 and H2O2 increase the photocurrent signal. At the same time, specific groups on BP5 react with H2O2 to specifically recognize it. The Au@BP5/GCE shows strong photoelectrochemical response for the detection of H2O2 with limit of detection (0.33 pM, S/N=3), an extended linear range (1–60 pM), high specificity, good stability and excellent reproducibility.

Spatial-resolved and self-calibrated 3D-printed photoelectrochemical biosensor engineered by multifunctional CeO2/CdS heterostructure for immunoassay

A spatial-resolved and self-calibrated photoelectrochemical (PEC) biosensor has been fabricated by a multifunctional CeO2/CdS heterostructure, achieving portable and sensitive detection of carcinoembryonic antigen (CEA) using a homemade 3D printing device. The CeO2/CdS heterostructure with matched band structure is prepared to construct the dual-photoelectrodes to improve the PEC response of CeO2. In particular, as the photoactive nanomaterial, the CeO2 also plays the role of peroxidase mimetic nanozymes. Therefore, the catalytic performance of CeO2 with different morphologies (e.g., nano-cubes, nano-rods and nano-octahedra) have been studied, and CeO2 nano-cubes (c-CeO2) achieve the optimal catalytic activity. Upon introducing CEA, the sandwich-type immunocomplex is formed in the microplate using GOx-AuNPs-labeled second antibody as detection antibody. As a result, H2O2 can be produced from the catalytic oxidization of glucose substrate by GOx, which is further catalyzed by CeO2 to form •OH, thus in situ etching CdS and decreasing the photocurrents. The self-calibration is achieved by the dual-channel photoelectrodes on the homemade 3D printing device to obtain the photocurrents ratio, thus effectively normalizing the fluctuations of external factors to enhance the accuracy. This integrated biosensor with a detection limit as low as 0.057 ng mL−1 provides a promising way for ultrasensitive immunoassay in clinic application in complex environments.

Correlating activities and defects in (photo)electrocatalysts using in-situ multi-modal microscopic imaging

Photo(electro)catalysts use sunlight to drive chemical reactions such as water splitting. A major factor limiting photocatalyst development is physicochemical heterogeneity which leads to spatially dependent reactivity. To link structure and function in such systems, simultaneous probing of the electrochemical environment at microscopic length scales and a broad range of timescales (ns to s) is required. Here, we address this challenge by developing and applying in-situ (optical) microscopies to map and correlate local electrochemical activity, with hole lifetimes, oxygen vacancy concentrations and photoelectrode crystal structure. Using this multi-modal approach, we study prototypical hematite (α-Fe2O3) photoelectrodes. We demonstrate that regions of α-Fe2O3, adjacent to microstructural cracks have a better photoelectrochemical response and reduced back electron recombination due to an optimal oxygen vacancy concentration, with the film thickness and extended light exposure also influencing local activity. Our work highlights the importance of microscopic mapping to understand activity, in even seemingly homogeneous photoelectrodes.

Surface plasmonic hot hole driven Ag2S/Au/Al2O3 photocathode for enhanced photoelectrochemical water splitting performance

Herein, Ag2S/Au/Al2O3 photoelectrode was fabricated for superior photoelectrochemical (PEC) water splitting response. The working electrodes were deposited using the glancing angle deposition (GLAD) method followed by RF sputtering and atomic layer deposition (ALD). The as-prepared Ag2S/Au/Al2O3 samples revealed a higher photocurrent density of 2.50 mA/cm2 (at 0.95 V Ag/AgCl) as compared to bare Ag2S (1.70 mA/cm2) with a corresponding less charge transfer resistance at the semiconducting interface. The superior PEC response may be ascribed to the synergic effect of plasmonic Au nanoparticles and the tilted Ag2S nanorods. The plasmonic effect of Au nanoparticles increases the visible-light response of Ag2S as well as provides the hot holes to enhance the photocurrent density. In addition, the increased trapping of light due to the tilted architecture of Ag2S nanorods resulted in an effective absorption of light. The theoretical simulations based on finite difference time domain (FDTD) were also performed to explore the distribution of the electric-field intensity and optical trapping of light between the nanorods of Ag2S and Ag2S/Au. The experimental and theoretical results show a deeper insight into the role of plasmonic nanostructures decorated Ag2S nanorods and shed light on designing hybrid hot hole harvesting semiconductor nanostructures for the next generation photoelectrodes.

