高选择性H2O2光合成: Ba原子注入面内高度有序结晶结构的g-C3N4纳米棒

doi:10.1016/S1872-2067(24)60008-2

催化学报 ›› 2024, Vol. 60: 231-241.DOI: 10.1016/S1872-2067(24)60008-2

高选择性H₂O₂光合成: Ba原子注入面内高度有序结晶结构的g-C₃N₄纳米棒

孟爱云, 马辛源, 温达, 钟威^*(), 周双^*(), 苏耀荣^*()

深圳技术大学新材料与新能源学院, 广东深圳 518118

收稿日期:2024-01-25 接受日期:2024-02-24 出版日期:2024-05-18 发布日期:2024-05-20
通讯作者: *电子信箱: zhongwei@sztu.edu.cn (钟威), zhoushuang@sztu.edu.cn (周双), suyaorong@sztu.edu.cn (苏耀荣).
作者简介:第一联系人：¹共同第一作者.
基金资助:
国家自然科学基金(22178224);国家自然科学基金(22272110);国家自然科学基金(22002091);深圳技术大学基本科研业务费(20211063010047);广东省基础与应用基础研究基金(2020A1515110873);广东省基础与应用基础研究基金(2023A1515110535);深圳市科技计划(20231127203830001)

Towards highly-selective H₂O₂ photosynthesis: In-plane highly ordered carbon nitride nanorods with Ba atoms implantation

Aiyun Meng, Xinyuan Ma, Da Wen, Wei Zhong^*(), Shuang Zhou^*(), Yaorong Su^*()

College of New Materials and New Energies, Shenzhen Technology University, Shenzhen 518118, Guangdong, China

Received:2024-01-25 Accepted:2024-02-24 Online:2024-05-18 Published:2024-05-20
Contact: *E-mail: zhongwei@sztu.edu.cn (W. Zhong), zhoushuang@sztu.edu.cn (S. Zhou), suyaorong@sztu.edu.cn (Y. Su).
About author:First author contact:¹Contributed equally to this work.
Supported by:
National Natural Science Foundation of China(22178224);National Natural Science Foundation of China(22272110);National Natural Science Foundation of China(22002091);Fundamental Research Funds for Shenzhen Technology University(20211063010047);Guangdong Basic and Applied Basic Research Foundation(2020A1515110873);Guangdong Basic and Applied Basic Research Foundation(2023A1515110535);Shenzhen Science and Technology Program(20231127203830001)

摘要/Abstract

摘要：

过氧化氢(H₂O₂)是一种重要的绿色氧化剂, 在医疗、军工、食品和绿色化学合成等领域有着广泛应用. 然而, 传统蒽醌法合成H₂O₂存在能耗高、污染严重等问题. 光催化合成H₂O₂技术, 利用来源丰富的太阳能实现氧气的两电子还原, 被认为是替代蒽醌工艺的理想方案. 石墨相氮化碳(g-C₃N₄)因具有成本低、化学性质稳定和电子结构易调等优点, 在光催化合成H₂O₂方面展现出很大潜力. 但传统g-C₃N₄的面内结晶度低, 且对两电子氧还原反应的选择性差, 这极大地限制了其光合成H₂O₂效率. 为解决这一难题, 本文合理设计了一种新策略: 将钡(Ba)原子注入面内高度有序结晶结构的g-C₃N₄纳米棒(BI-CN), 在增强g-C₃N₄的面内结晶度的同时, 进一步提高其对两电子氧还原反应的选择性.

本文采用BaCl₂诱导的面内聚合策略, 实现了Ba原子注入的面内高度有序结晶结构g-C₃N₄纳米棒的可控合成. 在合成过程中, 三聚氰胺分子选择性地吸附在BaCl₂的(200)晶面, 并与暴露在BaCl₂表面的Ba原子形成Ba‒N键. 这种强相互作用诱导了三嗪结构单元的定向富集和聚合, 从而形成面内有序结晶结构的g-C₃N₄结构. 同时, Ba原子通过Ba‒N键稳定地锚定在g-C₃N₄结构中, 构建了Ba原子注入的面内高度有序结晶结构的g-C₃N₄纳米棒. 实验和理论计算结果表明, 由于Ba原子和N原子的电负性差异, 电子从Ba原子迁移到N原子, 形成缺电子的Ba活性位点. 注入的Ba原子起到正电荷中心的作用, 氧气分子以Pauling构型稳定地吸附在Ba原子上, 该吸附构型使得O‒O键不易断裂并增强了*OOH中间体的稳定性, 从而抑制了四电子氧还原生成水的反应, 有效地提高了两电子氧还原的选择性, 最终实现高效的光催化H₂O₂合成. 其中, 最优的BI-CN3(三聚氰胺和BaCl₂质量比为9:2)光催化生成H₂O₂的速率达到353 μmol L^‒1 h^‒1, 是原始g-C₃N₄的6.1倍, 且表现出良好的光催化循环使用性能. 同时, BI-CN3光催化剂表现出更强的表面光电压信号、光电流信号以及更低的荧光强度, 表明其具有更强的光生电荷分离和迁移效率.

综上, 本文不仅为构建具有面内高结晶度和原子级活性位点的g-C₃N₄光催化剂提供了一种新策略, 还为提高两电子氧还原反应的选择性提供了新思路, 可为光催化H₂O₂的高效、绿色合成提供了参考.

