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Original Article
ARTICLE IN PRESS
doi:
10.25259/AJC_321_2026

Preparation of non-mestal boron-doped g-C3N5 composite for photocatalytic degradation of new fuchsin from wastewater

,
aIntelligent Construction School, Zhengzhou Business University, Zhengzhou, China

*Corresponding author: E-mail address: liu942846@126.com (Y. Liu)

Received: , Accepted: ,
© 2026 Arabian Journal of Chemistry - Published by Scientific Scholar
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This is an open-access article distributed under the terms of the Creative Commons Attribution-Non Commercial-Share Alike 4.0 License, which allows others to remix, transform, and build upon the work non-commercially, as long as the author is credited and the new creations are licensed under the identical terms.

Abstract

With the rapid development of industrialization, the treatment of organic dye wastewater has become an urgent environmental issue. To address the challenge of efficiently removing pollutants such as new fuchsin (NF), this study aims to enhance the photocatalytic performance of graphitic carbon nitride (g-C₃N₅) by mitigating its high recombination rate of photogenerated carriers. A non-metal boron-doped g-C3N5 composite (B/C3N5) is successfully synthesized via the high-temperature thermal polymerization method for photocatalytic degradation of the NF. The physicochemical properties of the B/C3N5 composite are characterized and analyzed, showing excellent photocatalytic degradation activity. The photocatalytic degradation performance of the B/C3N5 composite is improved compared to the g-C3N5 owing to the excellent separation efficiency of photogenerated carriers. NF degradation removal of B/C3N5 composite under visible light irradiation reaches the highest level of 97.36%, which is larger than that of C3N with the 70.98%. The apparent rate constant for photocatalytic degradation of NF is 0.0503 min-1, which is 4.98 times higher than that of the g-C₃N₅. Besides, the NF photocatalytic degradation process has excellent cyclic stability. The photocatalytic degradation mechanism analysis indicates that the N element vacancy defects are formed in the g-C3N5 structure, and unpaired electrons are generated after non-metal B doping. Besides, the vacant 2p orbitals and the delocalized π bonds of g-C3N5 form p-π electron delocalization, which promotes the transfer of photoelectrons and the separation of photogenerated carriers, contributing to NF photocatalytic degradation.

Keywords

Cyclic stability
Degradation
New fuchsin
Nitrogen-rich carbon nitride
Non-metal boron doping

1. Introduction

Environmental pollution and energy shortage are the two serious problems facing the world at present. With the acceleration of industrialization and the global population growth, industries such as printing, dyeing, pharmaceuticals, daily chemicals and leather have produced a large amount of organic pollutant wastewater, which generally has the characteristics of large water volume, high alkalinity, high chemical oxygen demand, high color and complex composition. In addition, mining, electroplating, printing, dyeing and other industries produce a large amount of heavy metal wastewater, which cannot be biodegraded [1-2]. Direct emissions without treatment will cause serious pollution to the water environment, which may severely endanger the survival of animals, plants and humans [3]. At present, industrial wastewater is mainly treated through methods such as adsorption, biological treatment, electrochemical, and membrane separation [4-5]. These methods generally have problems such as low efficiency, high cost and are prone to secondary pollution. Therefore, it is of great significance to find an appropriate wastewater treatment method.

Photocatalysis technology has been widely applied in the degradation of organic pollutants such as dyes and antibiotics [6]. Photocatalysis technology significantly relies on efficient and stable photocatalysts. Among many photocatalysts, the graphite phase carbon nitride (g-C3N4) has good chemical stability, easy to regulate morphology and energy band, and excellent photoelectrochemical performance, which has been widely used in organic pollutant degradation [7]. The g-C3N4 is synthesized by high-temperature thermal polymerization using melamine or urea [8]. However, the prepared g-C3N4 exhibits a blocky morphology, low specific surface area and low crystallinity [9]. In the g-C3N4 structure, the tertiary nitrogen atoms connecting the s-triazine ring do not participate in the composition of the lowest unoccupied molecular orbital and the highest occupied molecular orbital, which makes it difficult for the photoelectron to transfer between the two adjacent s-triazine rings [10]. Besides, the generated photogenerated carriers exhibit a high recombination probability, which greatly limits the photocatalytic activity and large-scale application of the g-C3N4 [11].

