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Unveiling the enhanced activity origin of BiO1-xCl/C3N5 photocatalyst in CO2-to-CO directional conversion
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Zhilei Chena, Zhaoxia Lia, Yunjiang Yub, Mingdeng Xiangb, Cheng Dinga, Entian Cuia, Jizhou Jiangc, d
Chinese Chemical Letters | 2026, 37(9) : 112313
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Chinese Chemical Letters | 2026, 37(9): 112313
• Communication •
Unveiling the enhanced activity origin of BiO1-xCl/C3N5 photocatalyst in CO2-to-CO directional conversion
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Zhilei Chena, Zhaoxia Lia, Yunjiang Yub, Mingdeng Xiangb, Cheng Dinga, Entian Cuia, Jizhou Jiangc, d
Affiliations
  • aSchool of Environmental Science and Engineering, Key Laboratory for Advanced Technology in Environmental Protection of Jiangsu Province, Yancheng Institute of Technology Yancheng, Yancheng 224051, China
  • bKey Laboratory of Environmental Pollution Health Risk Assessment, Ministry of Ecology and Environment of the People's Republic of China, South China Institute of Environmental sciences, Guangzhou 510655, China
  • cSchool of Materials Science and Engineering, State Key Laboratory of Green and Efficient Development of Phosphorus Resources, Engineering Research Center of Phosphorus Resources Development and Utilization of Ministry of Education, Key Laboratory of Green Chemical Engineering Process of Ministry of Education, Hubei Key Laboratory of Plasma Chemistry and Advanced Materials, Novel Catalytic Materials of Hubei Engineering Research Center, Wuhan Institute of Technology, Wuhan 430205, China
  • dCollege of Chemistry and Molecular Sciences, Wuhan University, Wuhan 430072, China
About Author:

CRediT authorship contribution statement

Zhilei Chen: Writing – original draft, Visualization, Validation, Software, Resources, Methodology, Investigation, Formal analysis, Data curation.

Zhaoxia Li: Writing – original draft, Validation, Software, Resources, Methodology, Investigation, Formal analysis, Data curation.

Yunjiang Yu: Writing – original draft, Validation, Resources, Methodology, Investigation, Formal analysis, Data curation.

Mingdeng Xiang: Writing – original draft, Resources, Methodology, Investigation, Formal analysis.

Cheng Ding: Writing – review & editing, Supervision, Software, Resources, Project administration, Methodology, Investigation, Funding acquisition, Formal analysis, Data curation.

Entian Cui: Writing – original draft, Validation, Software, Resources, Project administration, Methodology, Investigation, Funding acquisition, Formal analysis, Data curation.

Jizhou Jiang: Writing – review & editing, Visualization, Validation, Supervision, Software, Resources, Project administration, Methodology, Investigation, Funding acquisition, Formal analysis, Data curation, Conceptualization.

Published: 2026-09-15 doi: 10.1016/j.cclet.2025.112313
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The structure of photocatalysts largely determines the selectivity of CO2 conversion products in CO2 photoreduction reaction, while it is dynamic during the photoreaction. Therefore, how the dynamic structure affecting photoactivity deserves further investigation. Herein, with defective oxygen vacancies BiOCl/C3N5 nanosheets heterojunction (BiO1-xCl/C3N5) as model photocatalyst, the structure dynamic evolution in CO2 photoreduction reaction and its influence on the CO2-to-CO directional conversion were investigated. Specially, in BiO1-xCl/C3N5, the exposed Bi atoms adjected oxygen vacancies interacted with N atoms of C3N5 via the strong electrostatic effect, resulting in the shrinking crystalline structures. Once illuminated, the photogenerated electrons enriched on Bi active sites, which further strengthened the interfacial interaction between BiO1-xCl and C3N5 to a quasi-bonding state. The resulting changes in electronic structure destroyed the linear structure of CO2 molecule pre-adsorbed on Bi sites, accompanying with transformation of Bi atom valence states and heterostructure restoration. As a result, the *CO2 molecule activation and *CO intermediate desorption barrier energies both reduced, promoting the CO2-to-CO directional conversion with a CO evolution rate of 207.3 μmol g−1 h−1. This work demonstrated the importance of studying the structural dynamics evolution in photoreactions, which may be beneficial for future photocatalyst design.

Photocatalysis  /  CO2 reduction  /  Composite catalyst  /  Structure dynamic evolution  /  In-situ characterization
Zhilei Chen, Zhaoxia Li, Yunjiang Yu, Mingdeng Xiang, Cheng Ding, Entian Cui, Jizhou Jiang. Unveiling the enhanced activity origin of BiO1-xCl/C3N5 photocatalyst in CO2-to-CO directional conversion[J]. Chinese Chemical Letters, 2026 , 37 (9) : 112313 - . DOI: 10.1016/j.cclet.2025.112313
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Solar-driven CO2 reduction now is a promising technology to solve the environmental problem and energy crisis [1,2]. The carbon-contained products were various, and among them, carbon monoxide (CO) is a momentous constituent for bulk chemical manufacturing. Therefore, the photocatalytic CO2-to-CO conversion with high activity and selectivity is highly sought after. However, the dissociation energy of the C═O bond in CO2 molecules is as high as 750 kJ/mol, which makes the CO2 photoreduction an arduous reaction [3,4]. Up to now, the reported CO yields and selectivity in CO2 photoreduction reaction were relatively low [5,6], which greatly restricted the application of solar-driven CO2 reduction technology. Seeking a high-performance photocatalyst for CO2-to-CO directional conversion is the hotspot and difficulty in the photocatalytic field.
