cMOF Evidence Base

Synthesis evidence

Facile synthesis of Ni-, Co-, Cu-metal organic frameworks electrocatalyst boosting for hydrogen evolution reaction

Zhang M., Hu D., Xu Z. et al. · Journal of Materials Science and Technology · 2021 · 172-179

6 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

main p.3, article p.174 · Electrocatalytic hydrogen evolution reaction

Metal precursorsCo-BTC powder
SolventsIsopropyl alcohol, 20 mL
AtmosphereNot specified; oven treatment.
Temperature120; then 60
Time12; then 6
Substrate orientationCarbon fibre paper, 1 cm x 1 cm.
Work-upPrepared Co-BTC ink by ultrasonication for 30 min; treated Co-BTC ink and CFP together in 100 mL Teflon-lined vessel.
ActivationDried at 60 C for 6 h.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
OtherCo-BTC20 mgmain p.3, article p.174 · Electrocatalytic hydrogen evolution reaction
Solventisopropyl alcohol20 mLmain p.3, article p.174 · Electrocatalytic hydrogen evolution reaction
Othercarbon fiber paper1 cm x 1 cmmain p.3, article p.174 · Electrocatalytic hydrogen evolution reaction
Complete recipeSource: Main

Route 2: Other

main p.3, article p.174 · Electrocatalytic hydrogen evolution reaction

Metal precursorsCu-BTC powder
SolventsIsopropyl alcohol, 20 mL
AtmosphereNot specified; oven treatment.
Temperature120; then 60
Time12; then 6
Substrate orientationCarbon fibre paper, 1 cm x 1 cm.
Work-upPrepared Cu-BTC ink by ultrasonication for 30 min; treated Cu-BTC ink and CFP together in 100 mL Teflon-lined vessel.
ActivationDried at 60 C for 6 h.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
OtherCu-BTC20 mgmain p.3, article p.174 · Electrocatalytic hydrogen evolution reaction
Solventisopropyl alcohol20 mLmain p.3, article p.174 · Electrocatalytic hydrogen evolution reaction
Othercarbon fiber paper1 cm x 1 cmmain p.3, article p.174 · Electrocatalytic hydrogen evolution reaction
Complete recipeSource: Main

Route 3: Other

main p.3, article p.174 · Electrocatalytic hydrogen evolution reaction

Metal precursorsNi-BTC powder
SolventsIsopropyl alcohol, 20 mL
AtmosphereNot specified; oven treatment.
Temperature120; then 60
Time12; then 6
Substrate orientationCarbon fibre paper, 1 cm x 1 cm.
Work-upPrepared Ni-BTC ink by ultrasonication for 30 min; treated Ni-BTC ink and CFP together in 100 mL Teflon-lined vessel.
ActivationDried at 60 C for 6 h.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
OtherNi-BTC20 mgmain p.3, article p.174 · Electrocatalytic hydrogen evolution reaction
Solventisopropyl alcohol20 mLmain p.3, article p.174 · Electrocatalytic hydrogen evolution reaction
Othercarbon fiber paper1 cm x 1 cmmain p.3, article p.174 · Electrocatalytic hydrogen evolution reaction
Complete recipeSource: Both

Route 4: Solvothermal

SI text p.1 · Preparation and characterization of MOFs catalysts

Metal precursorsCobalt(II) nitrate hexahydrate, Co(NO3)2.6H2O, 15.4 mmol, 99.99 %
Linker precursorsH3BTC, benzene-1,3,5-tricarboxylic acid, 10.3 mmol
SolventsDMF 90 mL and ethanol 90 mL
AtmosphereNot specified; sealed 250 mL Teflon-lined stainless autoclave.
Temperature110
Time24
Work-upCooled to room temperature over about 6 h; crystals washed several times with methanol.
ActivationVacuum dried at 60 C.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCo(NO3)2.6H2O15.4 mmolSI text p.1 · Preparation and characterization of MOFs catalysts
LinkerH3BTC10.3 mmolSI text p.1 · Preparation and characterization of MOFs catalysts
SolventDMF90 mLSI text p.1 · Preparation and characterization of MOFs catalysts
Solventethanol90 mLSI text p.1 · Preparation and characterization of MOFs catalysts
Solventmethanolseveral washesSI text p.1 · Preparation and characterization of MOFs catalysts
Complete recipeSource: Both

Route 5: Solvothermal

SI text p.1 · Preparation and characterization of MOFs catalysts

Metal precursorsCopper(II) nitrate hydrate, Cu(NO3)2.H2O, 1.0 g, 99.99 %
Linker precursorsH3BTC, benzene-1,3,5-tricarboxylic acid, 0.50 g
Solvents8.3 mL H2O for metal precursor; 16.6 mL DMF/ethanol mixture, 1:1 v/v, for H3BTC
AtmosphereNot specified; sealed vessel/oven treatment.
Temperature85
Time20
Work-upCooled to ambient temperature; blue crystals filtered and washed with water/ethanol (1:1).
ActivationDried at 60 C for 12 h, then vacuum dried for 5 h to remove trace DMF.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCu(NO3)2.H2O1.0 gSI text p.1 · Preparation and characterization of MOFs catalysts
LinkerH3BTC0.50 gSI text p.1 · Preparation and characterization of MOFs catalysts
SolventH2O8.3 mLSI text p.1 · Preparation and characterization of MOFs catalysts
SolventDMF8.3 mL in 16.6 mL DMF/ethanol 1:1 mixtureSI text p.1 · Preparation and characterization of MOFs catalysts
Solventethanol8.3 mL in 16.6 mL DMF/ethanol 1:1 mixtureSI text p.1 · Preparation and characterization of MOFs catalysts
Complete recipeSource: Both

Route 6: Solvothermal

SI text p.1 · Preparation and characterization of MOFs catalysts

Metal precursorsNickel nitrate, Ni(NO3)2.6H2O, 3.8 mmol
Linker precursorsBenzene-1,3,5-tricarboxylic acid, C6H3(COOH)3, 2.1 mmol
SolventsMethanol, 60 mL
AtmosphereNot specified; sealed 80 mL Teflon-lined stainless steel autoclave.
Temperature150
Time24
Work-upNaturally cooled to room temperature; precipitates collected by centrifugation and washed with absolute methanol several times.
ActivationVacuum dried at 60 C for 12 h.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceNi(NO3)2.6H2O3.8 mmolSI text p.1 · Preparation and characterization of MOFs catalysts
LinkerC6H3(COOH)32.1 mmolSI text p.1 · Preparation and characterization of MOFs catalysts
Solventmethanol60 mLSI text p.1 · Preparation and characterization of MOFs catalysts
Solventabsolute methanolseveral washesSI text p.1 · Preparation and characterization of MOFs catalysts