In recent years, research on nitrogen-rich graphitic carbon nitride (g-C₃N₅) has advanced significantly. The study has found that the properties of the g-C3N5 are similar to those of g-C3N4, exhibiting good photocatalytic degradation performance [12]. The basic structural units of the g-C3N5 are heptazine rings connected by tertiary nitrogen atoms and two triazine rings with different structures [13]. The p-orbital of the azo bond (-N=N-) in the structure is superimposed with π-π* electron delocalization. Therefore, the g-C3N5 has strong electron delocalization compared to the g-C3N4, which makes the g-C3N5 exhibit more extensive spectral absorption and a narrower band gap energy [14]. The energy band structure of the g-C3N5 can be regulated by the non-metallic element doping to further improve its photocatalytic activity. In addition, the defects will be formed in the g-C3N5 structure after doping a non-metallic element, resulting in conjugation delocalization and a large number of unpaired electrons [13]. The recombination of unpaired electrons and photogenerated holes in the valence band positions effectively inhibits the recombination of photoelectrons and photogenerated holes, which is conducive to improving photocatalytic activity [15]. Kang et al. (2026) modified the g-C3N5 with non-metal P for photocatalytic degradation of atrazine [16]. The non-metal P replaces carbon in the skeleton of the g-C3N5 to form a P-N chemical bond, which is served as an electron capture center to promote the separation of photogenerated carriers, achieving efficient photocatalytic degradation of the atrazine [16]. Chen et al. (2024) modified the g-C3N5 with O and S elements for catalytic degradation of chlortetracycline [17]. The degradation removal of the chlortetracycline reaches 91.2%, which is significantly higher than that of pure phase g-C3N5 [17]. Tang et al. (2024) modified the g-C3N5 with non-metallic B to degrade tetracycline [18]. The existence of the B doping achieves efficient separation of photogenerated carriers, contributing to the tetracycline degradation with degradation removal of 88.6% [18]. Sareshkeh et al. (2025) prepared the phosphorous-doped g-C3N5 for tetracycline photocatalytic degradation from wastewater with the removal nearly to 100% [19]. Kumaravel et al. (2026) prepared the Br-modified g-C3N5 heterostructure for photocatalytic degradation norfloxacin detoxification from wastewater, achieving the 95% removal [20]. Therefore, the method of the non-metallic element doping g-C3N5 is feasible for pollution removal from wastewater.

In this work, the non-metallic B-doped g-C3N5 (B/C3N5) composite is synthesized by high-temperature thermal polymerization using boric acid and 3-amino-1,2,4-triazole as raw materials for photocatalytic degradation of new fuchsin (NF) from wastewater. The NF photocatalytic degradation performance and the photocatalytic activity of B/C3N5 composite are studied. Non-metal B doping of g-C3N5 effectively promotes the separation of photogenerated carriers and enhances the fluorescence lifetime of photogenerated carriers, achieving efficient degradation of NF. The non-metallic B doping substitution site is the C atom in the C3N5 structure by x-ray photoelectron spectroscopy (XPS) characterization analysis, forming nitrogen vacancy defects. The unpaired electrons are generated, and unpaired electrons and photoelectrons are recombined, effectively inhibiting the recombination of photoelectrons and holes. The charge transfer mechanism and photocatalytic mechanism are analyzed by photoelectrochemical characterization, active group quenching and band structure analysis. Besides, the possible degradation pathways of NF are proposed through high performance liquid chromatography-mass spectrometry (HPLC-MS) analysis.

2. Materials and Methods

2.1. Materials

The 3-amino-1,2,4-triazole, boric acid, methanol, potassium bromide (KBr), barium sulfate (BaSO4) and isopropanol (IPA) were purchased from Sigma-Aldrich. 1,4-benzoquinone (p-BQ), disodium ethylenediaminetetraacetate (EDTA-2Na), ascorbic acid (AA), NF, naphthol (AR, 99.0%) and acetonitrile were purchased from Sigma-Aldrich. All chemicals were used directly without any purification treatment. Besides, all solutions were prepared using deionized water made in the laboratory.

2.2. Preparation of the B/C3N5 composite

The g-C3N5 and B/C3N5 composite was synthesized by high-temperature thermal polymerization. Firstly, 5.0 g of 3-amino-1,2,4-triazole and 0.01 g of H3BO3 were uniformly dispersed into 50 mL of deionized water, magnetically stirred for 1h. The obtained solvent was evaporated at 100°C, and the obtained solid powder was dispersed in a porcelain boat. Secondly, the obtained solid powder was heated in the vacuum tube furnace at 520°C (5°C/min) for 3 h. The obtained powder was washed and then dried at 80°C for 12 h to prepare the 1.00% B/C3N5 composite after heating. By changing the mass ratio of H3BO3 and 3-amino-1,2,4-triazole, the 1.25% B/C3N5 and 1.50% B/C3N5 composites were prepared. The g-C₃N₅ was synthesized via the same procedure using 3-amino-1,2,4-triazole without H₃BO₃. The characterization methods of the samples are in the supporting material. The preparation process of the B/C3N5 composite is shown in Figure 1.

The preparation process of the B/C3N5 composite.
Figure 1. The preparation process of the B/C3N5 composite.

2.3. Photocatalytic experiments

The NF photocatalytic degradation experiment was carried out in a CME-TLSX300UV photocatalytic reaction device (Beijing Zhongke Microenergy Co., Ltd.), with the 500 W of xenon lamp (λ>420 nm). Firstly, 50 mg B/C3N5 composite or the C3N5 was uniformly added into 200 mL NF solution with the initial pH of 5.0 and a concentration of 100 mg/L. The 1 M NaOH and 1 M HCl were used to adjust the pH value of the solution. The mixture solution was placed in a dark environment and magnetically stirred for 90 min to achieve the adsorption-desorption equilibrium before NF photocatalytic degradation. Secondly, the xenon lamp was turned on to simulate visible light for 60 min to irradiate the above NF aqueous solution. The light source was 15 cm away from the liquid level with an average light intensity of 60 μW·cm-2. The solution sample was taken every 10 min to test the remaining NF concentration after filtering using the Hitachi UV-1900i UV-visible spectrophotomete at the maximum absorption wavelength of 546 nm. According to the relationship between absorbance and concentration of Lambert-Beer’s law, the NF degradation removal was calculated by Formula (1).