Recently, bismuth-based materials, such as Bi2O3 [7,8], BiOBr [9,10], BiOI3 [11,12], and BiOCl [13,14], have been proved to be promising photocatalysts for their unique electronic structures and layered crystal structures. Among them, BiOCl has received widespread attention [15–17]. However, its solar-to-fuel efficiency is restricted greatly by its wide band gap. Various strategies have been tried to improve the photocatalytic activity of BiOCl, such as exposed facets regulation [18–20], heterojunction configuration [21,22], (non)metal doping [23,24], and so on. Recently, studies have suggested that introducing oxygen vacancies in heterojunction structure can efficiently promote the photocatalytic performance [25–27]. Nevertheless, despite considerable efforts devoted to improving the performances of BiOCl-based heterojunction photocatalysts, the intrinsic mechanisms currently remain ambiguous.
In CO2 photoreduction reaction, the ultimate photocatalytic performance is a result of multiple factors working together, such as the photocarrier-separation efficiency, the adsorption type of CO2 molecules, the activation energy of CO2 molecules, and the *CO intermediates formation energy. Studies have shown that affected by the reaction environment, the surface structure and interface structure of photocatalysts were dynamically changing [28,29], which caused the changes in surface atomic configuration, electronic structure, and spatial distribution of active sites. For instance, by the selective photo-deposition of PtOx species on BiOIO3 surface, under light irradiation, the surface adsorbed CO2 molecules transformed into *CO intermediates, leading to the emergence of Bi3+ species and the expansion of crystalline structure of BiOIO3 nanocrystals [12]. Furthermore, the Pt1-ZnIn₂S₄@CoOx system underwent a hole-induced oxidative self-reconstruction of CoOx, which continuously scavenged photogenerated holes and effectively suppressed photocorrosion. Consequently, it achieved hydrogen evolution rates of 23.88 mmol g−1 h−1 in natural seawater and 48.99 mmol g−1 h−1 in deionized water [30]. Therefore, investigating the dynamic evolutions of crystal structure of BiOCl-based materials in CO2 photoreduction process and its fluence on the photocatalytic activity is a reasonable way to explore the essence of CO2 photoreduction reaction, which is also beneficial for the rational designs of efficient CO2 reduction photocatalysts.
Herein, by adopting quasi in-situ characterization techniques, we explored the dynamic structure and chemical-state variations on BiO1-xCl/C3N5 in CO2 photoreduction process with BiO1-xCl and BiOCl/C3N5 counterparts for comparison. The related studies clearly revealed that in BiO1-XCl/C3N5, electron offset could efficiently be promoted from interfacial N atoms to Bi atoms, inducing intimate interface contact and strengthening the adsorption of CO2 molecules. It resulted in the low oxidation state Bi atoms and the local contraction of BiO1-xCl structures. Under light irradiation, the interface interaction was further enhanced, which promoted the activation of CO2 molecule and the interfacial electron transport. Owing to the photoinduced electrons enrichment on interface Bi sites, the adsorbed CO2 molecules were transformed into *CO intermediates with the expansion of crystalline structures. As expected, BiO1-xCl/C3N5 exhibited the highest CO2-to-CO conversion performance in comparison to BiO1-xCl and BiOCl/C3N5. These findings might provide a feasible strategy to elucidate the dynamic evolution process of catalytically active sites for the significantly enhanced CO2-to-CO directional conversion, which offers new insights for the fabrication of highly efficient CO2 photo-reduction catalysts.
BiO1-xCl was prepared via a simple hydrothermal process [31]. Bi(NO3)3·5H2O (1 g) was first dissolved in 25 mL of ethylene glycol and stirred for 30 min to ensure the complete dissolution. After that, 5 mL of saturated NaCl solution was added. After stirring for another 60 min, the mixture was transferred into a 100 mL hydrothermal autoclave and kept at 160 ℃ for 5 h. The BiO1-xCl product was collected after washing, centrifugation, and freeze-dried treatment.
5-Amino-1,2,4-triazole (5 g) and NH4Cl (5 g) were milled to form an inhomogeneous solid mixture and then was treated at 550 ℃ for 3 h with a heating rate of 10 ℃/min. The product was naturally cooled and the obtained sample was bulk C3N5.
Bulk C3N5 (1 g) was processed into 40 mL of concentrated H2SO4 with continuous stirring for 12 h. The yellowish product was washed to neutral by deionized water and then dried under vacuum at 60 ℃ for 12 h.
The synthesis procedure of BiO1-xCl/C3N5 was similar to that of BiO1-xCl, except a certain amount of prepared C3N5 nanosheets was injected into the mixture solution of Bi(NO3)3·5H2O and ethylene glycol.
