Synthesis evidence

Copper-based conductive metal organic framework in-situ grown on copper foam as a bifunctional electrocatalyst

Zhang C., Chen Z., Lian Y. et al. · Wuli Huaxue Xuebao/ Acta Physico - Chimica Sinica · 2019 · 1404-1411

4 structured synthesis routes

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

Complete recipeSource: Main

Route 1: Other

1406 · 2.2.2 · Fig. 1, Fig. S1

Metal precursorsCu(OH)2/CF
Linker precursorsHITP.6HCl, 20 mg (0.038 mmol)
Solvents10 mL deionised water; acetone and distilled water wash
Atmospheresealed vessel; atmosphere not otherwise specified
Temperature65 degC reaction; 60 degC vacuum drying
Time10 min sonication of linker solution; 48 h sealed heating; 12 h vacuum drying
Substrate orientationCu(OH)2/CF immersed in HITP solution in a beaker
Oxidant / reductantin-situ conversion of Cu(OH)2 nanowires to Cu3HITP2
Work-upwashed with acetone and distilled water
Activationvacuum dried at 60 degC for 12 h
Scalability contextLoading measured by ultrasonic peeling as 7.2 mg cm-2 on copper foam.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCu(OH)2/CFone prepared electrode1406 · 2.2.2 · Fig. 1, Fig. S1
LinkerHITP.6HCl20 mg (0.038 mmol)1406 · 2.2.2 · Fig. 1, Fig. S1
Solventdeionised water10 mL1406 · 2.2.2 · Fig. 1, Fig. S1
Solventacetonewash1406 · 2.2.2 · Fig. 1, Fig. S1
Solventdistilled waterwash1406 · 2.2.2 · Fig. 1, Fig. S1
Partial recipeSource: Main

Route 2: Drop Cast

1409 · 3.3 · Fig. 6c

Metal precursorsCu3HITP2 removed from Cu3HITP2/CF
Linker precursorsalready incorporated HITP
Solvents500 uL ethanol; 500 uL deionised water
Additives100 uL Nafion, 5 wt%
Atmospherenot specified
Substrate orientationuniformly dropped on glassy carbon electrode surface
Work-upultrasonic removal from copper foam and dispersion
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
OtherCu3HITP2 removed from copper foamNot specified1409 · 3.3 · Fig. 6c
Solventethanol500 uL1409 · 3.3 · Fig. 6c
Solventdeionised water500 uL1409 · 3.3 · Fig. 6c
AdditiveNafion100 uL · 5 wt%1409 · 3.3 · Fig. 6c
Complete recipeSource: Main

Route 3: Electrochemical

1406 · 2.2.1 · Fig. 1

Metal precursorscommercial copper foam; copper foil counter/electrode fixture
Solventsdilute HCl wash; deionised water; 3 mol L-1 KOH electrolyte
AdditivesKOH electrolyte
Atmospherenot specified
Temperature60 degC drying
Time1 h acid immersion; 15 min electrolysis; 12 h vacuum drying
Substrate orientation1 cm x 1 cm copper foam fixed with copper foil as cathode/anode pair
Oxidant / reductant40 mA constant-current electrolysis
Work-upwashed with distilled water
Activationvacuum dried at 60 degC for 12 h
Scalability contextElectrode-area recipe reported for 1 cm x 1 cm copper foam.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Metal Sourcecommercial copper foam1 cm x 1 cm; thickness 1.5 mm1406 · 2.2.1 · Fig. 1
Metal Sourcecopper foilNot specified1406 · 2.2.1 · Fig. 1
ElectrolyteKOH3 mol L-11406 · 2.2.1 · Fig. 1
Aciddilute hydrochloric acidNot specified1406 · 2.2.1 · Fig. 1
Solventdeionised/distilled waterNot specified1406 · 2.2.1 · Fig. 1
Complete recipeSource: Main

Route 4: Drop Cast

1406 · 2.3

Metal precursorsRuO2 powder, 7.2 mg
Solvents500 uL ethanol; 500 uL deionised water
Additives100 uL Nafion, 5 wt%
Atmosphereair, not otherwise specified
Temperature45 degC drying
Time30 min sonication
Substrate orientation20 uL slurry drop-cast on 1 cm x 1 cm copper foam
Work-upsonicated dispersion; dried after drop-casting
Activationdried at 45 degC
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceRuO2 powder7.2 mg1406 · 2.3
Solventethanol500 uL1406 · 2.3
Solventdeionised water500 uL1406 · 2.3
AdditiveNafion100 uL · 5 wt%1406 · 2.3