NiS助催化剂的硫调控光沉积合成及其增强g-C3N4的光催化产氢性能

doi:10.1016/S1872-2067(20)63633-6

催化学报 ›› 2021, Vol. 42 ›› Issue (1): 37-45.DOI: 10.1016/S1872-2067(20)63633-6

NiS助催化剂的硫调控光沉积合成及其增强g-C₃N₄的光催化产氢性能

王敏^a, 程晶晶^a, 王雪飞^a^,^*(), 洪学鹍^b, 范佳杰^c, 余火根^a^,^d^,^#()

^a武汉理工大学化学化工与生命科学学院化学系, 湖北武汉430070
^b常熟理工学院物理与电子工程学院, 江苏常熟215500
^c郑州大学材料科学与工程学院, 河南郑州450001
^d武汉理工大学硅酸盐建筑材料国家重点实验室, 湖北武汉430070

收稿日期:2020-01-24 接受日期:2020-03-06 出版日期:2021-01-18 发布日期:2021-01-18
通讯作者: 王雪飞,余火根
基金资助:
国家自然科学基金(51672203);中央高校基本科研业务费专项基金(WUT2019IB002);中央高校基本科研业务费专项基金(185220002)

Sulfur-mediated photodeposition synthesis of NiS cocatalyst for boosting H₂-evolution performance of g-C₃N₄ photocatalyst

Min Wang^a, Jingjing Cheng^a, Xuefei Wang^a^,^*(), Xuekun Hong^b, Jiajie Fan^c, Huogen Yu^a^,^d^,^#()

^aDepartment of Chemistry, School of Chemistry, Chemical Engineering and Life Sciences, Wuhan University of Technology, Wuhan 430070, Hubei, China
^bCollege of Physics and Electronic Engineering, Changshu Institute of Technology, Changshu 215500, Jiangsu, China
^cSchool of Materials Science and Engineering, Zhengzhou University, Zhengzhou 450001, Henan, China
^dState Key Laboratory of Silicate Materials for Architectures, Wuhan University of Technology, Wuhan 430070, Hubei, China

Received:2020-01-24 Accepted:2020-03-06 Online:2021-01-18 Published:2021-01-18
Contact: Xuefei Wang,Huogen Yu
About author:^#E-mail: yuhuogen@whut.edu.cn
^*Tel: +86-27-87756662, Fax: +86-27-87879468; E-mail: xuefei@whut.edu.cn;
Supported by:
National Natural Science Foundation of China(51672203);Fundamental Research Funds for the Central Universities(WUT2019IB002);Fundamental Research Funds for the Central Universities(185220002)