(1)
ξ= 1− At A0 ×100%= 1− Ct C0 ×100%

The ξ and A0 are the NF degradation removal and absorbance of NF at the initial time, respectively. The At and C0 are the absorbance of NF at t time and the initial NF concentration (mg·L-1). While the Ct is the NF concentration at t time (mg·L-1).

After NF degradation, the sample was recycled, and washed using the deionized water and anhydrous ethanol to wash alternately for three times. And then the sample was dried at 65°C for 12 h. The dried sample was used to evaluate its recycling stability in the NF photocatalytic degradation system. In the reactive group quenching experiment, 0.15 mmol/L p-benzoquinone(p-BQ), IPA and triethanolamine (TEOA) were added to quench the generated ·O2-, ·OH and h+ in the NF photocatalytic degradation system, respectively. And then the role of the reactive group was analyzed in the NF photocatalytic degradation system.

3. Results and Discussion

3.1. X-ray diffraction (XRD) and Fourier transform infrared spectroscopy (FT-IR) analysis

The phase crystallography of the g-C3N5 and B/C3N5 composites with different B doping contents is characterized by XRD (Figure 2(a)). As shown in Figure 2(a), the (100) and (002) crystal planes of the C3N5 appear at 2θ=12.7° and 27.5°, respectively. The (100) plane relates to the triazine ring, while the (002) plane relates to the stacked conjugated aromatic CN heterocycles [21]. The diffraction peaks of the B/C3N5 composite are consistent with g-C3N5. With the B doping content increasing, the diffraction peak intensity of B/C3N5 composites gradually decreases, and the (002) crystal plane diffraction peak slightly shifts toward a lower diffraction angle. This result indicates that the B doping induces lattice distortion in g-C3N5, resulting in a decrease in crystallinity. This is primarily because the atomic radius of B is larger than that of C and N atoms. After B atom doping, the interlayer spacing of the conjugated aromatic carbon-nitrogen heterocyclic ring increases [22]. The crystallinity can be evaluated by the ratio R of the height to full width at half maximum of (002) crystal plane diffraction peak [23]. The R values of the g-C3N5, 1.00% B/C3N5, 1.25% B/C3N5, and 1.50% B/C3N5 are 1.42, 1.36, 1.31, and 1.27, respectively. This result further demonstrates that increasing B doping content gradually reduces the crystallinity of the g-C3N5. In addition, no additional impurity peaks are observed after B doping, indicating that the B/C3N5 composite exhibits excellent purity.

(a) XRD and (b) FT-IR spectra of C3N5 and B/C3N5 composites with different B doping contents.
Figure 2. (a) XRD and (b) FT-IR spectra of C3N5 and B/C3N5 composites with different B doping contents.

The functional groups of g-C3N5 and B/C3N5 composites with different B doping contents are characterized by FT-IR (Figure 2(b)). The absorption peaks at 1200-1700 cm-1 are attributed to the stretching vibration of the CN heterocycle formed by C-N and C=N bonds. The peak at 890 cm-1 is assigned to the bending vibration of the heptazine ring, while the peak at 809 cm-1 originates from the bending vibration of the triazine ring [24]. As the B doping content increases, the absorption peaks’ intensities in the 809, 890, and 1200-1700 cm-1 ranges gradually decrease. This result suggests that the B doping may have altered the structure of the CN heterocycle in g-C3N5 due to overlap with the absorption peaks of B-N stretching and bending vibrations [25]. However, no obvious B-N and B-C absorption peaks are observed, likely attributable to the low boron doping concentration.

3.2. Morphology and specific surface area analysis

The microstructures of the g-C3N5 and B/C3N5 composites with different ratios are observed by scanning electron microscopy (SEM) and transmission electron microscopy (TEM) images (Figure 3). As Figure 3(a) shown, the g-C3N5 exhibits a blocky morphology with noticeable agglomeration. As shown in Figures 3(b-d), B/C3N5 composites exhibit an irregular porous layered stacking structure, the pore structure of g-C3N5 becomes progressively more distinct with increasing non-metallic B doping content, which is conducive to enhancing its specific surface area. The formation of a strong B-N covalent bond induces local contraction, leading to a reduction in interlayer spacing and strengthened interlayer interaction, which in turn causes pore blockage and collapse. As Figures 3(e-f) show, the g-C3N5 exhibits a two-dimensional nanosheet morphology. While, the 1.25% B/C3N5 composite displays a two-dimensional nanosheet morphology with a distinct porous structure. The elemental mapping of the 1.25% B/C3N5 composite reveals the element distribution of the C, N, and B elements (Figure 3(g).

