Fe-MOF/g-C3N4嵌入式3D/2D S型异质结的构建及其光还原CO2性能

doi:10.1016/S1872-2067(22)64115-9

催化学报 ›› 2022, Vol. 43 ›› Issue (10): 2625-2636.DOI: 10.1016/S1872-2067(22)64115-9

Fe-MOF/g-C₃N₄嵌入式3D/2D S型异质结的构建及其光还原CO₂性能

赵小雪^a, 许梦阳^b, 宋相海^a, 周伟强^a, 刘鑫^a, 霍鹏伟^a^,^*()

^a江苏大学化学化工学院, 绿色化学与化工技术研究院, 江苏镇江 212013
^b郑州大学化学学院绿色催化中心, 河南郑州 450001

收稿日期:2022-03-29 接受日期:2022-04-28 出版日期:2022-10-18 发布日期:2022-09-30
通讯作者: 霍鹏伟
基金资助:
国家自然科学基金(22078131);国家自然科学基金(22108102);镇江市科技规划社会发展项目(SH2021013)

3D Fe-MOF embedded into 2D thin layer carbon nitride to construct 3D/2D S-scheme heterojunction for enhanced photoreduction of CO₂

Xiaoxue Zhao^a, Mengyang Xu^b, Xianghai Song^a, Weiqiang Zhou^a, Xin Liu^a, Pengwei Huo^a^,^*()

^aInstitute of Green Chemistry and Chemical Technology, School of Chemistry & Chemical Engineering, Jiangsu University, Zhenjiang 212013, Jiangsu, China
^bGreen Catalysis Center, College of Chemistry, Zhengzhou University, Zhengzhou 450001, Henan, China

Received:2022-03-29 Accepted:2022-04-28 Online:2022-10-18 Published:2022-09-30
Contact: Pengwei Huo
Supported by:
National Natural Science Foundation of China(22078131);National Natural Science Foundation of China(22108102);Science and Technology Planning Social Development Project of Zhenjiang City(SH2021013)

摘要/Abstract

摘要：

利用太阳能驱动温室气体CO₂转化为高价值燃料是解决环境和能源难题的策略之一. 二维薄层石墨氮化碳(g-C₃N₄)材料因具有丰富的表面活性位点、较大的比表面积、合适的导带位置、良好的稳定性、易于制备和改性等优点而备受关注, 并被认为是光催化还原CO₂的理想材料. 然而, 二维g-C₃N₄有限的光捕获能力和光生载流子的高电荷复合率限制了其光催化活性. S型异质结具有可控的内建电场强度和稳定的界面载流子传输热/动力学过程, 能够在保持最高氧化还原能力的同时, 最大限度地提高光生电子-空穴对的空间分离效率. S型异质结是通过耦合具有较小功函数的还原半导体(RP)和具有较大功函数的氧化半导体(OP)构建而成. 二维薄层g-C₃N₄完全满足RP材料S型异质结的要求. 由活性金属Fe组成的Fe-MOF具有丰富的配位不饱和位点, Fe-MOF中的铁-氧簇在可见光区具有较宽的吸收范围, 而且由于功函数明显不同, Fe-MOF是与2D g-C₃N₄形成S型异质结的理想OP材料.