Sample morphology was measured by transmission electron microscopy (TEM, FEI Tecnai TF20). XRD pattern was collected by X'Pert PRO, PANalytical with a scanning rate of 0.06°/s. The chemical valence and elemental composition of the catalyst surface were determined by ESCALAB 250 Xi X-ray photoelectron spectroscopy. UV–vis diffuse reflectance spectra were characterized on a UV-2550 (Shimadzu) spectrometer. Both steady and time-resolved Photoluminescence (PL) spectra were recorded on Fluorescence Spectrophotometer F-7000 and HORIBA FL-3, respectively. EPR measurements were recorded using Bruker EMX nano.
The synchronous irradiation X-ray diffraction (SI-XRD) was performed using a 300 W xenon lamp as the light source to record XRD data before and after CO2 adsorption as well as light irradiation. The CO2-preadsorption process was presented in Fig. S1 (Supporting information). Specially, after being made into thin sheets with suitable size, the photocatalyst was placed in a sealed adsorption chamber and purged with Ar (50 mL/min) for 30 min to remove the surface adsorbed impurities. Subsequently, a mixture gas of CO2 and water vapor was introduced into adsorption chamber for 60 min. Finally, the import valve and export valve of sealed chamber were closed and kept it for 60 min at room temperature to reach the adsorption equilibrium.
In-situ diffuse reflectance Fourier transform infrared spectroscopy (SI-DRIFTS) was carried out on a Bruker VERTEX 70 infrared spectrometer with a 300 W Xe lamp (PLS-SXE300, Perfectlight Technology Co, Ltd., Beijing) as light source. A mixed atmosphere (CO2 + H2O vapor) was injected into the reactor for 30 min at room temperature. After reaching the sorption equilibrium, SI-DRIFTS data were recorded under alternating dark and light conditions.
Synchronous irradiation X-ray photoelectron spectroscopy (SI-XPS): The synchronous irradiation X-ray photoelectron spectroscopy (SI-XPS) instrument was equipped with a 300 W Xe lamp as light source. Before SI-XPS measurements, after being made into thin sheets with suitable size, the photocatalyst was placed in a sealed adsorption chamber and purged with Ar (50 mL/min) at 120 ℃ for 30 min to remove the surface adsorbed impurities. Subsequently, a CO2/H2O (vapor) was purged into the chamber at room temperature for 20 min to reach the adsorption equilibrium. Finally, the as-prepared samples were quickly transferred to the analysis chamber of XPS instrument (ESCALAB 250Xi) for the SI-XPS measurements. The variations of XPS spectra were recorded by controlling light irradiation (on or off). The CO2-preadsorption process was presented in Fig. S1.
The photocatalytic CO2 reduction activity was carried out under the irradiation of 300 W Xe lamp (PLS-SXE300, Perfectlight Technology Co, Ltd., Beijing) equipped with a 420 nm cutoff filter (Perfect Light, Microsolar 300, 420–780 nm). In a typical reaction, 100 mg samples were dispersed uniformly in pure water. The hybrid suspension was then transferred into the tailor-made vessel. Before irradiation, ultrahigh purity CO2 (99.999%) gas was bubbled into the suspension at 300 mL/min for 30 min to remove air and saturate the solution. The reactor temperature was kept at 25 ℃ with a cooling water circulator. After 5 h magnetic stirring under light irradiation, the suspension was centrifuged to collect the catalyst. The products were analyzed using Agilent GC 6890 N gas chromatograph with thermal conductivity and flame ionization detectors.
For comparison, the CO2 photoreduction performance with sacrificial reagent MeCN addition was also carried out. The testing procedure was similar with MeCN solution replacing pure water.
In isotopic labeling experiment, 13CO2 gas was employed instead of 12CO2 gas as the carbon source, and H218O was utilized instead of H216O. The gas products were measured by GC–MS spectrometry.
The photoelectrochemical data were all measured by a three-electrode photoelectrochemical cell with sample photoelectrode as working electrode, Pt sheet as counter electrode, and Ag/AgCl as reference electrode. Additionally, the electrolyte solution and light source were 0.2 mol/L Na2SO4 (pH 6.8) solution and 300 W xenon lamp, respectively. The working electrode was prepared as following: Catalyst powder (5 mg) was dispersed into 250 μL of isopropanol, 750 μL of H2O and 20 μL 5% Nafion, and then sonicated for 30 min. 50 μL of the sample mixture was drop-coated onto FTO glass and dried at 60 ℃ to obtain working electrode.
All DFT calculations data was obtained by using the Quantum Espresso code [32]. The exchange-correlation energy was approximated by the generalized gradient approximation with the Perdew-Burke-Ernzerhof (PBE) functional. A 500 eV plane-wave kinetic energy cutoff was chosen. Geometry optimization was conducted with the Brillouin zone. The atomic positions were fully relaxed until a maximum energy difference and residual force on atoms, respectively. The vacuum slab of 15 Å was added to prevent the periodic interference of the unit cell.