摘要/Abstract

摘要：

作为一种非金属聚合半导体, 石墨相氮化碳(g-C₃N₄)具有特殊的能带结构、可见光响应能力以及优良的物理化学性质以及生产成本低等特点, 因而已成为目前光催化领域的研究热点. 然而, 由于g-C₃N₄被光激发的电子与空穴极易复合, 导致g-C₃N₄材料的光催化性能并不理想. 而助剂修饰是实现光生载流子有效分离以提高光催化活性的有效途径. 众所周知, 贵金属Pt可以作为光催化产氢的反应位点, 但高昂的成本限制了它的实际应用. 所以, 开发高效的非贵金属助剂很有必要. 近年来, NiS作为优良的电子助剂在光催化领域受到广泛关注. 大量研究表明, NiS可以作为g-C₃N₄的产氢活性位点用于提高其光催化产氢性能. NiS助剂主要是通过水热、煅烧和液相沉淀的方法修饰在g-C₃N₄的表面上. 相较而言, 助剂的光沉积方法具有一些独特的优势, 例如节能、环保、简易并且能够实现其原位牢固地沉积在光催化剂的表面. 然而g-C₃N₄光生电子和空穴强还原和氧化能力容易导致像Ni²⁺的还原和S^2-的氧化等副反应发生, 因此NiS助剂很难光沉积在g-C₃N₄材料表面.
本文采用硫调控的光沉积法成功合成了NiS/g-C₃N₄光催化材料, 该法利用g-C₃N₄在光照条件下产生的光生电子结合S以及Ni²⁺生成NiS, 然后原位沉积在g-C₃N₄表面. 由于E⁰(S/NiS)(0.096 V)比E⁰(Ni²⁺/Ni)(-0.23 V)更正, 所以NiS优先原位沉积在g-C₃N₄表面. 因此, 硫调控的光沉积法促进了NiS的生成, 并抑制了金属Ni等副反应的形成.
通过X射线光电子能谱分析NiS/g-C₃N₄的表面化学态, 表明该方法能成功地将NiS修饰在g-C₃N₄的表面, 这也得到透射电镜和高分辨透射电镜结果的证实. 光催化产氢的结果表明, NiS/g-C₃N₄光催化剂实现了良好的光催化性能, 其最优产氢速率(244 μmol h^-1 g^-1)接近于1 wt% Pt/g-C₃N₄(316 μmol h^-1 g^-1). 这是因为硫调控的光沉积法实现NiS助剂在g-C₃N₄表面的修饰, 从而促进光生电子与空穴的有效分离, 进而提高光催化制氢效率. 此外, 在该方法中, NiS的形成通常在g-C₃N₄光生电子的表面传输位点上, 因此也能够使NiS提供更多的活性位点以提高界面产氢催化反应速率. 电化学表征结果也进一步证明NiS/g-C₃N₄光催化剂加快了电子与空穴的分离和转移. 更重要的是, 这种简易且通用的方法还可以实现CoS_x, CuS_x, AgS_x对g-C₃N₄的助剂修饰, 并且都提高了g-C₃N₄的光催化产氢性能, 表明该方法具有一定的普适性, 为高效光催化材料的合成提供了新的思路.

关键词: g-C₃N₄, NiS, 助剂, 硫调控的光沉积法, 氢气, 光催化

Abstract:

Modification of nickel sulfide cocatalysts is considered to be a promising approach for efficient enhancement of the photocatalytic hydrogen production performance of g-C₃N₄. Providing more NiS cocatalyst to function as active sites of g-C₃N₄ is still highly desirable. To realize this goal, in this work, a facile sulfur-mediated photodeposition approach was developed. Specifically, photogenerated electrons excited by visible light reduce the S molecules absorbed on g-C₃N₄ surface to S^2-, and subsequently NiS cocatalyst is formed in situ on the g-C₃N₄ surface by a combination of Ni²⁺ and S^2- due to their small solubility product constant (K_sp = 3.2 × 10^-19). This approach has several advantages. The NiS cocatalyst is clearly in situ deposited on the photogenerated electron transfer sites of g-C₃N₄, and thus provides more active sites for H₂ production. In addition, this method utilizes solar energy with mild reaction conditions at room temperature. Consequently, the synthesized NiS/g-C₃N₄ photocatalyst achieves excellent hydrogen generation performance with the performance of the optimal sample (244 μmol h^-1 g^-1) close to that of 1 wt% Pt/g-C₃N₄ (316 μmol h^-1 g^-1, a well-known excellent photocatalyst). More importantly, the present sulfur-mediated photodeposition route is versatile and facile and can be used to deposit various metal sulfides such as CoS_x, CuS_x and AgS_x on the g-C₃N₄ surface, and all the resulting metal sulfide-modified g-C₃N₄ photocatalysts exhibit improved H₂-production performance. Our study offers a novel insight for the synthesis of high-efficiency photocatalysts.

Key words: g-C3N4, NiS, Co-catalyst, Sulfur-mediated photodeposition, H2, Photocatalysis

王敏, 程晶晶, 王雪飞, 洪学鹍, 范佳杰, 余火根. NiS助催化剂的硫调控光沉积合成及其增强g-C₃N₄的光催化产氢性能[J]. 催化学报, 2021, 42(1): 37-45.

