微小改变，显著差异：改良KSCN熔盐法一锅制备富Cd空位MoS<sub>2</sub>/CdS并实现光催化产氢性能提升

引用本文: 范育歌, 付先亮, 朱丽, 徐慢. 微小改变，显著差异：改良KSCN熔盐法一锅制备富Cd空位MoS₂/CdS并实现光催化产氢性能提升[J]. 物理化学学报, 2026, 42(10): 100221. doi: 10.1016/j.actphy.2025.100221 shu

Citation: Yuge Fan, Xianliang Fu, Li Zhu, Man Xu. Small changes, big differences: modified KSCN molten salt method for one-pot synthesis of Cd vacancy-enriched MoS₂/CdS and the enhanced photocatalytic H₂ evolution performance[J]. Acta Physico-Chimica Sinica, 2026, 42(10): 100221. doi: 10.1016/j.actphy.2025.100221 shu

微小改变，显著差异：改良KSCN熔盐法一锅制备富Cd空位MoS₂/CdS并实现光催化产氢性能提升

武汉工程大学材料科学与工程学院, 湖北省环境材料与膜技术工程技术研究中心, 湖北武汉 430073

通讯作者: 付先亮,徐慢,E-mail:fuxl@wit.edu.cn; 徐慢,E-mail:xuman@wit.edu.cn

基金项目:
本研究得到武汉工程大学研究生教育创新基金项目(CX2024301)与国家自然科学基金项目(52302365)的资助

摘要: 低温KSCN熔盐法已被用于一锅制备修饰型硫化物基光催化剂。然而，由于S₂^-的供给依赖于相对稳定的KSCN热分解，该反应体系实际存在S前体不足的问题，这可能不利于高性能催化剂的制备。为此，我们开发了一种添加外部硫源的改良KSCN熔盐法，并以1% MoS₂/CdS为原型进行了一锅制备。结果表明，与传统KSCN熔盐法制备的样品(MC)相比，在富S₂^-环境中可轻松制备出富罕见Cd空位(V_Cd，MC-S)的高效样品。此外，由于熔盐中能引入更多晶核，CdS与MoS₂的尺寸均可从微米级显著减小至纳米级，从而获得少层MoS₂均匀紧密锚定于平均尺寸仅为~33 nm的CdS上的复合结构。最终所得MC-S样品展现出15.01 mmol h^-1 g^-1的卓越产氢活性，较传统KSCN熔盐法制备的对照样品(MC)提升达6.5倍。这种高活性主要归因于V_Cd的引入以及小尺寸CdS与少层MoS₂之间的强耦合界面，二者均有利于电子-空穴分离。我们通过对比晶体成核与生长过程的差异，初步探讨了样品的形成机制。相信这种改进的制备方法也将有助于其他高性能硫化物基光催化剂的合成。

关键词:

Cd空位
/ MoS₂/CdS
/ KSCN熔盐法
/ 析氢
/ 光催化

English

Small changes, big differences: modified KSCN molten salt method for one-pot synthesis of Cd vacancy-enriched MoS₂/CdS and the enhanced photocatalytic H₂ evolution performance

Engineering Research Center of Environmental Materials and Membrane Technology of Hubei Province, School of Materials Science and Engineering, Wuhan Institute of Technology, Wuhan 430073, Hubei Province, China

Corresponding author: Xianliang Fu, ; Man Xu,

Received Date: 14 October 2025
Accepted Date: 16 November 2025
Revised Date: 14 November 2025

Abstract: Low-temperature KSCN molten salt method has been used for one-pot fabrication of decorated sulfide-based photocatalysts. However, the reaction system is actually short of S precursor, as it is determined by the decomposition of relatively stable KSCN, which may not be conducive to the production of high-performance catalysts. To this end, a modified KSCN flux route with a dosage of external S source was developed and used for the one-pot preparation of sulfide photocatalyst with 1% MoS₂/CdS as the prototype. The results indicated that, compared with the sample (MC) prepared in conventional KSCN flux, a highly efficient sample enriched with seldom reported Cd vacancy (V_Cd, MC-S) could be readily fabricated under the S₂^--rich environment. Furthermore, both the size of CdS and MoS₂ could be substantially reduced from micrometer to nanometer scale as more nuclei could be introduced in the flux, which leads to a few-layer MoS₂ that can be uniformly and tightly anchored on CdS with the average size of only ~33 nm. Consequently, the resulting MC-S demonstrated an exceptional H₂ evolution activity of 15.01 mmol h^-1 g^-1, a significant 6.5-fold improvement over its counterpart (MC) prepared through traditional KSCN molten salt method. The high activity can be mainly ascribed to the introduction of V_Cd and the close interface between small CdS and few-layer MoS₂, which both benefit electron-hole separation. The preparation mechanism of the samples was tentatively compared and discussed from the difference in the nucleation and the development of crystals. We believe that this improved preparation method will also benefit the synthesis of other high-performance sulfide-based photocatalysts.

Key words:

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1.
沈阳化工大学材料科学与工程学院沈阳 110142

微小改变，显著差异：改良KSCN熔盐法一锅制备富Cd空位MoS₂/CdS并实现光催化产氢性能提升

通讯作者: 付先亮,徐慢,E-mail:fuxl@wit.edu.cn; 徐慢,E-mail:xuman@wit.edu.cn

English

Small changes, big differences: modified KSCN molten salt method for one-pot synthesis of Cd vacancy-enriched MoS₂/CdS and the enhanced photocatalytic H₂ evolution performance

Corresponding author: Xianliang Fu, ; Man Xu,

CCS Chemistry：嵌段共聚物自组装成 “三明治”二维有机材料，实现纳米级压力传感功能

CCS Chemistry：颜徐州、鲍哲南：你的皮肤可能是一片SPMs

CCS Chemistry：工作高效不疲劳，只须让催化剂动起来

CCS Chemistry：静电组装导向聚合- 聚电解质纳米凝胶量化制备新策略

CCS Chemistry：金黄色葡萄球菌醛基脱氢酶是如何识别特异性底物的？

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中国化学会秘书处

微小改变，显著差异：改良KSCN熔盐法一锅制备富Cd空位MoS2/CdS并实现光催化产氢性能提升

通讯作者: 付先亮,徐慢,E-mail:fuxl@wit.edu.cn; 徐慢,E-mail:xuman@wit.edu.cn

English

Small changes, big differences: modified KSCN molten salt method for one-pot synthesis of Cd vacancy-enriched MoS2/CdS and the enhanced photocatalytic H2 evolution performance

Corresponding author: Xianliang Fu, ; Man Xu,

CCS Chemistry：嵌段共聚物自组装成 “三明治”二维有机材料，实现纳米级压力传感功能

CCS Chemistry：颜徐州、鲍哲南： 你的皮肤可能是一片SPMs

CCS Chemistry：工作高效不疲劳，只须让催化剂动起来

CCS Chemistry：静电组装导向聚合- 聚电解质纳米凝胶量化制备新策略

CCS Chemistry：金黄色葡萄球菌醛基脱氢酶是如何识别特异性底物的？

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通讯作者: 陈斌, bchen63@163.com

中国化学会秘书处

微小改变，显著差异：改良KSCN熔盐法一锅制备富Cd空位MoS₂/CdS并实现光催化产氢性能提升

Small changes, big differences: modified KSCN molten salt method for one-pot synthesis of Cd vacancy-enriched MoS₂/CdS and the enhanced photocatalytic H₂ evolution performance

CCS Chemistry：颜徐州、鲍哲南：你的皮肤可能是一片SPMs