碳量子点介导的Fe11多金属氧酸盐用于促进Zn0.5Cd0.5S体系的光催化产氢

doi:10.1016/S1872-2067(26)65071-1

催化学报 ›› 2026, Vol. 88: 218-232.DOI: 10.1016/S1872-2067(26)65071-1

碳量子点介导的Fe₁₁多金属氧酸盐用于促进Zn_0.5Cd_0.5S体系的光催化产氢

Khalid Umer^a, 方潇^a, Khuram Hasnain^a, Hira Shahid^a, 孙玮泽^a, 石宸宇^a, 谢俊晗^a, 马宝春^a, 丁勇^a^,^b^,^*()

^a 兰州大学化学化工学院, 甘肃省先进催化重点实验室, 天然产物化学国家重点实验室, 甘肃兰州 730000
^b 中国科学院兰州化学物理研究所, 羰基合成与选择氧化国家重点实验室, 低碳催化与二氧化碳利用全国重点实验室, 甘肃兰州 730000

收稿日期:2026-02-03 接受日期:2026-03-20 出版日期:2026-09-18 发布日期:2026-09-05
通讯作者: *电子信箱: dingyong1@lzu.edu.cn (丁勇).
基金资助:
国家自然科学基金(22472071);国家自然科学基金(22075119);国家自然科学基金(12404325);甘肃省自然科学基金(21JR7RA440);兰州市科技储备项目(2025-3-015);2026年甘肃省高校研究生“创新之星”项目(2026CXZX-055)

Carbon quantum dot-mediated Fe₁₁ polyoxometalate enrichment for accelerated photocatalytic H₂ evolution in a Zn_0.5Cd_0.5S system

Khalid Umer^a, Xiao Fang^a, Khuram Hasnain^a, Hira Shahid^a, Weize Sun^a, Chenyu Shi^a, Junhan Xie^a, Baochun Ma^a, Yong Ding^a^,^b^,^*()

^a State Key Laboratory of Natural Product Chemistry, Key Laboratory of Advanced Catalysis of Gansu Province, College of Chemistry and Chemical Engineering, Lanzhou University, Lanzhou 730000, Gansu, China
^b State Key Laboratory of Low Carbon Catalysis and Carbon Dioxide Utilization; State Key Laboratory for Oxo Synthesis and Selective Oxidation, Lanzhou Institute of Chemical Physics, Chinese Academy of Sciences, Lanzhou 730000, Gansu, China

Received:2026-02-03 Accepted:2026-03-20 Online:2026-09-18 Published:2026-09-05
Contact: *E-mail: dingyong1@lzu.edu.cn (Y. Ding).
Supported by:
The National Natural Science Foundation of China(22472071);The National Natural Science Foundation of China(22075119);The National Natural Science Foundation of China(12404325);The Natural Science Foundation of Gansu Province(21JR7RA440);The Lanzhou Municipal-Level Science and Technology Reserve Project(2025-3-015);The Gansu Province Postgraduate Students Innovation Star Project(2026CXZX-055)

摘要/Abstract

摘要：

开发利用太阳能驱动水分解制氢技术是应对能源危机与环境污染的可持续方案. 半导体光催化剂, 如锌镉硫(Zn_xCd_1-_xS)固溶体, 因其优异的可见光吸收能力而备受关注, 然而其光生载流子易复合及固有的光腐蚀问题严重制约了催化效率与稳定性. 多金属氧酸盐(POMs)作为优异的电子传递介质, 在光催化中展现出巨大潜力, 但其均相体系下的高溶解性与易浸出特性限制了其回收利用与长期稳定性. 因此, 设计一种能够协同发挥半导体光吸收优势与POMs催化特性, 并同时解决两者固有缺陷的异质结光催化剂, 对于实现高效、稳定的太阳能制氢具有重要意义.
本研究核心创新在于通过界面工程设计, 利用碳量子点(CQDs)作为桥梁, 通过静电作用实现了Na₂₇[Fe₁₁(H₂O)₁₄(OH)₂(W₃O₁₀)₂(α-SbW₉O₃₃)₆](Fe₁₁)多金属氧酸盐(Fe₁₁POM)在Zn_0.5Cd_0.5S表面的有效富集与稳定固载, 构建了高性能三元光催化剂Fe₁₁POM@CQD@Zn_0.5Cd_0.5S, 协同优化了光生电荷的分离与传输路径. 具体工作如下: 采用水热法合成Zn_0.5Cd_0.5S与Fe₁₁POM, 并通过柠檬酸热解制备CQDs. 基于zeta电位分析证实Fe₁₁POM(-21.30 mV)与CQD@Zn_0.5Cd_0.5S(+12.81 mV)间存在强静电吸引, 因此采用分步组装策略制备了三元复合材料. X-射线衍射、红外光谱、X-射线光电子能谱、扫描电镜、透射电镜及能量散射谱等表征证实了材料的成功复合与紧密界面作用. 光催化测试表明, 在可见光(420 nm)照射下, 以乳酸为牺牲剂, 最优的Fe₁₁POM@CQD@Zn_0.5Cd_0.5S催化剂产氢速率高达32.18 mmol·g^-1·h^-1, 表观量子效率在420 nm处约为40%, 太阳能-氢能转换效率为1.69%. 其转化数和转化频率分别高达32394和10798 h^-1, 性能显著优于所有二元参比样品. 催化剂在连续5次循环后(15 h)活性未明显衰减, 循环后表征也证实了其优异的结构与化学稳定性. 光电化学表征(瞬态光电流、电化学抗阻谱、荧光光谱和时间分辨荧光光谱)结果表明, 三元复合物具有最强的光电流响应、最小的电荷转移阻抗及最有效的载流子分离效率. 开尔文探针力显微镜测试显示其光照下表面电势变化最高, 达76 mV, 直接证实了其最优的电荷分离能力. 基于能带结构分析, 提出了合理的光催化机理: 可见光激发Zn_0.5Cd_0.5S产生电子-空穴对; 光生电子经导带迁移至CQDs; CQDs作为电子中继站将电子快速传递至Fe₁₁POM的最低未占用分子轨道能级; Fe₁₁POM作为还原助催化剂将质子还原为H₂; 同时牺牲剂清除空穴, 抑制复合与光腐蚀. CQDs的多功能角色与Fe₁₁POM的催化功能协同作用, 是性能提升的关键.
综上, 本工作通过CQDs介导的静电组装策略, 成功构建了稳定、高效的三元光催化系统, 为解决POMs在多相催化中的溶解性难题及提升半导体光催化性能提供了新思路. 该研究不仅深化了对多元复合材料中界面电荷转移机制的理解, 也为设计开发兼具高活性、高稳定性的新型复合光催化剂提供了可借鉴的普适性策略, 对推动太阳能光催化制氢技术的实际应用具有参考价值.

