cMOF Evidence Base

Synthesis evidence

sp-Carbon Incorporated Conductive Metal-Organic Framework as Photocathode for Photoelectrochemical Hydrogen Generation

Lu Y., Zhong H., Li J. et al. · Angewandte Chemie - International Edition · 2022 · e202208163

4 structured synthesis routes

Completeness describes how fully the route could be reconstructed from the main article and supporting information.

Complete recipeSource: SI

Route 1: Drop Cast

3 · Electrode preparation

Solventsisopropanol (200 uL)
Atmosphereair during preparation; Ar-degassed electrolyte during PEC measurement
Temperatureroom temperature
Substrate orientationCu foam substrate; orientation not specified
Work-upCu foam washed sequentially with dilute HCl solution, water, acetone and ethanol; catalyst ink sonicated at least 30 min before drop-casting.
Scalability contextCatalyst loading about 1 mg cm-2 on exposed geometric area.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Otheras-prepared Cu3HHAE2 sample1 mg3 · Electrode preparation
Solventisopropanol200 uL3 · Electrode preparation
Aciddilute HCl solutionused to wash Cu foam · dilute3 · Electrode preparation
Complete recipeSource: Both

Route 2: Solvothermal

6 · Cu3HHAE2 synthesis

Metal precursorsCuSO4.5H2O (1.5 eq)
Linker precursorsHHAE monomer (5 mg, 1 eq)
Solvents0.5 mL DMF and 1.5 mL H2O; main text describes 3:1 (v/v) H2O/DMF
Atmospherenot specified
Temperature85
Time12
Work-upFiltered; washed with a large amount of water and acetone; dried under vacuum.
ActivationFor N2 sorption, powder treated in supercritical CO2 dryer for 4 h and activated at 90 deg C overnight; main text also says activated by heating at 90 deg C under dynamic vacuum.
Scalability contextSmall batch: 5 mg HHAE in a 20 mL glass vial; no scale-up demonstrated.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCuSO4.5H2O1.5 eq6 · Cu3HHAE2 synthesis
LinkerHHAE monomer5 mg, 1 eq6 · Cu3HHAE2 synthesis
SolventDMF0.5 mL6 · Cu3HHAE2 synthesis
SolventH2O1.5 mL6 · Cu3HHAE2 synthesis
Complete recipeSource: SI

Route 3: Drop Cast

4 · PEC HER measurement · Figure 4

Linker precursorsHHAE monomer
Solventsisopropanol (200 uL)
Atmosphereair during preparation; Ar-degassed electrolyte during PEC measurement
Temperatureroom temperature
Substrate orientationCu foam substrate; orientation not specified
Work-upCu foam washed sequentially with dilute HCl solution, water, acetone and ethanol; catalyst ink sonicated at least 30 min before drop-casting.
Scalability contextCatalyst loading about 1 mg cm-2 on exposed geometric area.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
LinkerHHAE monomer1 mg as as-prepared sample in shared electrode recipe4 · PEC HER measurement · Figure 4
Solventisopropanol200 uL4 · PEC HER measurement · Figure 4
Aciddilute HCl solutionused to wash Cu foam · dilute4 · PEC HER measurement · Figure 4
Vague recipeSource: SI

Route 4: Unknown

6 · Section S2 Synthetic procedures

Show 1 structured reagent record
RoleReagentAmount / concentrationSource
LinkerHHAE monomerNot specified6 · Section S2 Synthetic procedures