SEM images of (a) g-C3N5, (b) 1.00% B/C3N5, (c) 1.25% B/C3N5, and (d) 1.50% B/C3N5 composite, TEM images of (e) g-C3N5, (f) 1.25% B/C3N5 composite and (g) Elemental mapping of 1.25% B/C3N5 composite.
Figure 3. SEM images of (a) g-C3N5, (b) 1.00% B/C3N5, (c) 1.25% B/C3N5, and (d) 1.50% B/C3N5 composite, TEM images of (e) g-C3N5, (f) 1.25% B/C3N5 composite and (g) Elemental mapping of 1.25% B/C3N5 composite.

The pore structure analysis of the g-C3N5 and B/C3N5 composites with different B doping contents is analyzed (Figure 4). As shown in Figure 4(a), both the g-C3N5 and B/C3N5 composites with different B doping contents exhibit Type IV isothermal curves with distinct H3 hysteresis loops, demonstrating the presence of mesopores in both g-C3N5 and B/C3N5 composites. The specific surface area of the g-C3N5, 1.00% B/C3N5, 1.25% B/C3N5, and 1.50% B/C3N5 composite is 7.42, 16.15, 36.64, and 14.63 m2/g, respectively. With the non-metallic B doping increasing, the specific surface area of the B/C3N5 composites gradually increases and then decreases. The 1.25% B/C3N5 exhibits the highest specific surface area of the 36.64 m2/g. The high specific surface area is conducive to enhancing the photocatalytic activity of the B/C3N5 composite. Compared with 1.25% B/C3N5 composite, the 1.50% B/C3N5 composite exhibits a significant decrease in specific surface area. This is attributed to the collapse of pores caused by the high non-metallic B doping content, resulting in a decrease in specific surface area. The pore size distribution of the g-C3N5 is primarily concentrated in the 0-20 nm range, while the B/C3N5 composite is mainly distributed within the 0-40 nm range (Figure 4(b)). The 1.25% B/C3N5 composite exhibits a broad pore size distribution, indicating the existence of multi-scale pores of mesopores and macropores. The abundant pore structure contributes to enhancing the photocatalytic activity of the C3N5. The 1.25% B/C3N5 composite exhibits high specific surface area, which is used as the representative for further analysis.

(a) N2 adsorption-desorption isotherms and (b) Pore size distribution curves of g-C3N5 and B/C3N5 composites with different B doping content.
Figure 4. (a) N2 adsorption-desorption isotherms and (b) Pore size distribution curves of g-C3N5 and B/C3N5 composites with different B doping content.

3.3. X-Ray photoelectron spectroscopy (XPS) analysis

The elemental composition of the g-C3N5 and 1.25% B/C3N5 composite is characterized by XPS (Figure 5). As shown in Figure 5(a), the g-C3N5 has C and N elements. While the 1.25% B/C3N5 composite has three elements of C, N, and B. The peak at 284.8 eV corresponds to the C-C bond, and the peak near 286.0 eV corresponds to the C=C-H bond in the triazole ring structure (Figure 5(b)). While the peak near 288.2 eV corresponds to the C=N-(N)2 bond, and the peak near 289.2 eV corresponds to the fitted peak of C-NH2 band at the terminal end of the heptazine ring [26-27]. Compared with g-C3N5, the fitting peaks for C=C-H, C=N-(N)2, and C-NH2 group have shifted after B doping, indicating that the electronic structure of the C3N5 changes following B doping. It can be seen from the N 1s spectra in Figure 5(c) that a fitted peak near 398.7 eV corresponds to the C=N-C band and a peak near 400.1 eV corresponds to the N-(C)3 band [28]. While the peak near 400.3 eV corresponds to the fitted peak of the terminal C-NH2 group of the heptazine ring [29]. After B doping, two new peaks appear at 399.5 and 401.0 eV, corresponding to the fitted peaks of B=N-C and B-N-(C)2 group, respectively [30]. This result confirms the successful incorporation of B into the g-C₃N₅ lattice. Compared with the g-C3N5, the shift in the fitted peaks is assigned to C=N-C, N-(C)3 and C-NH2 group upon B doping, indicating that the electronic structure of the g-C3N5 has changed following B doping. It can be seen from the B 1s spectra in Figure 5(d) that the fitted peaks of the B element replacing the N atom in g-C3N5 to form B-C and B-(C)3 band appear at 189.9 and 190.2 eV, respectively. While the peak of the B element replacing the C atom in g-C3N5 to form B-N appears at 191.6 eV [31]. The B/C3N5 composite exhibits only one fitted peak at 191.6 eV, indicating that B atom doping replaces the C atom rather than the N atom to form a new B-N chemical bond.

(a) Full XPS spectra of C3N5 and 1.25% B/C3N5 composite and high-resolution spectra of (b) C 1s, (c) N 1s, and (d) B 1s.
Figure 5. (a) Full XPS spectra of C3N5 and 1.25% B/C3N5 composite and high-resolution spectra of (b) C 1s, (c) N 1s, and (d) B 1s.

