Hierarchical Assembly of RuO2/MoOx/CoNi-LDH Nanocomposite for Enhanced Performance in Acidic Overall Water Splitting

Published: 16 May 2025| Version 1 | DOI: 10.17632/xg5cn5js8t.1
Contributors:
Amir Said, Binbin Qian, Ruiqian Zhang, Chunlei Yang, Ke Xu, Kunfeng Chen, Dongfeng Xue

Description

Title: Processed Data for “Hierarchical Assembly of RuO2/MoOx/CoNi-LDH Nanocomposite for Enhanced Performance in Acidic Overall Water Splitting” Authors: Amir Said, Binbin Qian, Ruiqian Zhang, Chunlei Yang, Ke Xu, Kunfeng Chen, and Dongfeng Xue Email: said@siat.ac.cn/amirsaidchem@gmail.com Description: This dataset contains the processed data used to generate the figures in the manuscript titled “Hierarchical Assembly of RuO2/MoOx/CoNi-LDH Nanocomposite for Enhanced Performance in Acidic Overall Water Splitting.” Each Excel file corresponds to one figure from the manuscript and includes all data related to its sub-figures (e.g., a, b, c, etc.). File Structure: Figure 1. Structure characterization data (includes subfigures 1e and 1j). Content: (e) Particle diameter distribution and (j) STEM-EDX line scan. Figure 2. Structure characterization data (includes subfigures 2a, 2b, ...2i and S6) Content: (a) XRD, (b) Raman, (c) BET (pore-size volume), XPS (d) Survey, (e) Ru3d/3p, (f) Mo3d, (g) Co2p, (h) Ni2p, and (i) O1s. Figure 3. OER data (includes subfigures 3a, 3b, ...3i and S8) Content: LSV OER, (b) Comparison of overpotential, (c) Tafel slopes, (d) Overpotential and Tafel slope comparison, (e) EIS, (f) ECSA, (g) Mass activity and TOF comparison, (h) Chronopotentiometry, and (i) Chronoamperometry (LSV before and after CV). Figure 4. HER data (includes subfigures 4a, 4b, ...4i and S11) Content: LSV HER, (b) Comparison of overpotential, (c) Tafel slopes, (d) Overpotential and Tafel slope comparison, (e) EIS, (f) ECSA, (g) Mass activity and TOF comparison, (h) Chronopotentiometry, and (i) Chronoamperometry (LSV before and after CV). Figure 5. OWS (includes subfigures 5b, 5c, 5d, and 5e) Content: (b) LSV OWS, (c) Chronopotentiometry, and (d) Chronoamperometry (LSV before and after CV), and (e) Overpotential comparison. Figure 6. Stability characterization data (includes subfigures 6b, 6c, ... 6f, S13, and S14). Content: XPS (b) Survey, (c) Ru3d/3p, (d) Mo3d, (e) Co2p, (f) Ni2p, and (g) O1s. A separate worksheet for each subfigure, or clearly labeled columns identifying which data belongs to each subfigure. Usage: These datasets can be used to reproduce the figures in the article. Each data point has been pre-processed and formatted for plotting. Units and labels are consistent with those reported in the manuscript. Notes: Raw data is not included in this repository. Please contact the author for additional data requests. Any script or software used to generate the plots is available upon request.

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1. Synthesis of CoNi-LDH: The CoNi-LDH was synthesized via a coprecipitation method by dissolving 130 mg (1 mmol) of CoCl2∙6H2O and 119 mg (0.5 mmol) of NiCl2∙6H2O in 50 mL of deionized water in a 100 mL round-bottom flask, then adding 600 mg (10 mmol) of EG. The resulting solution was kept for stirring for 2 h at 60 °C, cooled to room temperature, and a 0.5 M solution of Na2CO3 was added dropwise until the precipitate was formed (9 pH). The resulting suspension solution was aged at room temperature for 12 h. The obtained residue was collected by centrifugation, and dried in an oven at 60 °C overnight. 2. Synthesis of MoOx/CoNi-LDH: The MoOx/CoNi-LDH was synthesized via a hydrothermal method by dissolving 206 mg (1 mmol) of Na2MoO4, 240 mg (4 mmol) of urea, and 220 mg (6 mmol) of NH4F in 30 mL of deionized water and stirred for 2 h at room temperature. Then, 100 mg of the as-synthesized CoNi-LDH powder was added to the reaction mixture and stirred for 5 h at 60 °C. The resulting solution was transferred to a Teflon-lined stainless-steel autoclave and heated in an oven at 180 °C for 12 h. The obtained residue was collected by centrifugation, washed and dried in an oven at 60 °C overnight. 3. Synthesis of RuO2/MoOx/CoNi-LDH: The RuO2/MoOx/CoNi-LDH nanocomposite was synthesized by dissolving 100 mg of the MoOx/CoNi-LDH powder in 25 mL of deionized water and stirred for 30 min, then added a total 5 mL solution of RuCl3·xH2O (10 mg, 0.05 mmol) in deionized water and stirred for 5 h at 60 °C. The resulting solution was transferred to a Teflon-lined stainless-steel autoclave and heated in an oven at 180 °C for 12 h. The final residue was collected by centrifugation, washed three times and dried in an oven at 60 °C overnight. 4. Electrochemical Measurements: To prepare the working electrode, a specific amount of catalyst (5 mg) was dispersed in a 950 µL mixed solvent of H2O and EtOH (1:1, v/v) along with 50 µL of Nafion (5 wt.%). The mixture was sonicated for 30 min to obtain a colloidal suspension, and then 50 µL of the resulting ink (0.25 mg catalyst) was dispersed on the CP (1 x 1 cm) and allowed to air dry. A standard three-electrode system was employed measurement, as-prepared working electrode, an Ag/AgCl (KCl-saturated) as a reference electrode, and a Pt-wire as the counter electrode in 0.5 M H2SO4 electrolyte. All the potentials were converted to the reversible hydrogen electrode (RHE): E(RHE) = E(Ag/AgCl) + 0.059pH + 0.197. 6. The data analysis in the paper was analyzed using the following software tools: Electrochemical data were collected using CHI 660e electrochemical workstation. ZView4 was used for fitting EIS data based on equivalent circuit models. TEM data were analyzed using Digital Microgram. XPS data were analyzed using Avantage software XRD data were analyzed using MDI Jade9 software Electrochemical data were analyzed using OriginPro 2021 software

Institutions

  • Shandong University
  • Shenzhen Institutes of Advanced Technology Chinese Academy of Sciences

Categories

Materials Science, Electrocatalysis, Nanomaterials, Water Splitting, Hydrogen Evolution, Oxygen Evolution

Funders

  • National Natural Science Foundation of China
    China
    Grant ID: 52220105010, 52203343, and M-0755
  • Guangdong Basic and Applied Basic Research Foundation
    Grant ID: 2023A1515010052
  • Key Technologies R&D Program of Guangdong Province
    Grant ID: 2024B0101070003
  • Shenzhen Science and Technology Program
    Grant ID: RCBS20210609104609043, RCBS20221008093303001, and SGDX20230116092051001

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