设计p-n同质结构实现碳氮光催化剂的全解水性能

doi:10.1016/S1872-2067(20)63670-1

催化学报 ›› 2021, Vol. 42 ›› Issue (3): 501-509.DOI: 10.1016/S1872-2067(20)63670-1

• 论文 • 上一篇

设计p-n同质结构实现碳氮光催化剂的全解水性能

赵刚^a,†, 郝树华^a,†, 郭静华^a, 邢钰鹏^a, 张雷^b, 徐锡金^a^,^*()

^a济南大学物理科学与技术学院,功能微纳材料与器件实验室,山东济南250022
^b山东大学晶体功能材料国家重点实验室,山东济南250100

收稿日期:2020-05-21 接受日期:2020-06-27 出版日期:2021-03-18 发布日期:2021-01-23
通讯作者: 徐锡金
作者简介:^†共同第一作者.
基金资助:
国家自然科学基金(ZR2018BEM019);山东省自然科学基金重大基础研究项目(ZR2018BEM019);山东省自然科学基金(ZR2018BEM019)

Design of p-n homojunctions in metal-free carbon nitride photocatalyst for overall water splitting

Gang Zhao^a,†, Shuhua Hao^a,†, Jinghua Guo^a, Yupeng Xing^a, Lei Zhang^b, Xijin Xu^a^,^*()

^aLaboratory of Functional Micro-nano Material and Device,School of Physics and Technology,University of Jinan,Jinan 250022,Shandong,China
^bState Key Lab of Crystal Materials,Shandong University,Jinan 250100,Shandong,China

Received:2020-05-21 Accepted:2020-06-27 Online:2021-03-18 Published:2021-01-23
Contact: Xijin Xu
About author:^*Tel/Fax:+86-531-82769995; E-mail: sps_xuxj@ujn.edu.cn
First author contact:^†These authors contributed equally to this work.
Supported by:
National Natural Science Foundation of China (51802177,51672109,11504134)(ZR2018BEM019);Major Basic Program of the Natural Science Foundation of Shandong Province(ZR2018BEM019);Natural Science Foundation of Shandong Province(ZR2018BEM019)

摘要/Abstract

摘要：

非金属氮化碳(CN)因其独特的光催化性能而备受关注. 本文利用水热处理、高温烧结、高能球磨和烧结的方法成功制得一种具有混合结构的CN光催化剂. 先以三聚氰胺为原料进行水热处理(180^oC,24 h),过滤干燥后,转移到高纯氩气保护下的管式炉中,于550^oC处理1 h得到CN材料. 然后将CN用三聚氰胺和氟化铵水热180^oC处理24 h,过滤、干燥、煅烧(550 ^oC,1 h)得到第二种材料. 最后将其与CN材料按等比例混合,经高能球磨研磨,再于管式炉中在气氛保护下淬火,得到最终催化剂样品. 由于这种结构的界面作用,使CN光催化剂显示出了高的光催化活性. 它的产氢效果可以高达17028.82 μmol h^-1 g^-1,在420 nm光照下,其光量子效率也达到11.2%. 随后,采用纳秒级别的时间分辨萤光(PL)光谱测得其荧光寿命为9.9 ns. 有助于电子与空穴参与反应更有趣的是,在不加牺牲剂时,该光催化剂具有高效的全解水效果,其产氢效率为270.95 μmol h ^-1 g^-1,产氧效率为115.21 μmol h ^-1 g^-1,有望实际用于全解水反应中. 另外,通过紫外可见漫反射光谱,PL光谱和材料的比表面等测试来考察该CN光催化剂效果好的原因. 发现该材料具有更高比表面积有更多活性点参与反应. 同时,通过电化学测试获得了肖特基曲线和电流-电压曲线,发现该光催化剂里含有少量的pn结构,这种结构使材料在弱光下也会产生光生载流子,实际上它是起到光生载流子的激发作用,即在相同光照下,就会产生更多的光生载流子数量,从而进一步提高了其催化效果. 因此,本工作对优化碳氮光催化剂的催化效果有很好的指导意义.