3.4. Photoelectrochemical properties analysis

The spectral absorption of the g-C3N5 and B/C3N5 composites with different B doping contents is characterized by UV-vis DRS. As shown in Figure 6(a), the g-C3N5 exhibits excellent absorption response across the visible spectrum. After doping with different B contents, the absorption edges of the g-C3N5 all exhibit red shifts with enhanced visible light absorption response, which is conducive to improving its photocatalytic performance [32]. From the Tauc curve in Figure 6(b), the bandgap energies (Eg) of g-C3N5 and the 1.25% B/C3N5 composite are 2.00 eV and 1.83 eV, respectively. This result indicates that the non-metallic B doping reduces the bandgap energy of the g-C3N5. The slope of the Mott-Schottky curve reflects the type of semiconductor material. The intersection point of the tangents to each curve at different frequencies represents the semiconductor material’s equilibrium flat band potential (EFB) [12]. As shown in Figure 6(c), both g-C3N5 and 1.25% B/C3N5 composite exhibit Mott-Schottky curves with positive slopes. This result indicates that both g-C3N5 and 1.25% B/C3N5 composite are n-type semiconductor materials. The flat band potentials of the C3N5 and 1.25% B/C3N5 composite are determined to be -0.60 and -0.50 V vs. Ag/AgCl, respectively. According to the ESHE=EAg/AgCl + 0.197, the values are -0.403 V and -0.303 V vs. standard hydrogen electrode (SHE) for the g-C3N5 and 1.25% B/C3N5 composite, respectively.

(a) UV-vis DRS spectra of g-C3N5 and B/C3N5 composites with different B doping contents, (b) Tauc’s curves of g-C3N5 and 1.25 % B/C3N5 composite, (c) Mott-Schottky curves of g-C3N5 and 1.25 % B/C3N5 composite, and (d) Band structure of g-C3N5 and 1.25 % B/C3N5 composite.
Figure 6. (a) UV-vis DRS spectra of g-C3N5 and B/C3N5 composites with different B doping contents, (b) Tauc’s curves of g-C3N5 and 1.25 % B/C3N5 composite, (c) Mott-Schottky curves of g-C3N5 and 1.25 % B/C3N5 composite, and (d) Band structure of g-C3N5 and 1.25 % B/C3N5 composite.

Typically, the conduction band potential (ECB) of the n-type semiconductor material is 0.1-0.3 V more negative than the flat band potential vs. SHE [10]. Therefore, the conduction band potentials of the g-C3N5 and 1.25% B/C3N5 composite are -0.603 V and -0.503 V vs. SHE, respectively. The valence band potential (EVB) can be obtained by the equation EVB= Eg+ECB. Therefore, the valence band potentials for g-C3N5 and 1.25% B/C3N5 composite are 1.397 V and 1.327 V vs. SHE, respectively. As clearly shown in Figure 6(d), the conduction band (CB) position of g-C3N5 decreases, and the valence band (VB) position increases after B doping. The reason is that the substitution of the C atom by B atoms to form B-N bonds reduces the bandgap energy of the g-C3N5.

3.5. Photoluminescence (PL), time-resolved photoluminescence (TRPL), electron paramagnetic resonance (EPR) and EIS spectrum analysis

The photogenerated carrier recombination and separation of the g-C3N5 and B/C3N5 composites with different B doping contents are characterized by the PL spectrum. As Figure 7(a) shown, the g-C3N5 and B/C3N5 composites with different B doping contents exhibit emission peaks near 455 nm. Due to high recombination of the photogenerated carriers, the g-C3N5 exhibits the strongest emission peak intensity compared to the B/C3N5 composites with different B doping contents, which significantly limits its photocatalytic activity [16]. The emission peak intensity of g-C3N5 decreases to varying degrees after doping with different B contents. The 1.25% B/C3N5 composite exhibits the lowest emission peak intensity compared to the 1.00% B/C3N5 composite and 1.50% B/C3N5 composite, demonstrating high charge separation and migration efficiency. This result demonstrates that the non-metallic B doping effectively suppresses the recombination of photo-generated carriers [33].

(a) PL spectra of g-C3N5 and B/C3N5 composites with different B doping contents, (b) TRPL spectra of g-C3N5 and B/C3N5 composites with different B doping contents, (c) EPR spectra of g-C3N5 and 1.25 % B/C3N5 composite and (d) EIS spectra of g-C3N5 and B/C3N5 composites with different B doping contents.
Figure 7. (a) PL spectra of g-C3N5 and B/C3N5 composites with different B doping contents, (b) TRPL spectra of g-C3N5 and B/C3N5 composites with different B doping contents, (c) EPR spectra of g-C3N5 and 1.25 % B/C3N5 composite and (d) EIS spectra of g-C3N5 and B/C3N5 composites with different B doping contents.

