Synthesis evidence

Structural and electronic modulation of conductive MOFs for efficient oxygen evolution reaction electrocatalysis

Li J., Liu P., Mao J. et al. · Journal of Materials Chemistry A · 2021 · 11248-11254

4 structured synthesis routes

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

Partial recipeSource: Main

Route 1: Solvothermal

5 · Synthesis of NiPc-NiFe0.05, NiPc-NiFe0.20, and NiPc-Fe

Metal precursorsnickel acetate tetrahydrate (23.64 mg); anhydrous ferrous acetate (0.87 mg)
Linker precursorsNiPc (28 mg, 0.04 mmol); NiPc itself was synthesised according to prior work, not detailed here
SolventsWater (2 mL for metal acetate solution; 6 mL in reaction mixture) and DMF (5 mL)
AdditivesNH3.H2O (~22 wt%, 2.2 mL)
Atmospherenot specified
Temperature120
Time48
Oxidant / reductantnone explicitly specified
Work-upFiltered, washed with DMF and acetone, then dried at 25 C in a vacuum oven.
ActivationVacuum drying at 25 C; no separate activation reported.
Scalability contextSmall-batch milligram-scale autoclave synthesis; no scale-up reported.
Show 6 structured reagent records
RoleReagentAmount / concentrationSource
Metal Sourcenickel acetate tetrahydrate23.64 mg5 · Synthesis of NiPc-NiFe0.05, NiPc-NiFe0.20, and NiPc-Fe
Metal Sourceanhydrous ferrous acetate0.87 mg5 · Synthesis of NiPc-NiFe0.05, NiPc-NiFe0.20, and NiPc-Fe
LinkerNiPc = (2,3,9,10,16,17,23,24-octahydroxyphthalocyaninato) nickel(II)28 mg (0.04 mmol)5 · Synthesis of NiPc-NiFe0.05, NiPc-NiFe0.20, and NiPc-Fe
BaseNH3.H2O2.2 mL · ~22 wt%5 · Synthesis of NiPc-NiFe0.05, NiPc-NiFe0.20, and NiPc-Fe
SolventN,N-dimethylformamide (DMF)5 mL5 · Synthesis of NiPc-NiFe0.05, NiPc-NiFe0.20, and NiPc-Fe
SolventH2O6 mL plus 2 mL in metal acetate solution5 · Synthesis of NiPc-NiFe0.05, NiPc-NiFe0.20, and NiPc-Fe
Partial recipeSource: Main

Route 2: Solvothermal

5 · Synthesis of NiPc-NiFe0.09

Metal precursorsnickel acetate tetrahydrate (22.62 mg); anhydrous ferrous acetate (1.58 mg)
Linker precursorsNiPc (28 mg, 0.04 mmol); NiPc itself was synthesised according to prior work, not detailed here
SolventsWater (2 mL for metal acetate solution; 6 mL in reaction mixture) and DMF (5 mL)
AdditivesNH3.H2O (~22 wt%, 2.2 mL)
Atmospherenot specified
Temperature120
Time48
Oxidant / reductantnone explicitly specified
Work-upFiltered, washed with DMF and acetone, then dried at 25 C in a vacuum oven.
ActivationVacuum drying at 25 C; no separate activation reported.
Scalability contextSmall-batch milligram-scale autoclave synthesis; no scale-up reported.
Show 6 structured reagent records
RoleReagentAmount / concentrationSource
Metal Sourcenickel acetate tetrahydrate22.62 mg5 · Synthesis of NiPc-NiFe0.09
Metal Sourceanhydrous ferrous acetate1.58 mg5 · Synthesis of NiPc-NiFe0.09
LinkerNiPc = (2,3,9,10,16,17,23,24-octahydroxyphthalocyaninato) nickel(II)28 mg (0.04 mmol)5 · Synthesis of NiPc-NiFe0.09
BaseNH3.H2O2.2 mL · ~22 wt%5 · Synthesis of NiPc-NiFe0.09
SolventN,N-dimethylformamide (DMF)5 mL5 · Synthesis of NiPc-NiFe0.09
SolventH2O6 mL plus 2 mL in metal acetate solution5 · Synthesis of NiPc-NiFe0.09
Partial recipeSource: Main