关键词: H₂O₂光合成, 石墨相氮化碳, Ba原子注入, 高选择性两电子氧还原, 面内高结晶度

Abstract:

Graphitic carbon nitride (g-C₃N₄) shows great potential in photocatalytic H₂O₂ production. However, challenges arise from its low in-plane crystallinity and selectivity in two-electron oxygen reduction reaction (2e^--ORR), greatly limiting its H₂O₂ photosynthesis efficiency. Herein, we develop an ingenious strategy to simultaneously increase the in-plane crystallinity and induce the highly-selective 2e^--ORR by rationally designing barium (Ba) atom-implanted in-plane highly ordered g-C₃N₄ nanorods. The approach involves controllable synthesis of in-plane high crystallinity g-C₃N₄ nanorods with Ba implantation (BI-CN) using a BaCl₂-mediated in-plane polymerization strategy. The unique Ba-N interaction induces the oriented polymerization of 3-s-triazine units to form well-arranged in-plane structures. Experimental and theoretical calculations clarify that the implanted Ba atoms function as positive charge centers, resulting in a Pauling-type O₂ adsorption configuration. This minimizes O-O bond breaking energy, thus suppressing the four-electron oxygen reduction reaction (4e^--ORR) and facilitating a highly-selective 2e^--ORR pathway for efficient photocatalytic H₂O₂ production. Consequently, the optimized BI-CN3 photocatalyst exhibits an outstanding H₂O₂ production rate of as high as 353 μmol L^-1 h^-1, surpassing the pristine g-C₃N₄ by 6.1 times. This study concurrently optimizes the in-plane crystallinity and O₂ adsorption sites of g-C₃N₄ photocatalysts for highly-selective H₂O₂ production, providing innovative insights for designing efficient photocatalysts with diverse applications.

Key words: Hydrogen peroxide photosynthesis, Carbon nitride, Ba implantation, Highly-selective 2e^?-ORR, In-plane crystallinity

孟爱云, 马辛源, 温达, 钟威, 周双, 苏耀荣. 高选择性H₂O₂光合成: Ba原子注入面内高度有序结晶结构的g-C₃N₄纳米棒[J]. 催化学报, 2024, 60: 231-241.

Aiyun Meng, Xinyuan Ma, Da Wen, Wei Zhong, Shuang Zhou, Yaorong Su. Towards highly-selective H₂O₂ photosynthesis: In-plane highly ordered carbon nitride nanorods with Ba atoms implantation[J]. Chinese Journal of Catalysis, 2024, 60: 231-241.

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链接本文: https://www.cjcatal.com/CN/10.1016/S1872-2067(24)60008-2

https://www.cjcatal.com/CN/Y2024/V60/I5/231

图/表 7

Fig. 1. Graphical illustration about the conventional g-C3N4 with slow electron transfer and low-selectivity H2O2 photosynthesis (1), Ba implanted in-plane highly ordered g-C3N4 photocatalyst with simultaneously accelerating electron transfer and promoting H2O2 evolution selectivity (2).

Fig. 2. (a) The ordered growth mechanism of the BI-CN by BaCl2-mediated in-plane polymerization process. (b) The calculated adsorption energy of the melamine molecules on different BaCl2 crystal planes. (c) FTIR patterns of the BI-CN at different temperatures.

Fig. 3. SEM (a), TEM (b), high-resolution TEM (c) and TEM-EDS mapping images (d) of the typical BI-CN3 sample. XRD patterns (e), FT-IR patterns (f), Solid-state 13C NMR MAS spectra (g), high-resolution XPS curves (h), UV-vis DRS spectra (i) and Nitrogen adsorption-desorption isotherms (j) for the synthesized photocatalysts.

Fig. 4. (a) Photocatalytic H2O2-production rates for various samples. (b) Cycling H2O2-generation tests of BI-CN3 photocatalyst. (c) The photocatalytic H2O2-activities for bulk CN and BI-CN3 samples in 0.1 mol L?1 Na2SO4 solution. (d) H2O2 evolution activities of BI-CN3 samples under different conditions.

Fig. 5. High-resolution XPS spectra of N 2p (a) and Ba 3d (b). (c) The optimized structure models of conventional g-C3N4 (CN) and the Ba implanted in-plane highly ordered g-C3N4 (BI-CN). The calculated density of state (DOS) for bulk CN (d) and BI-CN (e). Bader charge analysis (f) and the electrostatic potential surface distribution for the optimized bulk CN (g) and BI-CN (h) models.

Fig. 6. (a) EPR spectra of DMPO?O2?. (b) Koutecky-Levich plots for CN and BI-CN. The calculated O2 adsorption models on CN (c) and BI-CN (d) structures and their corresponding local charge density differences. (e) Calculated free energy diagrams for 2e?-ORR (H2O2 production) and 4e?-ORR (H2O evolution).

Fig. 7. Mechanism of the highly-selective 2e- ORR process for efficient photocatalytic H2O2 production on the Ba implanted in-plane highly ordered g-C3N4 nanorods.

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高选择性H₂O₂光合成: Ba原子注入面内高度有序结晶结构的g-C₃N₄纳米棒

Towards highly-selective H₂O₂ photosynthesis: In-plane highly ordered carbon nitride nanorods with Ba atoms implantation

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