Improved photoelectrochemical performance of tungsten-catalyzed graphene nanoplatelet electrodes prepared by hot-wire chemical vapor deposition at low substrate temperatures

The current increase in demand for graphene in various energy applications such as electrode materials for supercapacitors, batteries, thermoelectric, and hydrogen production via water-splitting, the production of high-quality graphene, considering its fascinating physical and electrical properties, high-yield, and large-area has becoming more challenging at the research and development level. Therefore, in this work, graphene nanoplatelets (GNPs) were directly grown on tungsten nanoparticle (W NP)-coated p-type crystalline silicon and quartz substrates using hot-wire chemical vapor deposition at low substrate temperatures (<500 °C). Prior to the GNP deposition, a plasma process was employed to induce the formation of W NPs, which act as a metal catalyst for facilitating the growth of large-area and multi-layer GNPs. The W NPs were formed at substrate temperatures ranging from 250 to 550 °C, with the largest graphene sheet was grown at 450 °C. Higher substrate temperatures promote the growth of high-quality graphene layers with high intensities of G (IG) and 2D bands (I2D), and high I2D/IG ratio values. The GNP photoelectrode prepared at 450 °C demonstrated better photoelectrochemical responses with the highest photocurrent density of 1.65 mA/cm2 at 1.5 VAg/AgCl, the lowest charge transfer resistance (14.0 kΩ), and the highest donor density (2.57 × 10 28 cm−3) compared to the tungsten carbide thin film and W NP electrodes prepared at the same temperature. The effects of substrate temperature on the optical, structural, and photoelectrochemical properties of the as-grown GNPs are discussed.

Bulk and interface engineering with the combined addition of Na+ and E5+ (E = Nb5+, Ta5+) in the design of hematite photoanodes

In this letter, the synergistic effects of multiple element modification through a single polymeric precursor solution in hematite-based photoanodes using Na/Nb and Na/Ta as dopants are evaluated. Linear sweep voltammetry curves showed that the photoelectrochemical response was improved after Na/Nb (or Ta) addition. In both circumstances, an anodic shift (∼200 mV) in the onset potential was noticeable due to surface states created after Nb5+/Ta5+ segregation. The energetic loss caused by Nb (and Ta) segregation was partially restituted by NiFeOx addition due to the passivation of surface states, acting as recombination centers created by pentavalent modifiers. These combined modifications brought a three and four-fold increase for Na0.1HemNb1.5 NiFeOx and Na0.1HemTa1.0NiFeOx respectively. Charge carrier dynamics analysis studied by intensity modulated photocurrent spectroscopy revealed that the PEC enhancement in both systems is mainly associated with improved charge separation efficiency.

Electronic Structures of Passive Film Formed on Ti and Cr in a Phosphate Buffer Solution of pH 7

The electronic structures, including the semiconductive properties, of the passive films formed on Cr and Ti in a phosphate buffer solution of pH 7 were evaluated using photoelectrochemical response, electrochemical impedance spectroscopy and X-ray photoelectron spectroscopy (XPS). Based on the results, electronic band structure models of the passive films were proposed: the passive films on Cr consisted of an inner p-type oxide layer with a band gap energy, E g, of 3.6 eV and an outer p-type hydroxide layer with E g of 2.5 eV whereas those on Ti consisted of an inner n-type oxide layer with E g of 3.2 eV and an outer n-type hydroxide layer with E g of 2.5 eV. The type of semiconductor evaluated for the oxide and hydroxide layers was strongly supported by valence-band XPS, which can provide the energy difference between the Fermi energy of the underlying metal and the highest energy of the valence bands of the oxide and hydroxide layers in the passive films.