The photogenerated carrier lifetime of the g-C3N5 and B/C3N5 composites with different B doping contents is characterized by the TRPL spectrum. As Figure 7(b) shown, the fluorescence lifetimes τ1 and τ2 of the g-C3N5 are 0.34 ns and 2.40 ns, respectively, with an average lifetime τave=2.28 ns. The average lifetime τave of B/C3N5 increases with different B doping contents. The 1.25% B/C3N5 composite exhibits the longest average lifetime of the τave=2.97 ns compared to the 1% B/C3N5 composite and 1.5% B/C3N5 composite, indicating that the B doping extends the photogenerated carrier fluorescence lifetime of the C3N5. Therefore, the B doping can effectively prolong the fluorescence lifetime of photogenerated carriers, and enhance the photocatalytic activity of the g-C3N5 [34].

The generation of unpaired electrons of the g-C3N5 and 1.25% B/C3N5 composite is characterized by an EPR spectrum. As Figure 7(c) displays, the Lorenz signal of the g-C3N5 after B doping exhibits significant enhancement. This result indicates that the non-metallic B doping generates a substantial number of unpaired electrons. The recombination of these unpaired electrons with photo-generated holes suppresses the recombination of photoelectrons and photo-generated holes, thereby promoting the photocatalytic activity of the g-C3N5.

The charge transfer resistance of the g-C3N5 and B/C3N5 composites with different B doping contents is characterized by the electrochemical impedance spectroscopy (EIS) spectrum. As shown in Figure 7(d), the constant phase element (CPE) in the equivalent circuit diagram represents a constant phase angle element. The R1 denotes the series resistance affected by electrical contact at the interface, while R2 denotes the impedance associated with the charge transfer process in the photocatalyst [18]. Generally, the size of the Nyquist arc reflects the magnitude of the charge transfer resistance (R2), with a smaller Nyquist arc corresponding to a lower charge transfer resistance [14]. The g-C3N5 has the largest Nyquist arc radius and the highest charge transfer resistance (R2=44 Ω) compared to the B/C3N5 composites, which is unfavorable for charge transfer. The Nyquist arc radius of the g-C3N5 decreases after doping different B contents. The 1.25% B/C3N5 composite exhibits the smallest Nyquist arc radius compared to the g-C3N5 and other B/C3N5 composites, demonstrating excellent charge transfer and separation efficiency [10].

3.6. NF photocatalytic degradation performance analysis

Under simulated visible light (λ>420 nm) irradiation, the NF photocatalytic degradation experiments are conducted (NF concentration=100 mg/L, catalyst dosage=50 mg, pH=5.0). The NF photocatalytic performance of the g-C3N5 and B/C3N5 composites with different B doping contents is investigated. Simultaneously, the apparent rate constant k and correlation coefficient R2 are also obtained by fitting the NF photocatalytic degradation data to the pseudo-first-order kinetic model. The higher correlation coefficient R2 indicates a superior goodness-of-fit to the pseudo-first-order kinetic model [15].

As shown in Figures 8(a-b), the degradation removal of NF by g-C3N5, 1.00% B/C3N5, 1.25% B/C3N5, and 1.50% B/C3N5 composites are 45.66%, 70.98%, 97.36%, and 86.80% after 60 min, respectively. The degradation removal of the 1.25% B/C3N5 composite is 2.13 times that of pure g-C3N5. The NF photocatalytic performance of g-C3N5 is significantly enhanced after non-metallic B doping. This improvement stems from the optimization of the band structure and charge transport pathways achieved through atomic substitution following non-metallic B doping. This process alters the electronic distribution of the g-C3N5, introducing defect states to trap photoelectrons. It effectively suppresses the photoelectron-hole recombination, and enhances the separation efficiency of photogenerated carriers [33]. The degradation removal of the NF decreases significantly when the non-metallic B doping content increases from 1.25% to 1.50%. This is because a high non-metallic B doping content leads to pore collapse and reduces specific surface area of g-C3N5. This hinders transfer of photoelectrons through pore channels, accelerates photoelectron-hole recombination, and consequently inhibits photocatalytic performance [35].

The photocatalytic experiment is carried out under the conditions of the catalyst dosage of 50 mg, NF initial mass concentration of 100 mg/L and initial pH=5.0 to study the influence of the coexistence of inorganic salt ions such as Cl-, NO3-, SO42-, HCO3-, and CO32-on the photocatalytic performance of the NF (Figure S1). It can be seen from Figure S1 that the coexistence of inorganic salt ions such as Cl-, NO3-, and SO42- has little effect on the photocatalytic degradation performance of the NF. However, the degradation removal of NF is the 73.14% and 66.51% after adding the HCO3- and CO32-, respectively. This result indicates that the NF degradation removal significantly decreases. The reason is that the CO32- will be converted into HCO3- under the condition of pH=5. The HCO3-, as a free radical scavenger, consumes ·O2-, which is the main active species in the photocatalytic degradation system, resulting in a decrease in the degradation removal of NF.