Fig. 1a illustrated the basic synthetic procedure for in-situ growth of oxygen vacancies BiOCl on C3N5 nanosheets (BiO1-xCl/C3N5). As a new type of N-rich carbon nitride, C3N5 was chosen for its azo-linked structure, which has been proven to be ideal support to metal atoms. Additionally, it exhibited a enhanced visible-light response to provide photo-generated charge carriers [33]. Briefly, C3N5 nanosheets have been obtained by previously reported method [34], which were subsequently used as the in-situ growth substrate for BiO1-xCl nanoparticles. The XRD pattern of C3N5 presented a main characteristic peak at 27° (Fig. 1b) [33]. The absence of a (100) peak, a specific feature of in-plane packing, suggests the distortion of C3N5 framework and the broadening of nanochannel distance between heptazine units due to azo (–N═N–) bridging linkage [33,35,36]. Also, both BiOCl and BiO1-xCl were the tetragonal structure (JCPDS No 06-0249) (Fig. 1b and Fig. S2 in Supporting information). Notably, the oxygen vacancies treatment did not damage the crystalline structure of BiOCl. In BiO1-xCl/C3N5 heterojunction, the XRD peaks of BiO1-xCl and C3N5 were clearly observed. As shown in Fig. 1, Fig. 1, BiO1-XCl nanosheets were junctionalized with C3N5, confirming the formation of heterojunction structure. The spacing value of 0.275 nm was assigned to the BiO1-xCl (110) plane (Fig. 1e), which showed an obvious boundary line with C3N5 (Fig. 1e). The uniformly distributed C, O, Bi, Cl, and N elements were the directional evidence for the tight heterojunction interface between BiO1-xCl and C3N5 (Fig. 1f).
The defective nature of BiO1-xCl/C3N5 was verified via EPR spectra (Fig. 1g). Usually, the typical peak of vacancies at g = 2.004 was the signal for oxygen vacancies [37,38]. In comparison of BiOCl, BiO1-xCl showed a stronger signal, indicating the successful introduction of oxygen vacancies [13]. Interestingly, the intensity of BiO1-xCl/C3N5 showed no obvious different to that of BiO1-xCl, probably due to the absence of the authentic bonding effect between BiO1-xCl and C3N5 components. The result of Raman spectra further proved the existence of oxygen vacancies in BiO1-xCl/C3N5. As shown in Fig. 1h, BiOCl showed the characteristic peaks at 61, 143, 198, and 397 cm−1, which were assigned to active modes of A1g, A1g, B1g, and 2Eg, respectively [39]. These peaks of BiO1-xCl were much weaker and slightly shifted to lower wavenumbers direction, suggesting the existence of abundant oxygen vacancies and metallic Bi [40]. The combination of C3N5 component did not change the oxygen vacancy concentration for the no obvious change peak intensities in BiO1-xCl/C3N5.
The XPS survey spectra of BiO1-xCl/C3N5 consisted of Bi, O, Cl, C, and N elements (Fig. S3 and Table S1 in Supporting information), suggesting the heterojunction structure of BiO1-xCl/C3N5. Fig. 2a presented the O 1s spectra. For BiO1-XCl, the peak at 529.8 eV was the crystal lattice O of [Bi2O2]2+ crystal structure [41,42], and the peak at 531.9 eV originated from the oxygen vacancies [43,44]. The ~0.14 eV binding energy shifting between BiO1-xCl and BiO1-xCl/C3N5 was from the interface interaction in BiO1-xCl/C3N5. Similar conditions were also be detected on C 1s and Cl 2p spectra (Figs. S4 and S5 in Supporting information). Referring to Fig. 2b, two peaks at 158.9 and 164.4 eV in BiO1-xCl corresponded to Bi3+ 4f5/2 and 4f7/2, respectively. While in BiO1-xCl/C3N5, both peaks shifted down by ~0.16 eV for the increase in electron density of Bi atoms [45]. Correspondingly, the N 1s exhibited an opposite change. In BiO1-xCl, the peaks of two-coordinated (N2C) and three-coordinated (N3C) were detected at 398.5 and 399.8 eV, respectively (Fig. 2c) [33]. After constructing C3N5 component, these peaks shifted up by ~0.19 eV, indicating that the decrease in electron density in N nucleus. Thus, in BiO1-xCl/C3N5, the electrons shifted from the N atoms to Bi atoms. The similar situation was not detected in BiOCl/C3N5 counterpoint (Figs. S6 and S7 in Supporting information). Nevertheless, no peaks belong to Bi-N bond was detected in both Bi 4f (163.4 eV) and N 1s (398.18 eV) XPS spectra [46], which suggested in BiO1-xCl/C3N5 heterojunction, BiO1-xCl and C3N5 was connected by the strong electrostatic effect [47,48]. In addition, with the introduction of high concentration oxygen vacancies, the band gap (Eg) of BiO1-xCl was narrowed to 2.81 eV from 3.44 eV of BiOCl, a distinctive feature of defect-containing semiconductors (Fig. 2d and Fig. S8 in Supporting information) [49]. Similarly, the Eg of C3N5 was 2.19 eV. Moreover, the valence band potentials (EVB) of C3N5 and BiO1-xCl were determined by VB-XPS with light illumination (SI-VB XPS). The EVB of C3N5 and BiO1-xCl were 1.31 and 2.16 eV, respectively (Fig. 2e). Meanwhile, the corresponding the ECB of C3N5 and BiO1-xCl were −0.88 and −0.65 eV, respectively. Based on the above analysis, the band structures of BiO1-xCl and C3N5 were depicted in Fig. 2f. It can be observed that BiO1-xCl/C3N5 met simultaneously the thermodynamic conditions for CO2 reduction and H2O oxidization.
