电化学驱动结构工程构筑富氧氮化碳纳米片及其光催化性能调控研究

doi:10.1016/j.actphy.2026.100365

电化学驱动结构工程构筑富氧氮化碳纳米片及其光催化性能调控研究

Lole Jurado^1,2, Carmen Portillo-Hurtado¹, María Carmen Hidalgo¹, María Isabel Domínguez¹, Marcela Martínez-Tejada¹, Miguel Ángel Centeno¹, José Antonio Navío¹, Sergio García-Dalí¹

1 Departamento de Química Inorgánica e Instituto de Ciencia de Materiales de Sevilla, Centro Mixto CSIC-Universidad de Sevilla, Sevilla 41092, Andalusia, Spain;
2 Departamento de Química Inorgánica, Cristalografía y Mineralogía, Facultad de Ciencias, Universidad de Málaga, Málaga 29071, Andalusia, Spain

收稿日期:2026-04-28 修回日期:2026-07-08 录用日期:2026-07-08
通讯作者: Lole Jurado, Sergio García-Dalí E-mail:lolejurado@uma.es;sergio.dali@icmse.csic.es
基金资助:
LJ appreciates the financial support of Marie Curie Postdoctoral Fellowship (GA No. 101106349). SGD thanks the Spanish Ministry of Science, Innovation and Universities, Fondo Social Europeo Plus (FES+) and the State Research Agency for his Juan de la Cierva contract JDC2023-051536-I. All authors acknowledge funding from MCIN/AEI/10.13039/501100011033/FEDER (Ministry of Science and Innovation and State Research Agency, Spain), grant numbers PID2021-122413NB-I00 and PID2023- 147861OB-C22.

Electrochemical-driven structural engineering of highly oxidized carbon nitride nanosheets for tuneable photocatalytic performance

Lole Jurado^1,2, Carmen Portillo-Hurtado¹, María Carmen Hidalgo¹, María Isabel Domínguez¹, Marcela Martínez-Tejada¹, Miguel Ángel Centeno¹, José Antonio Navío¹, Sergio García-Dalí¹

1 Departamento de Química Inorgánica e Instituto de Ciencia de Materiales de Sevilla, Centro Mixto CSIC-Universidad de Sevilla, Avda. Américo Vespucio, 49, Sevilla, 41092, Spain;
2 Departamento de Química Inorgánica, Cristalografía y Mineralogía, Facultad de Ciencias, Universidad de Málaga, Campus de Teatinos, 29071 Málaga, Spain

Received:2026-04-28 Revised:2026-07-08 Accepted:2026-07-08
Contact: Lole Jurado, Sergio García-Dalí E-mail:lolejurado@uma.es;sergio.dali@icmse.csic.es

1. 2026.100365-D-26-00277-11p-2# SI.pdf(1330KB)

摘要/Abstract

摘要： 氮化碳是一类在光催化应用领域极具潜力的无金属半导体材料；但传统热合成方法通常难以实现对其结构有序度和表面化学性质的精准调控。本研究中，利用恒电流电化学合成策略可制备羟基功能化的类氮化碳量子点(OH-C₃N₄-QDs)，并以其作为可调控的前驱体，经酸处理进一步得到富O氮化碳纳米片(CNO)。通过系统调控电合成过程中的电流强度，制备得到缩合程度、氧化程度及表面N富集程度不同的氮化碳材料。采用X射线衍射(XRD)、傅里叶变换红外光谱(FTIR)、拉曼(Raman)光谱、扫描电子显微镜(SEM)、透射电子显微镜(TEM)、紫外-可见吸收光谱(UV-Vis)和X射线光电子能谱(XPS)等手段，系统研究了CNO纳米片的结构与组分变化，揭示了有序的CN中间体的形成以及氧官能团的可控引入。结果表明：电化学参数可以有效调控材料的层间堆垛相干性、层间相互作用及表面化学状态。在模拟太阳光照射下，以罗丹明B (RhB)降解为模型反应，进行光催化性能测试，结果证实：与OH-C₃N₄-QDs前驱体相比，酸处理后形成的富氧氮化碳纳米片显示出更高的光催化活性，其活性增强可归因于表面N富集和适度氧化，而并非比表面积或带隙的改变。本研究结果表明，电化学合成为调控氮化碳材料的结构和表面化学性质提供一条有效途径，同时有助于明确光催化过程中的构效关系。

关键词: 氧化氮化碳, 电合成, 量子点, 表面功能化, 光催化, 罗丹明B

Abstract: Carbon nitride is a promising metal-free semiconductor for photocatalytic applications; however, conventional thermal routes often provide limited control over its structural order and surface chemistry. In this work, a galvanostatic electrochemical strategy is presented for the synthesis of hydroxyl-functionalized carbon nitride quantum dot-like species (OH-C₃N₄-QDs), which act as tuneable precursors for oxygen-rich carbon nitride nanosheets (CNO) obtained after acid treatment. By systematically varying the applied current density, materials with different degrees of condensation, oxidation and surface nitrogen enrichment were produced. Structural and compositional evolution of the resulting CNO nanosheets was investigated by X-ray diffraction (XRD), Fourier Transform Infrared spectroscopy (FTIR), Raman spectroscopy, Scanning Electron Microscopy (SEM), Transmission Electron microscopy (TEM), UV-Vis spectroscopy and X-ray photoelectron spectroscopy (XPS), revealing the formation of ordered CN intermediate phases and controlled incorporation of oxygen functionalities. The electrochemical parameters were shown to govern stacking coherence, interlayer interactions and surface chemical environments. The photocatalytic behaviour was evaluated using Rhodamine B degradation under simulated solar irradiation. Compared with the OH-C₃N₄-QDs precursor, the oxidized nanosheets exhibit enhanced photocatalytic activity, which correlates with surface nitrogen enrichment and moderate oxidation rather than with surface area or band gap values. These results demonstrate that electrochemical synthesis provides an effective route for tailoring the structure and surface chemistry of carbon nitride materials, establishing clear structure– activity relationships relevant to photocatalytic processes.

Key words: Carbon nitride oxides, Electrosynthesis, Quantum dots, Surface functionalization, Photocatalysis, Rhodamine B

Lole Jurado, Carmen Portillo-Hurtado, María Carmen Hidalgo, María Isabel Domínguez, Marcela Martínez-Tejada, Miguel Ángel Centeno, José Antonio Navío, Sergio García-Dalí. 电化学驱动结构工程构筑富氧氮化碳纳米片及其光催化性能调控研究[J]. 物理化学学报 2026, (), 100365. doi: 10.1016/j.actphy.2026.100365

Lole Jurado, Carmen Portillo-Hurtado, María Carmen Hidalgo, María Isabel Domínguez, Marcela Martínez-Tejada, Miguel Ángel Centeno, José Antonio Navío, Sergio García-Dalí. Electrochemical-driven structural engineering of highly oxidized carbon nitride nanosheets for tuneable photocatalytic performance[J]. Acta Phys. -Chim. Sin. 2026, (), 100365. doi: 10.1016/j.actphy.2026.100365

链接本文: https://www.whxb.pku.edu.cn/CN/10.1016/j.actphy.2026.100365

https://www.whxb.pku.edu.cn/CN/Y2026/V/I/100365

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