Supplementary material

The NF photocatalytic kinetics is fitted and analyzed by the pseudo-first-order kinetic model -ln(Ct/C0)=kt. As shown in Figure 8(c), the correlation coefficients for the pseudo-first-order kinetic fitting of g-C3N5 and B/C3N5 composite with different doping B contents all exceed 0.90. This indicates that the photocatalytic degradation of NF by g-C3N5 and B/C3N5 composite conforms to the pseudo-first-order kinetic model. As shown in Figure 8(d), the apparent rate constant for photocatalytic degradation of NF by the 1.25% B/C3N5 composite is the highest (k=0.0503 min-1), which is 4.98 times higher than that of pure g-C3N5.

(a) The NF photocatalytic degradation curves, (b) NF degradation removal of C3N5 and B/C3N5 composites with different B doping content, (c) NF photocatalytic degradation kinetic fitting curves, (d) apparent rate constant k, (e) active group quenching results and (f) EPR spectra for DMPO-·OH and DMPO-·O2-.
Figure 8. (a) The NF photocatalytic degradation curves, (b) NF degradation removal of C3N5 and B/C3N5 composites with different B doping content, (c) NF photocatalytic degradation kinetic fitting curves, (d) apparent rate constant k, (e) active group quenching results and (f) EPR spectra for DMPO-·OH and DMPO-·O2-.

To analyze the role of active species in NF photocatalytic degradation by 1.25% B/C3N5 composite, the superoxide radicals (O2-), hydroxyl radicals (·OH), and holes (h⁺) in the photocatalytic degradation system are quenched using the p-BQ, IPA, and TEOA, respectively [17]. The NF degradation removal of 1.25% B/C3N5 composite is the 24.14%, 81.98% and 66.78% after adding quenchers such as p-BQ, IPA, and TEOA, respectively (Figure 8(e)). Compared with the NF degradation process without adding quenchers, the NF degradation removal decreases by 73.22%, 15.38% and 30.58%, respectively. The addition of the quencher p-BQ exhibits the most pronounced inhibitory effect, followed by TEOA. While the IPA shows the least inhibitory effect on the NF degradation process. Therefore, the active species contribute to NF photocatalytic degradation in the order •O₂⁻>h⁺>•OH. Therefore, the •O₂⁻ exhibits the dominant contribution. The EVB of the 1.25% B/C3N5 composite is 1.327 V vs. SHE, which is significantly lower than the redox potential of H2O/·OH (1.990 V vs. SHE). The holes in the valence band of the 1.25% B/C3N5 composite cannot oxidize H2O to ·OH. However, the photocatalytic reaction is inhibited upon addition of the quencher IPA, indicating that THE ·OH radicals may exist in the photocatalytic degradation system. To demonstrate the generation of the ·OH and ·O2- in the NF photocatalytic degradation system, the 5,5-dimethyl-1-pyrroline N-oxide (DMPO)-·OH and DMPO-·O2- signals are detected by EPR spectrum under visible light irradiation conditions. Figure 8(f) clearly shows the DMPO-·OH and DMPO-·O2- signals, indicating that reactive free radicals such as ·OH and·O2- are generated in the NF photocatalytic degradation system. In the NF photocatalytic degradation system, the ·OH radicals may originate from the reaction between H+ and ·O2- to form H2O2, which is oxidized by photoelectrons to produce ·OH radicals [24].

3.7. Photocatalytic degradation mechanism analysis

Based on photoelectrical performance characterization, the band structure analysis, and active group quenching analysis, the mechanism for B/C3N5 photocatalytic degradation of NF is proposed (Figure S2). Under visible light excitation (λ>420 nm), the charge separation occurs in the B/C3N5 composite. The photoelectrons transition from the VB to CB, leaving a large number of photogenerated holes in the VB and accumulating a number of photoelectrons in the CB. After non-metallic B doping on g-C3N5, the B atom replaces the C atom on the g-C3N5 structure to form a B-N chemical bond. Due to differences in atomic radius and electron density between the B and C atoms, the defect centers form in the g-C3N5 structure, leading to a substantial population of unpaired electrons. The unpaired electrons and photo-generated holes undergo recombination, which suppresses the recombination of photoelectrons and photo-generated holes, thereby enhancing the separation efficiency of photo-generated carriers [33]. Additionally, the non-metallic B doping creates vacant 2p orbitals, leading to the p-π electron delocalization between the empty 2p orbitals and the π electron clouds of aromatic heterocycles in the g-C3N5 structure. This facilitates electron transfer between g-C3N5 layers and suppresses photoelectron-hole recombination [22]. The unpaired electrons and p-π electron delocalization enhance the separation efficiency of photoelectrons and holes. The reactive species quenching experiment and electron paramagnetic resonance (EPR) characterization analysis indicate that the ·O2- serves as the key reactive species in the NF photocatalytic degradation process [12]. The conduction band potential of the B/C3N5 composite (-0.503 V vs. SHE) is more negative than the standard hydrogen electrode potential of O2/·O2- (-0.33 V vs. SHE). Consequently, the photoelectrons at the CB position can reduce O2 to ·O2-. Since the valence band potential of the B/C3N5 composite (+1.327 V vs. SHE) is more negative than the standard hydrogen electrode potential of H2O/·OH (+1.99 V vs. SHE). Therefore, the holes at the VB position cannot oxidize the H2O to ·OH [5]. However, the reactive species quenching experiment and EPR characterization analysis also indicate the presence of ·OH radicals in the NF photocatalytic degradation system. These ·OH radicals likely originate from the reaction between H+ and ·O2- to form H2O2, which is oxidized by photoelectrons to produce the ·OH. Under the oxidative action of active free radicals, the NF molecules in solution undergo complex demethylation, hydroxylation, ring-opening, and oxidation reactions, ultimately being mineralized and decomposed into the small-molecule inorganic compounds like CO2 and H2O [16].

