Na和O元素共掺杂氮化碳高效光催化制氢

doi:10.15541/jim20240345

无机材料学报 ›› 2025, Vol. 40 ›› Issue (5): 552-562.DOI: 10.15541/jim20240345 CSTR: 32189.14.10.15541/jim20240345

• 研究快报 • 上一篇

Na和O元素共掺杂氮化碳高效光催化制氢

陈莉波¹(), 盛盈¹, 伍明¹(), 宋季岭², 蹇建¹, 宋二红³()

1.湖南科技大学化学化工学院, 湘潭 411201
2.国家复合改性聚合物工程技术研究中心, 贵阳 550014
3.中国科学院上海硅酸盐研究所, 上海 200050

收稿日期:2024-07-20 修回日期:2024-10-15 出版日期:2025-05-20 网络出版日期:2024-10-28
通讯作者: 伍明, 副教授. E-mail: wuming10@mails.jlu.edu.cn;
宋二红, 副研究员. E-mail: ehsong@mail.sic.ac.cn
作者简介:陈莉波(2000-), 男, 硕士研究生. E-mail: 1871066627@qq.com

Na and O Co-doped Carbon Nitride for Efficient Photocatalytic Hydrogen Evolution

CHEN Libo¹(), SHENG Ying¹, WU Ming¹(), SONG Jiling², JIAN Jian¹, SONG Erhong³()

1. School of Chemistry and Chemical Engineering, Hunan University of Science and Technology, Xiangtan 411201, China
2. National Engineering Research Center for Compounding and Modification of Polymer Materials, Guiyang 550014, China
3. Shanghai Institute of Ceramics, Chinese Academy of Sciences, Shanghai 200050, China

Received:2024-07-20 Revised:2024-10-15 Published:2025-05-20 Online:2024-10-28
Contact: WU Ming, associate professor. E-mail: wuming10@mails.jlu.edu.cn;
SONG Erhong, associate professor. E-mail: ehsong@mail.sic.ac.cn
About author:CHEN Libo (2000-), male, Master candidate. E-mail: 1871066627@qq.com
Supported by:
National Natural Science Foundation of China(21806023);Natural Science Foundation of Hunan Province(2021JJ40199);Education Department Foundation of Hunan Province(20C0813);Hunan University of Science and Technology Fundamental Research Funds;Postgraduate Scientific Research Innovation Project of Hunan Province(CX20240877)

摘要/Abstract

摘要：

元素掺杂可以调控氮化碳(CN)能带结构以获取更好的光催化性能。本研究通过柠檬酸钠和纯CN粉末的固相反应, 在180 ℃空气气氛下制备了Na和O共掺杂CN(Na/O-CN_x, x=1.0、2.0、3.0、4.0)。Na/O-CN_3.0的比表面积达到18.8 m²/g, 比纯CN(11.7 m²/g)提升了60.7%。Na/O-CN_3.0样品的能带宽度为2.68 eV, 略低于纯CN(2.70 eV), 前者有助于可见光吸收。Na和O元素共掺杂有效抑制了材料的光生电子-空穴对复合, 提升了太阳光的利用率。因此, Na/O-CN_x样品在可见光条件下的光催化制氢效率得到了显著提升, 最优催化剂Na/O-CN_3.0的光催化制氢效率为103.2 μmol∙g^-1∙h^-1, 相比于纯CN(11.2 μmol∙g^-1∙h^-1)提升了8.2倍, 同时表现出良好的催化稳定性。此外, 通过调节反应气体中氧含量制备了一系列Na/O-CN_3.0-yO₂(y=0、20%、40%、60%、80%、100%)样品, 催化性能结果揭示了在Na/O-CN_x样品中掺杂Na和O原子均有助于提升光催化性能。本工作为较低温度下制备金属原子掺杂CN材料提供了新思路, 揭示了Na和O原子在Na/O-CN_x光催化制氢过程中的协同效应。

关键词: Na和O共掺杂氮化碳, 协同效应, 可见光, 光催化制氢

Abstract:

Elemental doping is an effective strategy for tuning the band structure of graphite carbon nitride (CN) to enhance its photocatalytic performance. In this study, sodium (Na) and oxygen (O) co-doped carbon nitride (Na/O-CN_x, x=1.0, 2.0, 3.0, 4.0) was synthesized via solid-phase reaction of sodium citrate (NaCA) and pure CN powder in the Teflon-sealed autoclave under air conditions at 180 ℃. Surface area of Na/O-CN_3.0 is measured to be 18.8 m²/g, increasing by 60.7% compared to that of pure CN (11.7 m²/g). Bandgap energy of Na/O-CN_3.0 is determined to be 2.68 eV, marginally lower than that of pure CN (2.70 eV), thereby enhancing its capacity for sunlight absorption. Meanwhile, the incorporation of Na and O atoms into Na/O-CN_x is found to effectively reduce recombination rates of photogenerated electron-hole pairs. As a result, Na/O-CN_x samples exhibit markedly enhanced photocatalytic hydrogen evolution activity under visible light irradiation. Notably, the optimal Na/O-CN_3.0 sample achieves a photocatalytic hydrogen production rate of 103.2 μmol∙g^-1∙h^-1, which is 8.2 times greater than that of pure CN (11.2 μmol∙g^-1∙h^-1). Furthermore, a series of Na/O-CN_x-yO₂ (y=0, 20%, 40%, 60%, 80%, 100%) samples were prepared by modulating the oxygen content within reaction atmosphere. The catalytic performance evaluations reveal that the incorporation of both Na and O atoms in Na/O-CN_3.0 enhances photocatalytic activity. This study also introduces novel methodologies for synthesis of metal atom-doped CN materials at lower temperature, highlighting the synergistic effect of Na and O atoms in photocatalytic hydrogen production of Na/O-CN_x samples.