Meanwhile, the weight ratios of BiO1-xCl and C3N5 in BiO1-xCl/C3N5 heterojunction had great influence on the photocatalytic CO2 conversion efficiency and CO selectivity. BiO1-xCl/C3N5 with 20 wt% BiO1-xCl loading showed the highest CO production rate (Fig. S9 in Supporting information) and selectivity (Fig. 3a). The CO production rate of BiO1-xCl/C3N5 was 207.3 μmol g−1 h−1 with a 96.1% selectivity (Fig. 3a), which was a 5.4-fold enhancement compared to that of BiOCl/C3N5. However, there was still a small amount of CO produced under the Ar atmosphere (Fig. S10 in Supporting information), which may be caused by the self-decomposition of C3N5 or added surfactants [50,51]. With sacrificial reagent addition, the CO evolution rate reached 1096.32 μmol g−1 h−1 (Fig. S11 in Supporting information). Furthermore, the obtained photocatalytic performance of BiO1-xCl/C3N5 was among the highest of reported works of Bi-based photocatalysis on CO2 photoreduction to date (Fig. 3b and Table S2 in Supporting information). Meanwhile, BiO1-xCl/C3N5 also exhibited excellent photocatalytic stability and structure stability (Fig. 3c, Figs. S12 and S13 in Supporting information)
Furthermore, the isotopic labeling experiment was conducted by using 13CO2 as a carbon source. As shown in Fig. 3d, the 13CO peak at m/z = 29 and 13COOH peak at m/z = 46 could be evidently detected in BiO1-xCl/C3N5 reaction system, confirming that CO should be produced from photocatalytic CO2 reduction instead of impurities or pollutants [52–54]. Additionally, the oxidation products have also been explored through the H218O isotopic labeling experiment. As illustrated in Fig. S14 (Supporting information), 18O (m/z = 18) and 18O2 (m/z = 36) were simultaneously detected, indicating that the O2 molecular product should be derived from water oxidation, which simultaneously provided electron/proton for CO2 reduction into CO.
To investigate the origins of the photocatalytic performance, the electron dynamic behaviors were studied first. As shown in Fig. 3e, BiO1-xCl/C3N5 displayed the highest photocurrent density compared to BiO1-xCl and BiOCl/C3N5, a result of the quicker charge transfer and separation rate after constructing the heterojunction. Meanwhile, similar conclusions were obtained from the electrochemical impedance spectroscopy (EIS). BiO1-xCl/C3N5 performed with the minimum radius (Fig. 3f), presenting that the fastest charge transfer rate and the lowest recombination ability of BiO1-xCl/C3N5 [55–57]. This was corroborated by the reduced photoluminescence (PL) intensity (Fig. 3g), where BiO1-xCl/C3N5 displayed significantly quenched signals compared to BiO1-xCl and BiOCl/C3N5, highlighting suppressed electron-hole recombination [58–60]. To probe the specific charge transfer dynamics, the TRPL spectra were collected (Fig. 3h and Table S3 in Supporting information). The lifetime decay curve was well fitted by a biexponential kinetic function (R2 > 0.98). The average carrier lifetime (τavg) of BiO1-xCl/C3N5 was 6.55 ns, which was much longer than these of BiO1-xCl (2.92 ns) and BiOCl/C3N5 (5.01 ns), indicating the lower recombination ratios during the charge carrier transfer process under the excitation state [61,62]. Note that the BiO1-xCl/C3N5 showed a longer lifetime than BiOCl/C3N5, which maybe from the strong interface interaction, a main reason for the enhanced CO2 photoreduction performance [63,64].
The effects of CO2 absorption under darkness and light excitation on the structural evolution of BiO1-xCl/C3N5 heterojunction were explored by synchronous irradiation X-ray diffraction (SI-XRD) technique [65]. As depicted in Fig. 4a, the CO2 adsorption on BiO1-xCl/C3N5 surface induced the evident shift of diffraction peaks toward the low D-spacing values, indicating that the shrinkage of crystalline structure owing to the electron deviated from BiO1-xCl/C3N5 to CO2 molecules. Similar phenomena could also be observed in BiOCl/C3N5 (Fig. 4b) and BiO1-xCl (Fig. 4c), respectively. Moreover, under light irradiation, the diffraction peaks of BiO1-xCl/C3N5 shifted to the high D-spacing direction, indicating that the formed intermediates induced the changes of crystalline structure in reverse. Similar phenomenon could be observed in the BiOCl/C3N5 with a smaller shift amplitude. However, no evident change could be observed on BiO1-XCl under light irradiation, revealing its relatively poor capability for the formation of reaction intermediates.