3.8. NF degradation pathways analysis

The mass-to-charge ratio (m/z) of intermediates formed during photocatalytic degradation of NF is determined by HPLC-MS, confirming the molecular formula of the intermediates and NF degradation pathways (Figure S2). The NF exhibits an m/z of 365.91, and the potential photocatalytic pathways for NF are proposed (Figure 9). The NF photocatalytic degradation process involves the reactions such as demethylation, hydroxylation, ring-opening, and oxidation, ultimately degrading these compounds into inorganic substances like CO2 and H2O. The degradation pathways of the NF primarily involve two pathways (Figure 9). Degradation pathway Ⅰ: NF ionization product A1 (m/z=330.09) undergoes demethylation to form intermediate A2 (m/z=316.08). The intermediate A2 undergoes further demethylation to form intermediate A3 (m/z=302.07). While, the intermediate A3 further undergoes ring-opening reactions upon attack by free radicals such as ·O2-, yielding intermediates A4 (m/z=204.06) and A8 (m/z=282.19). Subsequently, the intermediate A4 undergoes oxidation to form intermediate A5 (m/z=125.95). Finally, the intermediates of the A5 and A8 are decomposed into CO2 and H2O, and other inorganic ions. Degradation pathway II: the NF ionization product undergoes hydroxylation to form intermediate A6 (m/z=347.21). The intermediate A6 further undergoes oxidation to generate the intermediate A7 (m/z=223.05), which is ultimately decomposed into CO2 and H2O, and other inorganic ions.

The proposed NF degradation pathways analysis.
Figure 9. The proposed NF degradation pathways analysis.

3.9. Cycle stability analysis

The photocatalyst should not only exhibit excellent photocatalytic activity but also possess outstanding recyclability and stability. After photocatalytic experiments, the recycled 1.25% B/C3N5 composite for subsequent experiments is used to evaluate its recyclability. The phase structure and chemical composition of the 1.25% B/C3N5 composite are characterized by XRD and FT-IR before and after cycling. As shown in Figure S3(a), the degradation removal of NF for 1.25% B/C3N5 composite reaches 97.15% after five cycles. Compared with the fresh 1.25% B/C3N5 composite, the NF degradation removal decreases by only 0.21%, exhibiting excellent photocatalytic performance and demonstrating good cyclic stability. As shown in Figures S3(b-c), the XRD diffraction peaks and FT-IR vibration peaks of the 1.25% B/C3N5 composite exhibit no significant changes after five cycles. These results indicate that the cyclic reuse does not alter the phase crystallinity or chemical composition of the 1.25% B/C3N5 composite. Therefore, the 1.25% B/C3N5 composite not only exhibits outstanding cycling performance but also possesses excellent chemical stability.

4. Conclusions

The nonmetallic B/C3N5 is synthesized by high-temperature thermal polymerization for NF photocatalytic degradation. The doping of non-metal B effectively optimizes the band structure of the g-C3N5, and enhances photocatalytic degradation of NF. The photocatalytic degradation removal of NF on B/C3N5 reaches 97.36%. The recombination of generated unpaired electrons with holes enhances the separation efficiency of photogenerated carriers, contributing to NF photocatalytic degradation. Besides, the non-metallic B doping creates vacant 2p orbitals, which form p-π electron delocalization with the delocalized π bonds of the g-C3N5 aromatic heterocycle, facilitating NF photocatalytic degradation. The NF photocatalytic degradation pathway and mechanism are analyzed and put forward. The future work will expand to include degradation experiments of various typical organic pollutants, in order to systematically evaluate the broad-spectrum photocatalytic degradation performance of B/C3N5 composite.

Acknowledgment

The authors would like to express their gratitude to the Henan Province Science and Technology Research Project (252102241016 and 252102320019) for financial support.

CRediT authorship contribution statement

Suping Wang: Conceptualization, methodology, formal analysis,investigation, writing - original draft. Yujuan Liu: Formal analysis, investigation. methodology, supervision.

Declaration of competing interest

There are no conflicts of interest.

Data availability

Data will be made available on request.

Declaration of generative AI and AI-assisted technologies in the writing process

The authors confirm that there was no use of artificial intelligence (AI)-assisted technology for assisting in the writing or editing of the manuscript, and no images were manipulated using AI.

Supplementary data

Supplementary material to this article can be found online at https://dx.doi.org/10.25259/AJC_321_2026.

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