Min Wang, Jingjing Cheng, Xuefei Wang, Xuekun Hong, Jiajie Fan, Huogen Yu. Sulfur-mediated photodeposition synthesis of NiS cocatalyst for boosting H₂-evolution performance of g-C₃N₄ photocatalyst[J]. Chinese Journal of Catalysis, 2021, 42(1): 37-45.

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图/表 9

Fig. 1. (A) Schematic illustration of the synthesis of NiS/g-C3N4 in an ethanol system; (B) Schematics of g-C3N4 suspension (a), S2-/g-C3N4 suspension (b), Ni/g-C3N4 suspension (c), and NiS/g-C3N4 suspension (d) and corresponding redox potentials; (C) Schematic illustration of the formation of the NiS/g-C3N4 sample and the proposed photocatalytic hydrogen-generation mechanism of NiS/g-C3N4.

Fig. 2. FESEM/EDS images of various samples. (A) g-C3N4; (B) NiS/g-C3N4(1 wt%); (C) NiS/g-C3N4(3 wt%); (D) NiS/g-C3N4(5 wt%). TEM (E) and HRTEM (F) images of NiS/g-C3N4(1 wt%).

Fig. 3. XRD patterns of various samples. (a) g-C3N4; (b) NiS/g-C3N4(0.1 wt%); (c) NiS/g-C3N4(0.3 wt%); (d) NiS/g-C3N4(1 wt%); (e) NiS/g- C3N4(3 wt%).

Fig. 4. (A) Full-range XPS spectra and the high-resolution XPS spectra of C 1s (B), N 1s (C), O 1s (D), Ni 2p (E) and S 2p (F) for various samples. (a) g-C3N4; (b) NiS/g-C3N4(0.3 wt%); (c) NiS/g-C3N4(1 wt%); (d) NiS/g-C3N4(3 wt%).

Table 1 Elemental content (at%) of the various samples based on the XPS results.

Sample	C	N	O	Ni	S
g-C₃N₄	43.95	53.06	2.99	0	0
NiS/g-C₃N₄(0.3 wt%)	44.78	49.77	4.07	0.65	0.73
NiS/g-C₃N₄(1 wt%)	44.33	45	7.30	1.7	1.67
NiS/g-C₃N₄(3 wt%)	42.62	43.96	8.46	2.18	2.78

Fig. 5. (A) FTIR spectra, and (B) UV-vis absorption spectra and photographs (inset) of various samples: (a) g-C3N4, (b) NiS/g-C3N4(0.05 wt%), (c) NiS/g-C3N4(0.1 wt%), (d) NiS/g-C3N4(0.3 wt%), (e) NiS/g-C3N4(1 wt%) and (f) NiS/g-C3N4(3 wt%).

Fig. 6. (A) Photocatalytic H2-evolution rate of various samples. (B) Recycling test of NiS/g-C3N4(0.3 wt%) sample; (C) Transient photocurrent responses; (D) Electrochemical impedance spectra curves. (a) g-C3N4; (b) NiS/g-C3N4(0.05 wt%); (c) NiS/g-C3N4(0.1 wt%); (d) NiS/g-C3N4(0.3 wt%); (e) NiS/g-C3N4(1 wt%); (f) NiS/g-C3N4(3 wt%); (g) NiS/g-C3N4(0.3 wt%, wet-chemistry method); (h) Pt/g-C3N4(1 wt%).

Fig. 7. FESEM/EDS results for various samples. (A) CoSx/g-C3N4; (B) CuSx/g-C3N4; (C) AgSx/g-C3N4.

Fig. 8. (A) UV-vis absorption spectra and photographs (inset) and (B) Photocatalytic H2 evolution rate for various samples. (a) g-C3N4; (b) CoSx/g-C3N4; (c) CuSx/g-C3N4; (d) AgSx/g-C3N4.

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NiS助催化剂的硫调控光沉积合成及其增强g-C₃N₄的光催化产氢性能

Sulfur-mediated photodeposition synthesis of NiS cocatalyst for boosting H₂-evolution performance of g-C₃N₄ photocatalyst

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