The reaction intermediates during CO2 photoreduction were determined by synchronous irradiation diffuse reflectance Fourier transform infrared spectroscopy (SI-DRIFTS). Under the darkness, compared to BiO1-xCl and BiOCl/C3N5, BiO1-xCl/C3N5 presented a much higher CO2 adsorption peak (~2300–2400 cm−1) and H2O adsorption peak (~1600–1700 cm−1) (Fig. S15 in Supporting information), which revealed that the surface of BiO1-xCl/C3N5 was more favorable for the adsorption of CO2 molecules [66]. Upon light irradiation on BiO1-xCl/C3N5, the peaks at 1504, 1531, and 1267 cm−1 assigned to *CO2 intermediates could be evidently detected in Fig. 4d. Interestingly, the emergence of *COOH at 1698 cm−1 indicated the protonation of *CO2 [67,68], which was the key for CO2-to-CO conversion [69,70]. With increasing irradiation time, the peaks of *CO intermediates could be detected evidently. By comparison, the *CO peaks on BiO1-xCl and BiOCl/C3N5 were much smaller, which confirmed the low CO production efficiencies of BiO1-xCl and BiOCl/C3N5 (Fig. 4e and f).
Moreover, the dynamic evolutions of chemical bonds and electronic structures of BiO1-xCl/C3N5 during CO2 reduction process were studied via synchronous irradiation X-ray photoelectron spectroscopy (SI-XPS) (Fig. 5 and Table S4 in Supporting information) [38,71,72]. After CO2 absorption (Fig. 5a), the peaks at 289.3 and 286.2 eV in C 1s XPS spectrum can be indexed to *CO2 and *CO intermediates originating from the adsorption and dissociation of CO2 molecules [12]. Additionally, the slight peak at 290.8 eV indexed to carbonate species (CO32−), which was consistent with the DRIFTS results. Simultaneously, two evident peaks at 166.7 and 166.0 eV in Bi 4f spectrum should be attributed to *CO and *CO2 species on exposed Bi active sites (Fig. 5b). Under light irradiation, the intensities of CO32− and *CO2 peaks decreased evidently in C 1s region, while *CO peak increased obviously, indicating the dissociation of CO2 molecules. Simultaneously, an evident decrease in Bi-CO2* peak accompanying with increase in Bi-CO* peak was detected in Bi 4f spectrum. As illustrated in Fig. 5c, the O 1s peaks can be fitted into six peaks at 534.7, 533.3, 532.2, 531.9, 531.5, and 530.4 eV, which were assigned to H2O, O═C, OH, Ov, O–C, and lattice O, respectively. Upon light irradiation, the intensities of H2O and O═C peaks decreased evidently, while OH and O–C peaks increased obviously, revealing the dissociation of CO2 and H2O molecules over the BiO1-xCl/C3N5 surface. More importantly, all these chemical states and bond evolutions were dynamically reversible by controlling the light or dark conditions (Figs. 5d–f). Furthermore, Ar ion etching has been performed to remove the adsorbed CO2 molecules, and all the related changes have been disappeared (Figs. 5g–i, Fig. S16 and Table S5 in Supporting information), further confirming the effects of adsorption and dissociation of CO2 on the above chemical states and bond evolutions. For comparison, the related experiments of CO2 adsorption have also been performed on BiO1-xCl and BiOCl/C3N5, respectively. As illustrated in Figs. S17 and S18 (Supporting information), both BiO1-xCl and BiOCl/C3N5 exhibited the relatively low CO2 adsorption peaks compared with BiO1-xCl/C3N5, while no significant bond evolution could be detected, demonstrating the relatively poor CO2 reduction capability. Therefore, the combination of C3N5 and BiO1-xCl could effectively promote the adsorption of CO2 molecules owing to the electron enrichment on Bi active sites. Under light illumination, the adsorbed *CO2 molecules were transformed into *CO intermediates with the transformation of high oxidation state Bi atoms to Bi3+.
Furthermore, the surface charge distribution has been investigated by surface photovoltage (SPV) measurements. Fig. 5j confirmed that the light excitation induced the significant variations of surface potential, and the surface potential of BiO1-xCl/C3N5 was >138 mV, which was much higher than these of BiOCl/C3N5 (~74 mV) and BiO1-xCl (~32.5 mV) (Fig. 5k and l). Therefore, BiO1-xCl/C3N5 effectively promoted the charge separation, photoinduced electron migration, and CO2 adsorption.
The radicals during CO2 photoreduction are also the keys to unveil the reaction mechanism, which were investigated via the in-situ EPR spectra. As shown in Figs. 6a and b, the drastically reduced TEMPO signal and the increased DMPO–OH signal demonstrated that BiO1-xCl/C3N5 produced more photogenerated electrons and promoted more H2O molecules dissociation under light illumination. When CO2 was continually injected into BiO1-xCl/C3N5 system, the TEMPO signal showed no obvious changes during irradiation (Fig. 6c), suggesting that the photoinduced electrons were largely captured by CO2 during photoreduction [73]. Also, even though CO2 was injected, no any DMPO–OH signal was detected in BiO1-xCl/C3N5 system under dark, while switching to light illumination, DMPO–OH signal appeared and was higher with the illumination time prolonging (Fig. 6d), revealing the indispensable role of light in promoting water hydrolysis. Consequently, the CO2 reduction process was promoted by the protons and photoinduced electrons (CO2 + 2e− + 2H+ → CO + H2O). As a result, the ample photoinduced electrons and protons endowed BiO1-xCl/C3N5 favorable CO2 photoreduction performance.