关键词: 析氢反应, 含铁多金属氧酸盐, 三元催化剂, Zn_0.5Cd_0.5S, 碳量子点

Abstract:

Photocatalytic hydrogen evolution represents a sustainable and promising avenue for clean energy generation through harnessing solar energy. This study presents a photocatalytic system Fe₁₁POM@CQD@Zn_0.5Cd_0.5S, designed to enhance photocatalytic hydrogen evolution while addressing persistent environmental challenges. This advanced composite synergistically integrates iron polyoxometalate Na₂₇[Fe₁₁(H₂O)₁₄(OH)₂(W₃O₁₀)₂(α-SbW₉O₃₃)₆] (Fe₁₁POM) with carbon quantum dots (CQD) and a zinc cadmium sulfide (Zn_0.5Cd_0.5S) matrix, optimizing charge separation and light absorption efficiency. This composite exhibits a remarkable hydrogen production rate of 32.18 mmol·g^-1·h^-1, accompanied by a turnover number of 32,394 and a turnover frequency of 10798 h^-1. Notably, the apparent quantum yield reaches approximately 40%, while the solar-to-hydrogen efficiency is measured at 1.69%. The synergistic integration of Fe₁₁POM, the CQD and Zn_0.5Cd_0.5S components optimizes charge separation and transfer, significantly enhancing photocatalytic activity. This innovative approach provides a promising strategy for developing high-performance photocatalysts for sustainable hydrogen production, offering insights into the design of efficient heterostructures to address crises of energy scarcity and environmental pollution as well as pave the way for future research in multifunctional photocatalytic systems.

Key words: Hydrogen evolution, Iron containing polyoxometalate, Trinary catalyst, Zn_0.5Cd_0.5S, Carbon quantum dots

Khalid Umer, 方潇, Khuram Hasnain, Hira Shahid, 孙玮泽, 石宸宇, 谢俊晗, 马宝春, 丁勇. 碳量子点介导的Fe₁₁多金属氧酸盐用于促进Zn_0.5Cd_0.5S体系的光催化产氢[J]. 催化学报, 2026, 88: 218-232.

Khalid Umer, Xiao Fang, Khuram Hasnain, Hira Shahid, Weize Sun, Chenyu Shi, Junhan Xie, Baochun Ma, Yong Ding. Carbon quantum dot-mediated Fe₁₁ polyoxometalate enrichment for accelerated photocatalytic H₂ evolution in a Zn_0.5Cd_0.5S system[J]. Chinese Journal of Catalysis, 2026, 88: 218-232.

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链接本文: https://www.cjcatal.com/CN/10.1016/S1872-2067(26)65071-1

https://www.cjcatal.com/CN/Y2026/V88/I9/218

图/表 10

Fig. 1. (a) Schematic illustration of synthesis strategy. (b) Design of a three-component photocatalytic system.

Fig. 2. (a) FT-IR spectra of Fe11POM, CQD@Zn0.5Cd0.5S, and Fe11POM@CQD@Zn0.5Cd0.5S. (b) XRD plot of CQD, Zn0.5Cd0.5S and CQD@Zn0.5Cd0.5S, Fe11POM and Fe11POM@CQD@Zn0.5Cd0.5S. SEM images of Zn0.5Cd0.5S (c), CQD@Zn0.5Cd0.5S (d), and Fe11POM@CQD@Zn0.5Cd0.5S (e).

