A Synthetic Route to MoS2 Catalysts Supported on a Metal–Organic Framework for Electrochemical Hydrogen Evolution Reaction Utilizing Chemical Vapor Deposition,Energy & Fuels

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A Synthetic Route to MoS2 Catalysts Supported on a Metal–Organic Framework for Electrochemical Hydrogen Evolution Reaction Utilizing Chemical Vapor Deposition
Energy & Fuels ( IF 5.2 ) Pub Date : 2021-12-20 , DOI: 10.1021/acs.energyfuels.1c03454
Kenichi Nishigaki _{1,

2} , Makoto Katagiri ₁ , Masaya Matsuoka ₁ , Yu Horiuchi ₁

Affiliation

MoS₂ catalysts for electrochemical hydrogen evolution reaction (HER) have been synthesized in a Zr-based metal–organic framework, UiO-66, by a new two-step chemical vapor deposition (CVD) method. The first CVD process was performed to construct the arenetricarbonyl Mo complex on the phenylene moiety of the UiO-66 framework by using Mo(CO)₆ as a precursor. Subsequently, the Mo complex was converted to MoS₂ by the second CVD process with dimethyl sulfide (CH₃S₂CH₃). The successful formation of the Mo complex and MoS₂ in UiO-66 was confirmed by using FT-IR and Raman spectroscopy, respectively. In addition, XRD and N₂ adsorption–desorption measurements revealed the preservation of the UiO-66 framework after the two-step CVD method. The thus-synthesized MoS₂-immobilized UiO-66 exhibited a higher activity for electrochemical HER than bulk MoS₂. Electrochemical impedance spectroscopy suggested that a low charge transfer resistance at the electrode interface for MoS₂ particles grown in the cavity of UiO-66 was responsible for the high electrochemical HER activity.

中文翻译：

利用化学气相沉积制备用于电化学析氢反应的金属-有机骨架负载的 MoS2 催化剂的合成路线

用于电化学析氢反应 (HER) 的MoS ₂催化剂已通过新的两步化学气相沉积 (CVD) 方法在 Zr 基金属有机骨架 UiO-66 中合成。通过使用Mo(CO) ₆作为前体，进行第一次CVD工艺以在UiO-66骨架的亚苯基部分上构建芳烃三羰基Mo配合物。随后，使用二甲硫醚 (CH ₃ S ₂ CH ₃ )通过第二次 CVD 工艺将 Mo 络合物转化为 MoS ₂。分别使用FT-IR和拉曼光谱证实了在UiO-66中成功形成Mo配合物和MoS ₂。此外，XRD 和 N ₂吸附-解吸测量表明，在两步 CVD 方法后 UiO-66 骨架得以保留。由此合成的MoS ₂固定的UiO-66 表现出比块体MoS ₂更高的电化学HER活性。电化学阻抗谱表明，在 UiO-66 腔中生长的MoS ₂颗粒的电极界面处的低电荷转移电阻是高电化学 HER 活性的原因。

更新日期：2022-01-06

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