本文通过原位合成策略制备了CN/Fe-MOF光催化体系, 并用于光催化还原CO₂. X射线衍射和X射线光电子能谱结果表明, CN和Fe-MOF通过化学相互作用形成异质结构. 研究了不同催化剂在300 W氙弧灯下100 mL水中CO₂还原的光催化活性. 照射6 h后, CN和Fe-MOF将CO₂转化为CO的活性较差, 分别为1.92和0.50 μmol g^‒1. 而CN/Fe-MOF中CN的负载量对光催化活性有至关重要的影响, 当CN的负载量为50 mg (50CN/Fe-MOF)时, 样品催化生成CO产率(19.17 μmol g^‒1)最高, 并且在循环30 h内保持稳定. 稳态荧光、时间分辨荧光、瞬态光电流响应和电化学阻抗谱结果表明, 该异质结的形成降低了光生电子-空穴对的复合率, 降低了界面电荷转移电阻, 为电荷转移提供了更好的路径. 原位傅里叶变换红外(FT-IR)结果不仅证明了CN是活性位点, 而且表明50CN/Fe-MOF比CN具有更强的生成HCOO^‒的能力. 莫特-肖特基测试、紫外光电子能谱测试和电子自旋共振分析结果证实了S型异质结的成功构建. Fe-MOF具有较大的功函数和较小的费米能级, 而CN正好相反, 当CN和Fe-MOF发生界面接触时, 由于费米能级不同, CN的电子自发转移到Fe-MOF, 直到界面处的费米能级达到平衡. 同时, CN侧的界面电子耗尽, Fe-MOF侧的界面电子富集, 使CN的带边向上弯曲带正电, 而Fe-MOF的带边向下弯曲带负电, 因此, 在50CN/Fe-MOF的界面处形成了内建电场. 在光照条件下, 50CN/Fe-MO样品中的CN和Fe-MOF的电子分别被激发, 由于库仑相互作用和内建电场影响, 其电子转移遵循S路线, 即位于Fe-MOFs的导带(CB)上的光生电子将与CN的价带(VB)中的光生空穴复合, 然后CN的CB中积累的光生电子与表面吸附的CO₂反应生成CO, H₂O与Fe-MOF的空穴反应生成O₂. 综上, 本文可为深入了解CO₂的光还原过程提供一定帮助.

关键词: 薄层多孔g-C₃N₄, S型异质结, 光催化CO₂还原, Fe-MOF, 表面中间体

Abstract:

Regulating charge transfer to achieve specific transfer path can improve electron utilization and complete efficient photoreduction of CO₂. Here, we fabricated a S-scheme heterojunction of CN/Fe-MOF by an in-situ assembly strategy. The S-scheme charge transfer mechanism was confirmed by band structure, electron spin resonance (ESR) and work function (Φ) analysis. On the one hand, the response of Fe-MOF in the visible region improved the utilization of light energy, thus increasing the ability of CN/Fe-MOF to generate charge carriers. On the other hand, CN, as the active site, not only had strong adsorption capacity for CO₂, but also retained photogenerated electrons with high reduction capacity because of S-scheme charge transfer mechanism. Hence, in the absence of any sacrificial agent and cocatalyst, the optimized 50CN/Fe-MOF obtained the highest CO yield (19.17 μmol g^-1) under UV-Vis irradiation, which was almost 10 times higher than that of CN. In situ Fourier transform infrared spectra not only revealed that the photoreduction of CO₂ occurred at the CN, but also demonstrated that the S-scheme charge transfer mechanism enabled 50CN/Fe-MOF to have a stronger ability to generate HCOO^- than CN.

Key words: Thin layer porous g-C₃N₄, S-Scheme heterojunction, Photocatalytic CO₂ reduction, Fe-MOF, Surface intermediate

赵小雪, 许梦阳, 宋相海, 周伟强, 刘鑫, 霍鹏伟. Fe-MOF/g-C₃N₄嵌入式3D/2D S型异质结的构建及其光还原CO₂性能[J]. 催化学报, 2022, 43(10): 2625-2636.

Xiaoxue Zhao, Mengyang Xu, Xianghai Song, Weiqiang Zhou, Xin Liu, Pengwei Huo. 3D Fe-MOF embedded into 2D thin layer carbon nitride to construct 3D/2D S-scheme heterojunction for enhanced photoreduction of CO₂[J]. Chinese Journal of Catalysis, 2022, 43(10): 2625-2636.

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链接本文: https://www.cjcatal.com/CN/10.1016/S1872-2067(22)64115-9

https://www.cjcatal.com/CN/Y2022/V43/I10/2625

图/表 14

Scheme 1. Schematic of synthesis of CN/Fe-MOF.