Optimization of Photoelectrochemical Response on TiO2 Nanotube Arrays Treated by H3PO4 and Mechanism Analysis of the Slowing Down Effect during Preparation.

The process control of anodization has been a hot topic for a long time. In this study, the addition of phosphoric acid to the traditional electrolyte changed the ion distribution on the reaction interface and the composition of the anion contamination layer so as to achieve the slowing down effect on anodization, the mechanism and theoretical model of which are also given in this paper. TiO2 is a common material in photoelectrocatalysis, but there are few studies on the photoelectrochemical performance of TiO2 nanotube arrays. The stability and rapidity of the photoelectrochemical response of TiO2 nanotube arrays prepared in phosphoric acid containing an electrolyte were effectively optimized in this study.

A coupled faradaic/electrostatic boosting strategy for decolorization of a refractory dye inside a dually-biased photoelectrochemical reactor: Time and energy saving

A green sustainable strategy for environmental remediation and treatment of dye-polluted water is the application/development of effective photoelectrochemical (PEC) reactors. Despite some recent progress in PEC systems, achieving a complete decolorization is still a challenging issue and often requires a long period of reactor operation. Herein, the authors address this interesting time/energy-related problem, demonstrating how without consuming extra electricity/chemicals, fabricating complex photoelectrodes, or changing the pH of medium, one can effortlessly promote the activity of a PEC reactor just by its coupling to a non-faradaic bias source. By applying this novel dually biased (faradaic/electrostatic) boosting strategy, we reveal that decolorization of methyl orange (a refractory dye pollutant) is significantly improved and the decolorization time (thereby energy consumption) is reduced by almost half in comparison to that of a conventional PEC reactor–operating under a single-bias (faradaic) condition. The reactor activity and its photoelectrochemical response are finally discussed in detail in terms of applied potential biases, semiconductor's band bending, open-circuit-potential displacement, electrostatic interaction and electrosorption of dye pollutant.

G-C3N4/Porphyrin-based graphdiyne (PDY) 2D/2D heterojunction for the ultrasensitive photoelectrochemical detection of microRNA-21

As an n-type semiconductor material with a wide band gap, g-C3N4 has been applied in the photoelectrochemical (PEC) sensing field, while the narrow absorption light range and tendency of electron-hole recombination significantly limit its practical applications. In this study, we developed a new g-C3N4/porphyrin-based graphdiyne (PDY) 2D/2D heterojunction photoelectric nanocomposites via in-situ growth of PDY on the g-C3N4 nanosheets. The introduction of PDY significantly enhances the light capture ability of g-C3N4 in terms of absorbance and the absorption range throughout the entire UV-Vis region. More importantly, the well-matched band structure between PDY and g-C3N4 inhibits the electron-hole recombination to improve the charge separation efficiency. In addition, such 2D/2D heterojunction has a short charge transfer distance and a large contact area, further promoting the interfacial charge transfer. As a result, the PEC response of g-C3N4/PDY is 2.54 times higher compared with that of g-C3N4, enabling the ‘turn on’ PEC determination of miRNA-21 according to the sandwich-type sensing strategy, and the linear range of 0.01 fM-100 pM with a limit of detection (LOD) of 0.005 fM was achieved. Due to the diversity of graphdiyne monomers, we envision that the g-C3N4/PDY 2D/2D heterojunction carrying different graphdiyne-based materials may exhibit great potential in PEC sensing, photocatalysis, and solar cells.

