Synthesis evidence

Copper-cobalt bimetallic conductive metal–organic frameworks as bifunctional oxygen electrocatalyst in alkaline and neutral media

Zhang M.-C., Liu M.-Y., Yang M.-X. et al. · Journal of Solid State Chemistry · 2023 · 124133

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: Drop Cast

main p.2 · Experimental section - Electrochemical measurement

SolventsEthanol, 980 uL in ink
AdditivesNafion, 20 uL of 5 wt% stock
AtmosphereAmbient drying
Time1 h sonication; drying time not specified
Substrate orientationGlassy carbon electrode
Work-up10 uL uniformly dispersed ink spread on glassy carbon electrode and dried naturally.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
OtherCu3(HITP)2 powder5 mgmain p.2 · Experimental section - Electrochemical measurement
Solventethanol980 uLmain p.2 · Experimental section - Electrochemical measurement
AdditiveNafion20 uL · 5 wt% stockmain p.2 · Experimental section - Electrochemical measurement
Complete recipeSource: Both

Route 2: Other

main p.2 · Experimental section - Material synthesis

Metal precursorsCuSO4.5H2O, 35 mg (0.14 mmol)
Linker precursorsHITP.6HCl, 50 mg (0.093 mmol)
SolventsDeionized water; acetone workup solvent
AdditivesConcentrated ammonia, 500 uL
AtmosphereNot explicitly specified; aqueous synthesis described under ambient laboratory conditions for the CuCo analogue.
Time96 h post-precipitation stirring (75 mL water for 3 days, then 75 mL acetone for 1 day)
Work-upBlack precipitate formed immediately; suspension stirred in 75 mL water for three days, then 75 mL acetone for one day; collected by centrifugation.
ActivationVacuum drying
Scalability contextYield 63.7% based on HITP.6HCl.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCuSO4.5H2O35 mg (0.14 mmol)main p.2 · Experimental section - Material synthesis
LinkerHITP.6HCl50 mg (0.093 mmol)main p.2 · Experimental section - Material synthesis
Solventdeionized water10 mL for Cu salt; 15 mL aqueous linker solution; 75 mL stirring/washingmain p.2 · Experimental section - Material synthesis
Baseconcentrated ammonia500 uL · concentratedmain p.2 · Experimental section - Material synthesis
Solventacetone75 mLmain p.2 · Experimental section - Material synthesis
Complete recipeSource: Main

Route 3: Drop Cast

main p.2 · Experimental section - Electrochemical measurement

SolventsEthanol, 980 uL in ink
AdditivesNafion, 20 uL of 5 wt% stock
AtmosphereAmbient drying
Time1 h sonication; drying time not specified
Substrate orientationGlassy carbon electrode
Work-up10 uL uniformly dispersed ink spread on glassy carbon electrode and dried naturally.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
OtherCuCo-HITP powder5 mgmain p.2 · Experimental section - Electrochemical measurement
Solventethanol980 uLmain p.2 · Experimental section - Electrochemical measurement
AdditiveNafion20 uL · 5 wt% stockmain p.2 · Experimental section - Electrochemical measurement
Partial recipeSource: Both

Route 4: Other

main p.2 · Experimental section - Material synthesis

Metal precursorsEqual mole CuSO4.5H2O and CoCl2.6H2O replacing CuSO4.5H2O
Linker precursorsHITP.6HCl, same as Cu3(HITP)2 route
SolventsDeionized water; acetone workup solvent
AdditivesConcentrated ammonia
AtmosphereAmbient conditions
Time96 h post-precipitation stirring by same procedure as Cu3(HITP)2
Work-upSame as Cu3(HITP)2: black precipitate/suspension stirred in water for three days and acetone for one day, then centrifuged.
ActivationVacuum drying
Scalability contextYield 61.3% based on HITP.6HCl.
Show 6 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCuSO4.5H2Oequal mole with CoCl2.6H2O; exact mass not reportedmain p.2 · Experimental section - Material synthesis
Metal SourceCoCl2.6H2Oequal mole with CuSO4.5H2O; exact mass not reportedmain p.2 · Experimental section - Material synthesis
LinkerHITP.6HClsame synthesis procedure as Cu3(HITP)2; 50 mg (0.093 mmol) implied but not separately restatedmain p.2 · Experimental section - Material synthesis
Solventdeionized watersame synthesis procedure as Cu3(HITP)2main p.2 · Experimental section - Material synthesis
Baseconcentrated ammoniasame synthesis procedure as Cu3(HITP)2; 500 uL implied but not separately restated · concentratedmain p.2 · Experimental section - Material synthesis
Solventacetonesame synthesis procedure as Cu3(HITP)2main p.2 · Experimental section - Material synthesis