物理化学学报 >> 2026, Vol. 42 >> Issue (10): 100221.doi: 10.1016/j.actphy.2025.100221

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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

范育歌, 付先亮*(), 朱丽, 徐慢*()   

  1. 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
  • 收稿日期:2025-10-14 修回日期:2025-11-14 录用日期:2025-11-16 发布日期:2026-09-03
  • 通讯作者: Email: fuxl@wit.edu.cn (付先亮)xuman@wit.edu.cn (徐慢)

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

Yuge Fan, Xianliang Fu*(), Li Zhu, Man Xu*()   

  1. 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
  • Received:2025-10-14 Revised:2025-11-14 Accepted:2025-11-16 Published:2026-09-03
  • Contact: Email: fuxl@wit.edu.cn (Xianliang Fu)xuman@wit.edu.cn (Man Xu)

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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(ⅤCd，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ⅤCd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

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 (ⅤCd, 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 ⅤCd 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: Cd vacancy, MoS2/CdS, KSCN molten salt method, Hydrogen evolution, Photocatalysis