CdS quantum dots sensitized Ti-MOFs as high-performance photocathodic materials for immunoassay of alpha-fetoprotein based on Ag+ exchange strategy

Cathodic photoelectrochemical (PEC) analysis has drawn much attention because of its excellent anti-interference capability toward reductive substances in samples, but the development high-performance photocathodic materials is challenging. We report here CdS quantum dots (QDs) sensitized titanium-based metal–organic frameworks (Ti-MOFs) as high-performance photocathodic materials for ultrasensitive immunoassay of alpha-fetoprotein (AFP) based on Ag+ exchange strategy. Due to the excellent sensitization effect of CdS QDs, the photocathodic current of CdS QDs decorated MIL-125-NH2(Ti) is 25-fold that of MIL-125-NH2(Ti) alone. The photocathodic current of CdS/MIL-125-NH2(Ti) can be quenched after Ag+ exchange, because CdS is partially converted to Ag2S that serves as a charge-recombination center. Based on the PEC response of CdS/MIL-125-NH2(Ti) to Ag+, a cathodic PEC immunoassay platform is constructed for AFP detection by using CdS/MIL-125-NH2(Ti) as the photoactive material and Ag nanoparticles modified SiO2 nanospheres as labels. The linear range for AFP detection is from 1.0 × 10−4 to 1.0 × 102 ng mL−1, and the detection limit is 20 fg mL−1. The constructed PEC immunosensor is successfully used for detecting AFP in human serum samples. In this work, a novel and high-performance photoactive material is developed for cathodic PEC analysis, and a simple and effective PEC immunoassay platform for AFP detection is constructed based on Ag+ exchange strategy.

A photoelectrochemical aptasensing platform assembled at the heterojunction interface of Cu3BiS3 sensitized CuV2O6 for bisphenol A.

The interaction between the sensitive interfaces of photoelectrochemical (PEC) semiconductor nanomaterials and microscopic matter creates endless potential for the efficient detection of endocrine disruptor. Thiswork presents the development of a high-efficiency PEC aptasensor for bisphenol A (BPA) monitoring based on Cu3BiS3 sensitized CuV2O6 nanocomposites with exceptional visible-light PEC activity. We implemented the integration of Cu3BiS3 nanosheet photosensitizer to sensitize the CuV2O6 nanowire structure that was synthesized utilizing a facile hydrothermal approach. The band gap alignment between Cu3BiS3 and CuV2O6 facilitated enduring PEC response yielding an efficient interfacial structure. The surface of the CuV2O6/Cu3BiS3 electrode was modified with BPA aptamer, enabling specific binding with BPA and precise quantification of its content. The developed aptamer sensors possess a wide detection range of5.00 × 10-1 to 5.00 × 104 ng/mL, and a low detection limit of 1.60 × 10-1 ng/mL (at S/N = 3). After undergoing 20 testing cycles and enduring long-term storage, the sensor maintained its stability and showcased excellent repeatability and reproducibility. This study presents a promising methodology for the detection of BPA in environmental settings.

Wavelength-dependent photoelectrochemical response demonstrated by the determination of acetaminophen and rutin in differential molecularly imprinted polymers strategy

Herein, the excitation wavelength-dependent responses of the molecularly imprinted polymer (MIP) photoelectrochemical (PEC) sensors were investigated, using acetaminophen (AP), rutin (RT) and perfluorooctanoate (PFOA) as the model templates, pyrrole as functional monomer, CuInS2@ZnS/TiO2 NTs as the basic photoelectrode. With wavelength λ > 240 nm, the photocurrent of MIPPFOA enhanced at higher concentrations of PFOA. With increasing AP concentration, the photocurrents of MIPAP could decline with λ < 271 nm, not change at λ = 270 nm, or increase with λ > 270 nm. As RT concentration increased, the photocurrents of MIPRT could decrease (λ < 431 nm), not change (λ = 431 nm) or increase (λ > 431 nm). The PEC responses depend on the comprehensive interaction of two contrary mechanisms from the template molecules within the MIP membrane. The photocurrent is enhanced by the role of the electron donor for photo-generated holes but attenuated due to the steric hindrance effect and the excitation light intensity loss via absorption or scattering. The apparent molar absorption coefficient of AP and RT within MIP membranes are 9.1–19.4 folds of those measured from dilute solutions. By using a routine UV lamp as the light source, the photocurrents of MIPRT at 254 nm and MIPAP at 365 nm were used to determine RT and AP, with the detection limits of 5.3 and 16 nM, respectively. The interference from the non-specific adsorption of interferents on the surfaces of MIPAP and MIPRT was reduced by one order of magnitude via a differential strategy.

