Thirty-second Joule-heating synthesis of Cu-intercalated Mo₆S₈ Chevrel phases with pH-symmetric hydrogen evolution behavior.
- 1Superconducting Materials Research Center, Northwest Institute for Non-ferrous Metal Research Xi'an 710016 China [email protected] [email protected].
- 2School of Materials Science and Engineering, Northeastern University Shenyang 110004 China.
- 3School of Metallurgy Engineering, Xi'an International Science and Technology Cooperation Base for Manufacturing of Special Powder and Powder Metallurgy, Xi'an University of Architecture and Technology Xi'an 710055 China [email protected] [email protected].
Abstract
Chevrel-phase compounds are structurally robust transition-metal chalcogenides, and their tunable ion-intercalation chemistry makes them of considerable interest for electrochemical applications. However, the conventional synthesis of high-purity Chevrel phases generally relies on prolonged high-temperature sintering, which is unfavorable for rapid materials screening and compositional regulation. Herein, we propose a Joule-heating strategy that enables the rapid synthesis of Cu-intercalated Mo₆S₈ Chevrel phases with a holding time of 30 s at 1500 °C. Among the prepared Cu x Mo₆S₈ samples, Cu2.76Mo₆S₈ exhibits a high phase purity of 99.6% and a relatively uniform Cu distribution within the examined particles. Hydrogen evolution reaction (HER) measurements show that Cu2.76Mo₆S₈ displays a nearly pH-symmetric electrocatalytic response, requiring overpotentials of 403 and 400 mV to reach a current density of 10 mA cm⁻² in 0.5 M H₂SO₄ and 1.0 M KOH, respectively. The corresponding Tafel slopes are also comparable in acidic and alkaline electrolytes, indicating relatively balanced HER kinetics under different pH conditions. Further electrochemical cycling tests reveal electrolyte-dependent structural reconstruction: enhanced HER activity in acidic media is accompanied by structural changes consistent with partial Cu deintercalation, whereas moderate catalytic degradation in alkaline media is accompanied by more complex evolution of Cu species. XRD and XPS characterizations indicate that the Mo₆S₈ cluster framework is largely retained after cycling, while the Cu species undergo electrolyte-dependent evolution. This work provides an effective route for the rapid preparation of high-purity Chevrel phases and demonstrates that Cu-intercalated Mo₆S₈ can serve as a model system for investigating pH-dependent HER behavior and electrochemical reconstruction mechanisms.
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BibTeX
@article{jiang2026thirtysecond,
title = {{Thirty-second Joule-heating synthesis of Cu-intercalated Mo₆S₈ Chevrel phases with pH-symmetric hydrogen evolution behavior.}},
author = {Zongchen Jiang and Wenqi Li and Zhenyu Chen and Shengnan Zhang and Botao Shao and Fan Yang and Ping Hu and Chengshan Li and Pingxiang Zhang},
journal = {RSC advances},
year = {2026},
month = oct,
doi = {10.1039/d6ra05873f},
url = {https://europepmc.org/article/MED/42899087},
note = {CC BY},
}
RIS
TY - JOUR
TI - Thirty-second Joule-heating synthesis of Cu-intercalated Mo₆S₈ Chevrel phases with pH-symmetric hydrogen evolution behavior.
AU - Zongchen Jiang
AU - Wenqi Li
AU - Zhenyu Chen
AU - Shengnan Zhang
AU - Botao Shao
AU - Fan Yang
AU - Ping Hu
AU - Chengshan Li
AU - Pingxiang Zhang
PY - 2026
DA - 2026/10/19
JO - RSC advances
DO - 10.1039/d6ra05873f
UR - https://europepmc.org/article/MED/42899087
AB - Chevrel-phase compounds are structurally robust transition-metal chalcogenides, and their tunable ion-intercalation chemistry makes them of considerable interest for electrochemical applications. However, the conventional synthesis of high-purity Chevrel phases generally relies on prolonged high-temperature sintering, which is unfavorable for rapid materials screening and compositional regulation. Herein, we propose a Joule-heating strategy that enables the rapid synthesis of Cu-intercalated Mo₆S₈ Chevrel phases with a holding time of 30 s at 1500 °C. Among the prepared Cu x Mo₆S₈ samples, Cu2.76Mo₆S₈ exhibits a high phase purity of 99.6% and a relatively uniform Cu distribution within the examined particles. Hydrogen evolution reaction (HER) measurements show that Cu2.76Mo₆S₈ displays a nearly pH-symmetric electrocatalytic response, requiring overpotentials of 403 and 400 mV to reach a current density of 10 mA cm⁻² in 0.5 M H₂SO₄ and 1.0 M KOH, respectively. The corresponding Tafel slopes are also comparable in acidic and alkaline electrolytes, indicating relatively balanced HER kinetics under different pH conditions. Further electrochemical cycling tests reveal electrolyte-dependent structural reconstruction: enhanced HER activity in acidic media is accompanied by structural changes consistent with partial Cu deintercalation, whereas moderate catalytic degradation in alkaline media is accompanied by more complex evolution of Cu species. XRD and XPS characterizations indicate that the Mo₆S₈ cluster framework is largely retained after cycling, while the Cu species undergo electrolyte-dependent evolution. This work provides an effective route for the rapid preparation of high-purity Chevrel phases and demonstrates that Cu-intercalated Mo₆S₈ can serve as a model system for investigating pH-dependent HER behavior and electrochemical reconstruction mechanisms.
SN - 2046-2069
ER -