Fig. 1. (a) XRD of all samples. (b) FT-IR spectra of CN, Fe-MOF and 50CN/ Fe-MOF.

Fig. 2. (a,b) SEM of Fe-MOF. (c) SEM of 50CN/Fe-MOF. (d-i) The element mappings of 50CN/Fe-MOF. (j) TEM of 50CN/Fe-MOF.

Fig. 3. (a) N2 adsorption-desorption isotherms. (b-d) BJH mesopore size distributions.

Table 1 SBET, pore volume and pore diameter of CN, Fe-MOF and 50CN/Fe-MOF.

Sample	S_BET (m² g^-1)	Average pore size (nm)	Pore volume (cm³ g^-1)
CN	48.021	22.923	0.344
Fe-MOF	7.545	15.554	0.049
50CN/Fe-MOF	203.470	9.340	0.459

Fig. 4. XPS spectra of samples. (a) C 1s; (b) Fe 2p; (c) O 1s; (d) N 1s.

Fig. 5. (a) CO evolution amount vs. illumination time. (b) AQY values for photocatalytic CO2 reduction over the 50CN/Fe-MOF at various wavelengths. (c) Evolution of CO under various reaction conditions. (d) Mass spectrum of the 13CO generated from the photoreduction of 13CO2 isotopic experiment.

Fig. 6. The PL (a) and TRPL (b) of CN, Fe-MOF and 50CN/ Fe-MOF. The TPR (c) and EIS (d) of all the photocatalysts. (e) The LSV of CN, Fe-MOF and 50CN/Fe-MOF in CO2. (f) The LSV of 50CN/Fe-MOF in N2 and CO2.

Table 2 The fitted parameters obtained from decay curves of the samples.

Sample	τ₁ (ns)	A₁ (%)	τ₂ (ns)	A₂ (%)	τ_av (ns)
CN	8.79	73.02	96.29	26.98	9.33
Fe-MOF	8.41	58.75	84.10	41.25	8.82
50CN/Fe-MOF	7.24	36.56	60.35	63.44	7.39

Fig. 7. The 3D color-mapped surface map with projection (a,d), in situ FT-IR spectra (b,e) and Partial enlarged view (c,f) for 50CN/Fe-MOF (a-c) and CN (d-f).

Fig. 8. (a) UV-vis diffuse reflectance spectra of all photocatalysts. (b) Tauc plots of CN, Fe-MOF and 50CN/Fe-MOF derived from the corresponding DRS.

Fig. 9. Mott-Schottky curves of CN (a) and Fe-MOF (b). The schematic diagram of the band structure of CN and Fe-MOF (c).

Fig. 10. (a) UPS spectra of CN and Fe-MOF. (b) The work functions of CN and Fe-MOF before/after contact and the formation of internal electric field. DMPO/•O2- (c) and DMPO/•OH (d) of ESR detection.

Fig. 11. The mechanism of S-scheme 3D/2D CN/Fe-MOF as a photocatalyst for CO2 reduction.

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Fe-MOF/g-C₃N₄嵌入式3D/2D S型异质结的构建及其光还原CO₂性能

3D Fe-MOF embedded into 2D thin layer carbon nitride to construct 3D/2D S-scheme heterojunction for enhanced photoreduction of CO₂