A label-free photoelectrochemical biosensor for silver ions based on Zn-Co doped C and CdS QD nanomaterials.

A sensitive photoelectrochemical (PEC) biosensor for silver ions (Ag+) was developed based on Zn-Co doped C and CdS quantum dot (CdS QD) nanomaterials. Hydrophobic modified sodium alginate (HMA), which could stabilize and improve the PEC performance of CdS QDs, was also used for the construction of PEC sensors. Especially, Zn-Co doped C, CdS QDs and HMA were sequentially modified onto an electrode surface via the drop-coating method, and a C base rich DNA strand was then immobilized onto the modified electrode. As the C base in DNA specifically recognized Ag+, it formed a C-Ag+-C complex in the presence of Ag+, which created a spatial steric hindrance, resulting in a reduced PEC response. The sensing platform is sensitive to Ag+ in the range of 10.0 fM to 0.10 μM, with a limit of detection of 3.99 fM. This work offers an ideal platform to determine trace heavy metal ions in environmental monitoring and bioanalysis.

Efficient sensitization of CdTe QDs towards PTCDA for sensitive photoelectrochemical Hg2+ assay.

Herein, a sensitive photoelectrochemical (PEC) biosensor was designed for the detection of mercury ions (Hg2+) on the basis of the efficient sensitization of cadmium telluride quantum dots (CdTe QDs) towards 3,4,9,10-perylenetetracarboxylic dianhydride (PTCDA) and the significant quenching ability of a thymine-Hg2+-thymine (T-Hg2+-T) structure. The proposed CdTe QD/PTCDA sensitized structure was successfully constructed via continuous incubation of PTCDA and CdTe QDs on the glassy carbon electrode (GCE) interface, which embraced strong light absorption capacity and high carrier separation efficiency, giving rise to a remarkably improved initial photocurrent response. Notably, the PEC signal generated from the CdTe QD/PTCDA sensitized structure was almost fivefold higher than that of PTCDA owing to the efficient sensitization of CdTe QDs towards PTCDA. Once target Hg2+ ions were added, a T-rich S1 strand modified on the surface of 1-hexanethiol (HT)/S1/gold nanoparticles (Au NPs)/CdTe QDs/PTCDA/GCE immediately reacted with Hg2+ to produce multiple stable T-Hg2+-T structures. Therefore, the initial PEC signal would be considerably quenched by a high steric hindrance effect derived from the T-Hg2+-T structures. As a result, a quenched PEC response could achieve the detection of Hg2+ in concentrations ranging from 100 fM to 1000 nM. More importantly, the combination of the CdTe QDs/PTCDA sensitization structure and the T-Hg2+-T structure paves a promising pathway to developing a novel PEC biosensing platform for Hg2+ detection and also provides a favorable strategy for monitoring environmental pollution related to Hg2+.

A sandwich-type photoelectrochemical biosensor based on Ru(bpy)32+ sensitized In2S3 for aflatoxin B1 detection.

