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Electrodeposition of MoSx Hydrogen Evolution Catalysts from Sulfur-Rich Precursors
ACS Applied Materials & Interfaces ( IF 8.3 ) Pub Date : 2019-08-15 00:00:00 , DOI: 10.1021/acsami.9b07277 Oluwaniyi Mabayoje , Yang Liu 1 , Michael Wang , Ahmed Shoola , Amani M. Ebrahim 2 , Anatoly I. Frenkel 2, 3 , C. Buddie Mullins
ACS Applied Materials & Interfaces ( IF 8.3 ) Pub Date : 2019-08-15 00:00:00 , DOI: 10.1021/acsami.9b07277 Oluwaniyi Mabayoje , Yang Liu 1 , Michael Wang , Ahmed Shoola , Amani M. Ebrahim 2 , Anatoly I. Frenkel 2, 3 , C. Buddie Mullins
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Amorphous molybdenum sulfides (a-MoSx) are known to be active electrocatalysts for the hydrogen evolution reaction (HER), but the role stoichiometry of the sulfur atoms plays in the HER activity remains unclear. In this work, we deposited thin films of a-MoSx from two thiomolybdate deposition baths with different sulfur ratios (MoS42– and Mo2S122–) and showed that the sulfur stoichiometry, as determined by X-ray photoelectron spectroscopy, is controlled by the precursor of choice and the electrochemical method used to deposit the thin films. Using the Mo2S122– precursor allows access to a MoS6 thin film, with a higher S/Mo ratio compared with that of any previously reported electrodeposited films. We also examined the effect of electrochemistry on the resulting S/Mo ratio in the as-prepared a-MoSx thin films. Samples with S/Mo ratios ranging from 2 to 6 were electrodeposited on glassy carbon (GC) substrates by using anodic, cathodic, or cyclic voltammetry deposition. The a-MoSx thin films deposited on GC substrates were tested as HER catalysts in acidic electrolytes. The overpotentials needed to drive current densities of 10 mA/cm2 ranged from 160 mV for MoS6 samples to 216 mV for MoS2 samples, signifying the important role sulfur content plays in HER activity of the prepared films. Furthermore, we characterized the deactivation of the a-MoSx films and found that the sulfur content is gradually depleted over time, leading to a slow deactivation of the a-MoSx thin-film catalysts. We showed a facile procedure that affords a-MoSx films with high sulfur content by using S-rich precursors and highlighted the role of sulfur in the prepared films for HER.
中文翻译：
富硫前驱体对MoS x析氢催化剂的电沉积
非晶态硫化钼（a-MoS x）是氢释放反应（HER）的活性电催化剂，但硫原子的化学计量在HER活性中的作用尚不清楚。在这项工作中，我们从两个硫比率不同（MoS 4 2–和Mo 2 S 12 2–）的硫代钼酸盐沉积浴中沉积了a-MoS x薄膜，并显示了由X射线光电子能谱测定的硫化学计量由选择的前体和用于沉积薄膜的电化学方法控制。使用Mo 2 S 12 2–前驱体可以访问MoS 6薄膜，具有比以前报道的任何电沉积薄膜更高的S / Mo比。我们还检查了电化学对制备的a-MoS x薄膜中所得S / Mo比的影响。通过使用阳极，阴极或循环伏安法沉积，将S / Mo比为2至6的样品电沉积在玻璃碳（GC）基底上。测试了沉积在GC基材上的a-MoS x薄膜作为酸性电解质中的HER催化剂。驱动10 mA / cm 2的电流密度所需的过电位范围从MoS 6样品的160 mV到MoS 2的216 mV样品，表明硫含量在制备的薄膜的HER活性中起着重要作用。此外，我们表征了a-MoS x薄膜的失活，发现硫含量随着时间的流逝逐渐减少，从而导致a-MoS x薄膜催化剂的缓慢失活。我们展示了一种简单的方法，该方法可通过使用富含S的前体来提供具有高硫含量的a-MoS x膜，并强调了硫在HER制备膜中的作用。
更新日期：2019-08-15
中文翻译：
富硫前驱体对MoS x析氢催化剂的电沉积
非晶态硫化钼（a-MoS x）是氢释放反应（HER）的活性电催化剂，但硫原子的化学计量在HER活性中的作用尚不清楚。在这项工作中，我们从两个硫比率不同（MoS 4 2–和Mo 2 S 12 2–）的硫代钼酸盐沉积浴中沉积了a-MoS x薄膜，并显示了由X射线光电子能谱测定的硫化学计量由选择的前体和用于沉积薄膜的电化学方法控制。使用Mo 2 S 12 2–前驱体可以访问MoS 6薄膜，具有比以前报道的任何电沉积薄膜更高的S / Mo比。我们还检查了电化学对制备的a-MoS x薄膜中所得S / Mo比的影响。通过使用阳极，阴极或循环伏安法沉积，将S / Mo比为2至6的样品电沉积在玻璃碳（GC）基底上。测试了沉积在GC基材上的a-MoS x薄膜作为酸性电解质中的HER催化剂。驱动10 mA / cm 2的电流密度所需的过电位范围从MoS 6样品的160 mV到MoS 2的216 mV样品，表明硫含量在制备的薄膜的HER活性中起着重要作用。此外，我们表征了a-MoS x薄膜的失活，发现硫含量随着时间的流逝逐渐减少，从而导致a-MoS x薄膜催化剂的缓慢失活。我们展示了一种简单的方法，该方法可通过使用富含S的前体来提供具有高硫含量的a-MoS x膜，并强调了硫在HER制备膜中的作用。
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