Temperature-programmed desorption (TPD) experiments were performed to study the interactions between BiO1-xCl/C3N5 and the reaction gases CO2 and the product CO. The maximum CO2 desorption temperature of BiO1-xCl/C3N5 was 400.8 ℃, which was higher than these of BiO1-xCl (346.1 ℃) and BiOCl/C3N5 (323.7 ℃), demonstrating the stronger interaction between CO2 molecules and BiO1-xCl/C3N5 (Fig. S19 in Supporting information). In contrast, BiO1-xCl/C3N5 exhibited lower maximum CO desorption temperature (316.2 ℃) compared to BiO1-xCl (350.2 ℃) and BiOCl/C3N5 (328.7 ℃) (Fig. S20 in Supporting information), which illustrated that the CO molecules were more easier to release from BiO1-xCl/C3N5 [16,74]. Consequently, the CO2-to-CO conversion was enhanced in BiO1-xCl/C3N5 system.
The interface interaction of BiO1-xCl/C3N5 was studied theoretically with an electron introduction. As depicted in Fig. 6e, compared to BiOCl/C3N5, the C3N5 component on BiO1-xCl/C3N5 deformed obviously with a deformation energy of −2.26 eV, almost twice that of BiOCl/C3N5 (−1.19 eV). The obvious deformation energy difference may originate from the amplified interfacial interaction. Additionally, as a result of the stronger interfacial interaction, the distance between BiO1-xCl and C3N5 (2.31 Å) was shorter in comparison to that in BiOCl/C3N5 (2.79 Å), and the binding energy Eb in BiO1-xCl/C3N5 (−4.03 eV) was much smaller than that in BiOCl/C3N5 (−2.91 eV), showing the stronger interfacial interaction between C3N5 and BiO1-xCl (Fig. S21 in Supporting information).
Herein, the dynamic CO2 conversion on BiO1-xCl/C3N5 was simulated. To model CO2 adsorption on BiO1-xCl/C3N5, a CO2 molecule was placed above BiO1-xCls side. Five adsorption sites were designed (Fig. S22 in Supporting information), including Bi atom, Bi atom adjected Ov (Bi-Ov), O atom, Ov site, and Cl atom. Also, adsorption energy (Eads) was calculated as Eads = ECO2@BiO1-xCl/C3N5 − EBiO1-xCl/C3N5 − ECO2, where ECO2@BiO1-xCl/C3N5 was the CO2 adsorption energy on BiO1-xCl/C3N5. As a result, EBiO1-xCl/C3N5 and ECO2 referred to the energies of BiO1-xCl/C3N5 and a CO2 molecule, respectively. The Eads values for Bi, Bi-Ov, O, Ov, and Cl were −0.24, −0.32, −0.02, −0.14, and 0.15 eV, respectively. The Bi-Ov site was the most suitable site towards CO2 adsorption.
In order to identify the dynamic evolution of CO2 molecule on Bi-Ov site, one electron was introduced into the calculation models. As illustrated in Fig. 6f, after geometry optimization, the CO2 molecule adsorbed on Bi-Ov site induced the deformation of BiO1-xCl and C3N5 components in the interface, while there was no so obvious deformation in BiOCl/C3N5, implying the bigger interaction strength of CO2 on BiO1-xCl/C3N5. The CO2 molecule adsorbed on BiOCl/C3N5 showed no obvious deformation with a distance of 2.81 Å on BiOCl layer. While on BiO1-xCl/C3N5, the distance between CO2 molecule and BiO1-xCl layer was decreased to 2.53 Å. The CO2 molecule distorted with O═C═O angle of 135.12°, and C and O atoms formed Bi–C and Bi–O bonds with Bi atoms. By introducing an electron, the C–O bond in Bi–O–C–Bi group was stretched from 1.18 Å to 1.33 Å and the O═C═O angle was reduced to 128.06°, which indicated the approaching dissociation of CO2 molecule [16]. In summary, BiO1-xCl/C3N5 enhanced the interaction between exposed Bi atoms and CO2 molecules and then destructed the linear structure of CO2 molecules, thereby achieving the efficient activation of CO2 molecules.
From the energy aspect, the adsorption energy of CO2 molecules on BiO1-xCl/C3N5 surface was bigger compared to these on BiOCl/C3N5 and BiO1-xCl (Fig. 6g), revealing that oxygen vacancies in BiO1-xCl/C3N5 enhanced the interaction between electrons and CO2. While the adsorption energies (Ead*CO) of BiO1-xCl/C3N5 was smaller than that of BiOCl/C3N5, which demonstrated that *CO intermediates on BiO1-xCl/C3N5 was easier to release (Fig. 6h). Moreover, the free energy of H2O dissociation on BiO1-xCl/C3N5 was calculated to be ca. −0.52 eV, which was smaller than these of BiOCl/C3N5 (1.55 eV) and BiO1-xCl (−0.23 eV) (Fig. 6i), confirming that the BiO1-xCl/C3N5 accelerated H2O dissociation and facilitated proton-feeding [75]. Besides, the *H acquisition ability of BiO1-xCl/C3N5 provided the enough *H for the formation of *COOH intermediates, thereby enhancing the photocatalytic reduction process [76].