Aflatoxin B1 (AFB1), classified as a class I carcinogen, is a widespread mycotoxin that poses a serious threat to public health and economic development, and the food safety problems caused by AFB1 have aroused worldwide concern. The development of accurate and sensitive methods for the detection of AFB1 is significant for food safety monitoring. In this work, a sandwich-type photoelectrochemical (PEC) biosensor for AFB1 detection was constructed on the basis of an aptamer-antibody structure. A good photocurrent response was obtained due to the sensitization of In2S3 by Ru(bpy)32+. In addition, this sandwich-type sensor constructed by modification with the antibody, target detector, and aptamer layer by layer attenuated the migration hindering effect of photogenerated carriers caused by the double antibody structure. The aptamer and antibody synergistically recognized and captured the target analyte, resulting in more reliable PEC response signals. CdSe@CdS QDs-Apt were modified as a signal-off probe onto the sensor platform to quantitatively detect AFB1 with a "signal-off" response, which enhanced the sensitivity of the sensor. The PEC biosensor showed a linear response range from 10-12 to 10-6 g mL-1 with a detection limit of 0.023 pg mL-1, providing a feasible approach for the quantitative detection of AFB1 in food samples.

CRISPR/Cas12a-Derived Photoelectrochemical Aptasensor Based on Au Nanoparticle-Attached CdS/UiO-66-NH2 Heterostructures for the Rapid and Sensitive Detection of Ochratoxin A.

The sensitive and accurate detection of ochratoxin A (OTA) is crucial for public health due to its high toxicity. Herein, using Au nanoparticle (NP)-attached CdS/UiO-66-NH2 heterostructures as photoactive materials, a photoelectrochemical (PEC) aptasensor was presented for the ultrasensitive assay of OTA based on a competitive displacement reaction triggering the trans-cleavage ability of CRISPR/Cas12a. In this sensing strategy, methylene blue-labeled single-stranded DNA (MB-ssDNA) was immobilized on the Au NPs/CdS/UiO-66-NH2 electrode to accelerate the separation of the photogenerated carrier, thus producing a significantly increased PEC response. In the presence of OTA, it specifically bound with the aptamer (Apt) and resulted in the release of the activation chain, triggering the trans-cleavage characteristics of CRISPR/Cas12a. MB-ssDNA was cut randomly on the electrode surface to convert the PEC signal from the "on" to the "off" state, thereby achieving a quantitative and accurate detection of OTA. The CRISPR/Cas12a-derived PEC aptasensor exhibited excellent sensitivity and specificity, with a linear range from 100 to 50 ng/mL and a detection limit of 38 fg/mL. Overall, the proposed aptasensor could provide a rapid, accurate, and sensitive method for the determination of OTA in actual samples.

Photocatalytic degradation of butyl benzyl phthalate by S-scheme Bi/Bi2O2CO3/Bi2S3 under simulated sunlight irradiation

As a kind of plasticizer, butyl benzyl phthalate (BBP) presents a serious hazard to the ecosystem. Therefore, there is a strong need for an effective technique to eliminate the risk of BBP. In this work, a new photocatalyst of Bi/Bi2O2CO3/Bi2S3 with an S-scheme heterojunction was synthesized using Bi(NO3)3 as the Bi source, Na2S as the S source, and DMF as the carbon source and reductant. Numerous techniques have been used to characterize Bi/Bi2O2CO3/Bi2S3, such as scanning electron microscopy, high-resolution transmission electron microscopy, X-ray diffraction, and X-ray photoelectron spectroscopy. The improved photoactivity of Bi/Bi2O2CO3/Bi2S3 was evaluated by photoelectrochemical response, electrochemical impedance spectroscopy, photoluminescence, UV–Vis diffuse reflectance spectroscopy, and electrochemical Mott Schottky spectroscopy. The enhanced photocatalytic activity of this composite for BBP degradation under simulated sunlight irradiation could be attributed to the surface plasmon resonance effect of Bi metal and the heterojunction structure of Bi2O2CO3 and Bi2S3. The degradation rate of Bi/Bi2O2CO3/Bi2S3 was 85%, which was 4.52 and 1.52 times that of Bi2O2CO3 and Bi2S3, respectively. The prepared photocatalyst possessed good stability and reproducibility in eliminating BBP. The improved photocatalytic activity of Bi/Bi2O2CO3/Bi2S3 was demonstrated with the formation of an S-scheme heterojunction, and the degradation mechanism was discussed with a liquid chromatograph mass spectrometer.