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[1]	蔡铭洁, 刘艳萍, 董珂欣, 陈晓波, 李世杰. 漂浮型Bi₂WO₆/C₃N₄/碳布S型异质结光催化材料用于高效净化水体环境[J]. 催化学报, 2023, 52(9): 239-251.
[2]	孙丽娟, 于晓慧, 唐丽永, 王伟康, 刘芹芹. 构建K₃PW₁₂O₄₀/CdS核壳S型异质结实现同步太阳能光催化分解水和选择性苯甲醇氧化反应[J]. 催化学报, 2023, 52(9): 164-175.
[3]	宋明明, 宋相海, 刘鑫, 周伟强, 霍鹏伟. ZnIn₂S₄/MOF-808微球结构S型异质结光催化剂的制备及其光还原CO₂性能研究[J]. 催化学报, 2023, 51(8): 180-192.
[4]	邵秀丽, 李可, 李静萍, 程强, 王国宏, 王楷. 揭示NiS@Ta₂O₅纳米纤维中梯型电荷转移路径及光催化CO₂转化性能[J]. 催化学报, 2023, 51(8): 193-203.
[5]	李世杰, 王春春, 董珂欣, 张鹏, 陈晓波, 李鑫. 新型MIL-101(Fe)/BiOBr S型异质催化剂用于高效光催化降解抗生素和还原六价铬: 光催化性能分析和光催化机理研究[J]. 催化学报, 2023, 51(8): 101-112.
[6]	李嘉明, 李源, 王小田, 杨直雄, 张高科. TiO₂上原子分散的Fe位点促进光催化CO₂还原: 增强的催化活性、 DFT计算和机制洞察[J]. 催化学报, 2023, 51(8): 145-156.
[7]	何厚伟, 王中辽, 代凯, 李素文, 张金锋. LSPR效应增强碳包覆In₂O₃/W₁₈O₄₉ S型异质结用于高效CO₂光还原[J]. 催化学报, 2023, 48(5): 267-278.
[8]	李瀚, 陶善仁, 万思杰, 邱国根, 龙庆, 余家国, 曹少文. ZnCdS纳米球和二苯并噻吩修饰的g-C₃N₄构成的S型异质结用于增强光催化产氢[J]. 催化学报, 2023, 46(3): 167-176.
[9]	陈成成, 刘芳庭, 张巧钰, 张正国, 刘琼, 方晓明. 理论设计和实验研究吡啶掺杂聚合氮化碳提升光催化CO₂还原性能[J]. 催化学报, 2023, 46(3): 91-102.
[10]	张志洁, 王雪盛, 唐慧玲, 李德本, 徐家跃. 调控Cs₃Bi₂Br₉@V_O-In₂O₃ S型异质结的费米能级和内建电场促进光生电荷分离和二氧化碳还原[J]. 催化学报, 2023, 55(12): 227-240.
[11]	吴优, 杨祎, 谷苗莉, 别传彪, 谭海燕, 程蓓, 许景三. 用于改进H₂O₂制备的1D/0D异质结的ZnIn₂S₄@ZnO S型光催化剂[J]. 催化学报, 2023, 53(10): 123-133.
[12]	王可, 程淼, 王楠, 张千一, 刘懿, 梁俊威, 管杰, 刘茂昌, 周建成, 李乃旭. 2D/2D超薄La₂Ti₂O₇/Ti₃C₂ Mxene肖特基异质结用于高效光催化CO₂还原[J]. 催化学报, 2023, 44(1): 146-159.
[13]	赵振龙, 边辑, 赵丽娜, 吴红君, 徐帅, 孙磊, 李志君, 张紫晴, 井立强. 2D ZnMOF/BiVO₄ S型异质结的构建及其可见光催化还原CO₂性能[J]. 催化学报, 2022, 43(5): 1331-1340.
[14]	赵君泽, 薛敏, 季梦夏, 王彬, 王雨, 李英杰, 陈自然, 李华明, 夏杰祥. “电子集流体”Bi₁₉S₂₇Br₃/BiOBr复合材料的制备及其增强光催化CO₂还原性能[J]. 催化学报, 2022, 43(5): 1324-1330.
[15]	徐阳锐, 朱晓蝶, 颜欢, 王盼盼, 宋旼珊, 马长畅, 陈自然, 储金宇, 刘馨琳, 逯子扬. 盐酸介导策略合成的具有优异光催化能力的ZnFe₂O₄小颗粒点缀一维苝二酰亚胺S型异质结[J]. 催化学报, 2022, 43(4): 1111-1122.