关键词: 二维非金属光催化剂, 氮化碳, 全解水, 时间分辨光谱, 密度泛函理论, 多相结构

Abstract:

Two-dimensional (2D) carbon nitride (CN) photocatalysts are attracting extensive attention owing to their excellent photocatalytic properties. In this study,we successfully prepared CN materials with heterogeneous structures via hydrothermal treatment,high-temperature roasting,ball milling,sintering,and other processes. Benefitting from interface interactions in hybrid architectures,the CN photocatalysts exhibited high photocatalytic activity. The rate of hydrogen production using these CN photocatalysts reached 17028.82 μmol h-1 g-1,and the apparent quantum efficiency was 11.2% at 420 nm. The ns-level time-resolved photoluminescence (PL) spectra provided information about the time-averaged lifetime of fluorescence charge carriers; the lifetime of the charge carriers causing the fluorescence of CN reached 9.99 ns. Significantly,the CN photocatalysts displayed satisfactory results in overall water splitting without the addition of sacrificial agents. The average hydrogen and oxygen production rates were 270.95 μmol h-1 g-1 and 115.21 μmol h-1 g-1 in 7 h,respectively,which were promising results for the applications of the catalysts in overall water splitting processes. We investigated the high efficiency of the prepared CN photocatalysts via a series of tests (UV-vis diffuse reflectance spectroscopy,photocurrent response measurements,PL emission spectroscopy,time-resolved PL spectroscopy,and Brunauer-Emmett-Teller analysis). Furthermore,the Mott-Schottky plot and current-voltage curve were acquired via electrochemical tests. The fabricated CN photocatalyst had a small p-n junction in its heterogeneous structure,which further enhanced its photocatalytic efficiency. Therefore,this work can promote the development of CN photocatalysts.

Key words: Heterogeneous structure, 2D Metal-free photocatalyst, Carbon nitride, Overall water splitting, Time-resolved photoluminescence, spectra, Density-functional theory, Heterogeneous structure

赵刚, 郝树华, 郭静华, 邢钰鹏, 张雷, 徐锡金. 设计p-n同质结构实现碳氮光催化剂的全解水性能[J]. 催化学报, 2021, 42(3): 501-509.

Gang Zhao, Shuhua Hao, Jinghua Guo, Yupeng Xing, Lei Zhang, Xijin Xu. Design of p-n homojunctions in metal-free carbon nitride photocatalyst for overall water splitting[J]. Chinese Journal of Catalysis, 2021, 42(3): 501-509.

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链接本文: https://www.cjcatal.com/CN/10.1016/S1872-2067(20)63670-1

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图/表 9

Fig. 1. Process flow diagram of the preparation of CN photocatalyst with a heterogeneous structure.

Fig. 2. SEM images of CN nanotubes (a),CN nanosheets (b),CN photocatalyst (c) with heterogeneous structure,and ordinary g-C3N4 photocatalyst (d); IR spectra (e) and XRD patterns (f) of photocatalysts.

Fig.3. (a) Typical time course of H2 production from aqueous solution (100 mL) containing triethanolamine (20 vol%) as a sacrificial electron donor and 50 mg of 1 wt% Pt-loaded catalyst under 300 W Xe lamp with an optical cut-off filter (λ > 420 nm); (b) Hydrogen evolution rates with different CN photocatalysts; (c) Wavelength dependent AQE by this work-CN; (d) H2 and O2 production from aqueous solution (100 mL) and 50 mg of 1 wt% Pt-loaded catalyst under 300 W Xe lamp; (e) H2 and O2 evolution rates based on this work-CN photocatalyst; (f) H2 and O2 evolution cycling curves of this work-CN photocatalyst.

Fig.4. (a) UV-vis diffuse reflectance spectra of different CN photocatalysts; (b) Plot of (AEphoton)2-Ephoton; (c) Photocurrent response of samples to on-off cycles of illumination; (d) PL emission spectra.

Fig. 5. ns-Level time-resolved PL spectra monitored at 450 nm under 420 nm excitation for CN nanotubes (a),CN nanosheets (b),and this work-CN (c)

Fig. 6. Typical nitrogen adsorption-desorption isotherms of different CN photocatalysts. (a) CN nanotubes; (b) CN nanosheets; (c) this work-CN; (d) g-C3N4.

Fig. 7. High-resolution XPS spectra of different CN photocatalysts. (a,c,e) C1s; (b,d,f) N1s.

Fig. 8. Optimized structures of C2.83N (a) and C0.82N (b); carbon atoms are gray and nitrogen atoms are blue. Electronic band structures of C2.83N (c) and C0.82N (d). The energy at the Fermi level was set to zero. (e,f) Mott-Schottky plots for determining CN nanotubes and nanosheets.

Fig. 9. (a) Characteristic current-voltage curve of CN (this work). (b) Schematic diagram showing the production of hydrogen and oxygen,energy band structure,and electron-hole pair separation in this CN photocatalyst containing a p-n heterojunction.

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设计p-n同质结构实现碳氮光催化剂的全解水性能

Design of p-n homojunctions in metal-free carbon nitride photocatalyst for overall water splitting

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