Gibbs free energies of the CO2 reduction elementary steps were performed (Fig. 6j). Generally, in CO2-to-CO conversion process, the *COOH and *CO intermediates were the keys [77]. The *COOH intermediates was first formed on Bi sites via the process of *CO2 + H+ +e− → *COOH, which was considered as the rate-determining step for the CO2-to-CO conversion [78]. The smallest *COOH formation energy on BiO1-xCl/C3N5 was from the compact heterojunction structure and optimized electron states. In the second hydrogenation step, *COOH was converted into *CO specie and remained absorbed on the catalyst surface. Owing to the negative energy for *CO intermediates desorption, the adsorbed CO molecules were easily to form product CO rather than the products involved with more than two-electron processes (such as CH3OH and CH4). From the above analysis, the CO2 reduction produced CO as the final product on BiO1-xCl/C3N5.
Based on the above demonstrations, a potential mechanism has been proposed to clarify the charge separation, electron transport, structure and bond evolutions over BiO1-xCl/C3N5 during the photocatalytic CO2 reduction. Firstly, the strong interfacial interaction enriched the electrons on Bi sites, facilitating the CO2 molecules adsorption. Subsequently, the strong electron-attracting ability of absorbed CO2 molecules pushed up the oxidation state of Bi atoms and the shrinkage of BiO1-xCl/C3N5 crystalline structures. Upon light illumination, the photoinduced electron further strengthened the interaction between CO2 molecule and Bi active site, which efficiently destroyed the linear structure of CO2 molecule, facilitating *CO2 to form *COOH intermediates. Then, *COOH was further reduced to *CO via reacting with proton and photoinduced electron. Finally, the *CO desorbed and formed CO gas, accompanying with the restoration of the crystalline structures of BiO1-xCl/C3N5. Thus, the dynamic structure and chemical state evolutions of BiO1-xCl/C3N5 during photoreaction were the main reasons for the high CO2-to-CO conversion.
In summary, using BiO1-xCl/C3N5 as a model photocatalyst in CO2 reduction, we revealed the strong relationship between dynamic structure evolution and photocatalytic performance. More specifically, owing to the combination of C3N5 and BiO1-xCl, the interface electron enriched on Bi sites, which effectively promoted the adsorption of CO2 molecules. Under light illumination, at the joint action of photoinduced electrons and protons, the adsorbed structure-twisted CO2 molecules were transformed into *CO intermediates, leading to restoration of crystalline structure and valence state of Bi active sites. As expected, BiO1-xCl/C3N5 photocatalyst exhibited excellent CO2-to-CO conversion activity with an CO evolution rate of 207.3 μmol g−1 h−1. These findings might help to reveal the origin of photocatalytic performance of catalysts during CO2 conversion and provide a new insight to design efficient and stable photocatalysts for CO2 reduction.
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doi: 10.1016/j.cclet.2025.112313
  • Receive Date：2025-10-22
  • Online Date：2026-10-27
  • Published：2026-09-15
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  • Received：2025-10-22
  • Revised：2025-12-08
  • Accepted：2025-12-22
Affiliations
    aSchool of Environmental Science and Engineering, Key Laboratory for Advanced Technology in Environmental Protection of Jiangsu Province, Yancheng Institute of Technology Yancheng, Yancheng 224051, China
    bKey Laboratory of Environmental Pollution Health Risk Assessment, Ministry of Ecology and Environment of the People's Republic of China, South China Institute of Environmental sciences, Guangzhou 510655, China
    cSchool of Materials Science and Engineering, State Key Laboratory of Green and Efficient Development of Phosphorus Resources, Engineering Research Center of Phosphorus Resources Development and Utilization of Ministry of Education, Key Laboratory of Green Chemical Engineering Process of Ministry of Education, Hubei Key Laboratory of Plasma Chemistry and Advanced Materials, Novel Catalytic Materials of Hubei Engineering Research Center, Wuhan Institute of Technology, Wuhan 430205, China
    dCollege of Chemistry and Molecular Sciences, Wuhan University, Wuhan 430072, China

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表12种不同金属材料的力学参数
科
Family		 属数
Number of
genus		 种数
Number of
species		 占总种数比例
Percentage of
total species (%)		 属
Genus		 种数
Number of
species		 占总种数比例
Percentage of total
species (%)
鹅膏菌科Amanitaceae 2 11 5.26 鹅膏菌属 Amanita 10 4.78
小菇科 Mycenaceae 2 12 5.74 丝盖伞属 Inocybe 5 2.39
多孔菌科 Polyporaceae 8 14 6.70 蜡蘑属 Laccaria 5 2.39
红菇科 Russulaceae 3 23 11.00 小皮伞属 Marasmius 6 2.87
小菇属 Mycena 11 5.26
光柄菇属 Pluteus 5 2.39
红菇属 Russula 17 8.13
栓菌属 Trametes 5 2.39
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