Key words: Na and O co-doped carbon nitride, synergistic effect, visible light, photocatalytic hydrogen evolution

中图分类号:

TQ174

陈莉波, 盛盈, 伍明, 宋季岭, 蹇建, 宋二红. Na和O元素共掺杂氮化碳高效光催化制氢[J]. 无机材料学报, 2025, 40(5): 552-562.

CHEN Libo, SHENG Ying, WU Ming, SONG Jiling, JIAN Jian, SONG Erhong. Na and O Co-doped Carbon Nitride for Efficient Photocatalytic Hydrogen Evolution[J]. Journal of Inorganic Materials, 2025, 40(5): 552-562.

图/表 12

Fig. 1 Synthetic schematic of Na/O-CNx and Na/O-CN3.0-yO2 samples

Fig. 2 Structure analyses of samples (a, b) XRD patterns of (a) pure CN and Na/O-CNx, and (b) Na/O-CN3.0-yO2; (c) FT-IR spectra of pure CN, Na/O-CN3.0 and Na/O-CN3.0-40%O2

Fig. 3 Morphologies of samples (a, b) SEM images of (a) pure CN and (b) Na/O-CN3.0; (c) TEM and (d) HRTEM images of Na/O-CN3.0

Fig. 4 High-resolution XPS spectra of pure CN, Na/O-CN3.0 and Na/O-CN3.0-40%O2 samples (a) C1s; (b) N1s; (c) O1s; (d) Na1s

Fig. 5 Band structure analysis of pure CN and Na/O-CN3.0 (a) UV-Vis DRS spectra; (b) Related Tauc plots; (c) VB XPS spectra; (d) Band structure diagram

Fig. 6 Photocurrent and PL spectra analysis of pure CN and Na/O-CN3.0 samples (a) Photocurrent test; (b) EIS plots; (c) PL spectra; (d) Time-resolved PL spectra

Fig. 7 Photocatalytic hydrogen activity (a, b) Photocatalytic hydrogen evolution of (a) pure CN and Na/O-CNx, and (b) Na/O-CN3.0-yO2; (c) PHER of pure CN, Na/O-CN3.0 and Na/O-CN3.0-40%O2; (d) Cycling performance of Na/O-CN3.0

Fig. 8 Photocatalytic hydrogen evolution mechanism of Na/O-CN3.0 under visible light irradiation

Fig. S1 Nitrogen adsorption-desorption isotherms and corresponding pore diameter distribution curves of pure CN and Na/O-CN3.0

Fig. S2 XPS survey spectra of pure CN, Na/O-CN3.0 and Na/O-CN3.0-40%O2

Fig. S3 ESR spectra of pure CN, Na/O-CN3.0 and Na/O-CN3.0-40%O2 samples

Table S1 Photocatalytic hydrogen evolution performance under visible light irradiation (> 420 nm) and surface area of alkali metal doped carbon nitride[S1-S12]

Catalyst	Synthesis temperature/℃	Catalyst weight/mg	Sacrificial reagent/% (in volume)	Surface area/ (m²·g^-1)	Activity compared with CN (times)	Ref.
Na/O-CN_3.0	180	50	TEOA 10%	18.8	9.2	This work
3% NaCl-CN	550	10	TEOA 17%	76.8	4.3	[S1]
KCN-10	550	50	TEOA 10%	11	5.6	[S2]
K(0.05)-CN	550	50	TEOA 17%	11.1	5	[S3]
LiNa-K-CN2	520	50	TEOA 10%	116.2	15	[S4]
Na(30)-MCN	550	100	TEOA 10%	56.1	12.9	[S5]
Na0.1-CNNTs	650	20	TEOA 10%	94	11	[S6]
CN-Na-7	550	50	TEOA 10%	11.7	9.9	[S7]
CN-100	520	50	TEOA 10%	14.9	9.2	[S8]
(Na,O)g-C₃N₄	160	50	ethyl alcohol 40%	-	7	[S9]
CN_0.05	550	20	TEOA	46.7	1.9	[S10]
GCN-Na-5	550	50	TEOA	10.3	1.5	[S11]
K@C₃N₄	600	100	TEOA	27.5	8	[S12]

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Na和O元素共掺杂氮化碳高效光催化制氢

Na and O Co-doped Carbon Nitride for Efficient Photocatalytic Hydrogen Evolution

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