Route 3: Solvothermal

5 · Synthesis of NiPc-NiFe0.05, NiPc-NiFe0.20, and NiPc-Fe

Metal precursorsnickel acetate tetrahydrate (19.91 mg); anhydrous ferrous acetate (3.48 mg)
Linker precursorsNiPc (28 mg, 0.04 mmol); NiPc itself was synthesised according to prior work, not detailed here
SolventsWater (2 mL for metal acetate solution; 6 mL in reaction mixture) and DMF (5 mL)
AdditivesNH3.H2O (~22 wt%, 2.2 mL)
Atmospherenot specified
Temperature120
Time48
Oxidant / reductantnone explicitly specified
Work-upFiltered, washed with DMF and acetone, then dried at 25 C in a vacuum oven.
ActivationVacuum drying at 25 C; no separate activation reported.
Scalability contextSmall-batch milligram-scale autoclave synthesis; no scale-up reported.
Show 6 structured reagent records
RoleReagentAmount / concentrationSource
Metal Sourcenickel acetate tetrahydrate19.91 mg5 · Synthesis of NiPc-NiFe0.05, NiPc-NiFe0.20, and NiPc-Fe
Metal Sourceanhydrous ferrous acetate3.48 mg5 · Synthesis of NiPc-NiFe0.05, NiPc-NiFe0.20, and NiPc-Fe
LinkerNiPc = (2,3,9,10,16,17,23,24-octahydroxyphthalocyaninato) nickel(II)28 mg (0.04 mmol)5 · Synthesis of NiPc-NiFe0.05, NiPc-NiFe0.20, and NiPc-Fe
BaseNH3.H2O2.2 mL · ~22 wt%5 · Synthesis of NiPc-NiFe0.05, NiPc-NiFe0.20, and NiPc-Fe
SolventN,N-dimethylformamide (DMF)5 mL5 · Synthesis of NiPc-NiFe0.05, NiPc-NiFe0.20, and NiPc-Fe
SolventH2O6 mL plus 2 mL in metal acetate solution5 · Synthesis of NiPc-NiFe0.05, NiPc-NiFe0.20, and NiPc-Fe
Partial recipeSource: Main

Route 4: Solvothermal

5 · Synthesis of NiPc-NiFe0.05, NiPc-NiFe0.20, and NiPc-Fe

Metal precursorsnickel acetate tetrahydrate (0 mg); anhydrous ferrous acetate (17.42 mg)
Linker precursorsNiPc (28 mg, 0.04 mmol); NiPc itself was synthesised according to prior work, not detailed here
SolventsWater (2 mL for metal acetate solution; 6 mL in reaction mixture) and DMF (5 mL)
AdditivesNH3.H2O (~22 wt%, 2.2 mL)
Atmospherenot specified
Temperature120
Time48
Oxidant / reductantnone explicitly specified
Work-upFiltered, washed with DMF and acetone, then dried at 25 C in a vacuum oven.
ActivationVacuum drying at 25 C; no separate activation reported.
Scalability contextSmall-batch milligram-scale autoclave synthesis; no scale-up reported.
Show 6 structured reagent records
RoleReagentAmount / concentrationSource
Metal Sourcenickel acetate tetrahydrate0 mg5 · Synthesis of NiPc-NiFe0.05, NiPc-NiFe0.20, and NiPc-Fe
Metal Sourceanhydrous ferrous acetate17.42 mg5 · Synthesis of NiPc-NiFe0.05, NiPc-NiFe0.20, and NiPc-Fe
LinkerNiPc = (2,3,9,10,16,17,23,24-octahydroxyphthalocyaninato) nickel(II)28 mg (0.04 mmol)5 · Synthesis of NiPc-NiFe0.05, NiPc-NiFe0.20, and NiPc-Fe
BaseNH3.H2O2.2 mL · ~22 wt%5 · Synthesis of NiPc-NiFe0.05, NiPc-NiFe0.20, and NiPc-Fe
SolventN,N-dimethylformamide (DMF)5 mL5 · Synthesis of NiPc-NiFe0.05, NiPc-NiFe0.20, and NiPc-Fe
SolventH2O6 mL plus 2 mL in metal acetate solution5 · Synthesis of NiPc-NiFe0.05, NiPc-NiFe0.20, and NiPc-Fe