Fig. 3. (a) TEM image of Fe11POM@CQD@Zn0.5Cd0.5S. (b) HRTEM image of Fe11POM@CQD@Zn0.5Cd0.5S. (c-e) EDS mapping of the various elements present in Fe11POM@CQD@Zn0.5Cd0.5S.

Fig. 4. High resolution XPS spectra containing comparison of peaks in Zn0.5Cd0.5S and Fe11POM@CQD@Zn0.5Cd0.5S: Zn 2p (a); Cd 3d (b); S 2p (c). XPS spectrum comparison of peaks presented in Fe11POM and Fe11POM@CQD@Zn0.5Cd0.5S for region: Fe 2p (d); Sb 3d (e); W 4f (f).

Fig. 5. (a) Photocatalytic hydrogen evolution rate using CdS (1), Mn0.5Cd0.5S (2), Zn0.5Cd0.5S (3), MoS2 (4), Mn-MoS2 (5), Zn-MoS2 (6), SnS2 (7), Mn-SnS2 (8), and Zn-SnS2 (9) catalysts. (b) Photocatalytic hydrogen evolution activity by attaching Fe11POM with catalysts CdS, Mn0.5Cd0.5S, Zn0.5Cd0.5S, MoS2, Mn-MoS2, Zn-MoS2, SnS2, Mn-SnS2 and Zn-SnS2. (c) Photocatalytic hydrogen evolution activity of CQD@CdS, CQD@Mn0.5Cd0.5S, CQD@Zn0.5Cd0.5S, CQD@MoS2, CQD@Mn-MoS2, CQD@Zn-MoS2, CQD@SnS2, CQD@Mn-SnS2 and CQD@Zn-SnS2. (d,e) Photocatalytic hydrogen evolution activity of Fe11POM@CQD@Zn0.5Cd0.5S, Fe11POM@Zn0.5Cd0.5S, CQD@Zn0.5Cd0.5S and Zn0.5Cd0.5S. (f) Durability test for composite photocatalyst material Fe11POM@CQD@Zn0.5Cd0.5S under same reaction conditions. (g) Comparison of AQY for H2 evolution of reported POM based catalysts with Fe11POM@CQD@Zn0.5Cd0.5S. Reaction conditions: 29 mL reactor, 5 mg of catalyst, 15 mL of aqueous lactic acid solution (10%, v/v), light source 420 nm LED lamp (100 mW·cm-2).

Fig. 6. (a) FT-IR spectra and (b) XRD patterns of fresh and used Fe11POM@CQD@Zn0.5Cd0.5S catalyst. XPS analysis of Fe11POM@CQD@Zn0.5Cd0.5S catalyst in its fresh and used states for Fe 2p (c), W 4f (d), Cd 3d (e), Zn 2p (f), S 2p (g), O 1s (h), and C 1s (i).

Fig. 7. (a) UV-vis DRS measurements of Fe11POM@CQD@Zn0.5Cd0.5S, CQD@Zn0.5Cd0.5S, Zn0.5Cd0.5S, Fe11POM, and CQD. (b) Tauc plots of Zn0.5Cd0.5S. (c) Mott-Schottky plot of Zn0.5Cd0.5S and Fe11POM. (d) VB-XPS of Fe11POM.

Fig. 8. (a) The transient i-t curves, (b) EIS plots and (c) PL emission spectra of Zn0.5Cd0.5S, Fe11POM and Fe11POM@CQD@Zn0.5Cd0.5S. (d) TRPLS of Zn0.5Cd0.5S and Fe11POM@CQD@Zn0.5Cd0.5S.

Fig. 9. (a-d) KPFM images of Fe11POM, Zn0.5Cd0.5S, CQD@Zn0.5Cd0.5S, and Fe11POM@CQD@Zn0.5Cd0.5S. (e-h) KPFM potential images of Fe11POM, Zn0.5Cd0.5S, CQD@Zn0.5Cd0.5S and Fe11POM@CQD@Zn0.5Cd0.5S under dark conditions. (i-l) KPFM images of Fe11POM, Zn0.5Cd0.5S, CQD@Zn0.5Cd0.5S and Fe11POM@CQD@Zn0.5Cd0.5S under light conditions. (m-p) Surface potential distribution diagrams across Fe11POM, Zn0.5Cd0.5S, CQD@Zn0.5Cd0.5S and Fe11POM@CQD@Zn0.5Cd0.5S before and after illumination.

Fig. 10. Possible reaction mechanism of photocatalytic hydrogen evolution reaction using Fe11POM@CQD@Zn0.5Cd0.5S system.

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碳量子点介导的Fe₁₁多金属氧酸盐用于促进Zn_0.5Cd_0.5S体系的光催化产氢

Carbon quantum dot-mediated Fe₁₁ polyoxometalate enrichment for accelerated photocatalytic H₂ evolution in a Zn_0.5Cd_0.5S system

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