Synthesis · Fabrication of 3D Co-doped Ni-based MOF hierarchical micro-flowers as a high-performance electrode material for supercapacitors

6 structured synthesis routes

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

Partial recipeSource: Main

Route 1: Hydrothermal

2 · 2.1.2 Synthesis of Co-doped Ni-MOFs

Metal precursorsNi(NO3)2.6H2O plus Co(NO3)2.6H2O; nominal Co/Ni = 0.5%

Linker precursors1,4-benzenedicarboxylic acid (4 mmol, from Ni-MOF route)

SolventsDMF

AdditivesHCl (0.5 mL, from Ni-MOF route)

Temperature180

Time24

Work-upSame as Ni-MOF: centrifugation and rinsing with DMF and ethanol.

ActivationVacuum oven drying for 12 h at 60 deg C; BET degassing at 150 deg C for 4 h before porosity test.

Scalability context100 mL autoclave by analogy to Ni-MOF route.

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Ni(NO3)2.6H2O	from Ni-MOF route	2 · 2.1.2 Synthesis of Co-doped Ni-MOFs
Metal Source	Co(NO3)2.6H2O	Co/Ni = 0.5 mol%	2 · 2.1.2 Synthesis of Co-doped Ni-MOFs
Linker	1,4-benzenedicarboxylic acid	4 mmol	2 · 2.1.2 Synthesis of Co-doped Ni-MOFs
Solvent	DMF	as for Ni-MOF route	2 · 2.1.2 Synthesis of Co-doped Ni-MOFs
Acid	HCl	0.5 ml	2 · 2.1.2 Synthesis of Co-doped Ni-MOFs

Partial recipeSource: Main

Route 2: Other

7 · 3.3 Electrochemical measurements of Co2-Ni-MOF//AC HSC device

Work-upPositive and negative electrodes mass-balanced using q = C x m x dV.

Show 2 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	Co2-Ni-MOF positive electrode	1.76 mg	7 · 3.3 Electrochemical measurements of Co2-Ni-MOF//AC HSC device
Other	active carbon negative electrode	6.31 mg	7 · 3.3 Electrochemical measurements of Co2-Ni-MOF//AC HSC device

Partial recipeSource: Main

Route 3: Hydrothermal

2 · 2.1.2 Synthesis of Co-doped Ni-MOFs

Metal precursorsNi(NO3)2.6H2O plus Co(NO3)2.6H2O; nominal Co/Ni = 2%

Linker precursors1,4-benzenedicarboxylic acid (4 mmol, from Ni-MOF route)

SolventsDMF

AdditivesHCl (0.5 mL, from Ni-MOF route)

Temperature180

Time24

Work-upSame as Ni-MOF: centrifugation and rinsing with DMF and ethanol.

ActivationVacuum oven drying for 12 h at 60 deg C; BET degassing at 150 deg C for 4 h before porosity test.

Scalability context100 mL autoclave by analogy to Ni-MOF route.

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Ni(NO3)2.6H2O	from Ni-MOF route	2 · 2.1.2 Synthesis of Co-doped Ni-MOFs
Metal Source	Co(NO3)2.6H2O	Co/Ni = 2 mol%	2 · 2.1.2 Synthesis of Co-doped Ni-MOFs
Linker	1,4-benzenedicarboxylic acid	4 mmol	2 · 2.1.2 Synthesis of Co-doped Ni-MOFs
Solvent	DMF	as for Ni-MOF route	2 · 2.1.2 Synthesis of Co-doped Ni-MOFs
Acid	HCl	0.5 ml	2 · 2.1.2 Synthesis of Co-doped Ni-MOFs

Partial recipeSource: Main

Route 4: Hydrothermal

2 · 2.1.2 Synthesis of Co-doped Ni-MOFs

Metal precursorsNi(NO3)2.6H2O plus Co(NO3)2.6H2O; nominal Co/Ni = 5%

Linker precursors1,4-benzenedicarboxylic acid (4 mmol, from Ni-MOF route)

SolventsDMF

AdditivesHCl (0.5 mL, from Ni-MOF route)

Temperature180

Time24

Work-upSame as Ni-MOF: centrifugation and rinsing with DMF and ethanol.

ActivationVacuum oven drying for 12 h at 60 deg C; BET degassing at 150 deg C for 4 h before porosity test.

Scalability context100 mL autoclave by analogy to Ni-MOF route.

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Ni(NO3)2.6H2O	from Ni-MOF route	2 · 2.1.2 Synthesis of Co-doped Ni-MOFs
Metal Source	Co(NO3)2.6H2O	Co/Ni = 5 mol%	2 · 2.1.2 Synthesis of Co-doped Ni-MOFs
Linker	1,4-benzenedicarboxylic acid	4 mmol	2 · 2.1.2 Synthesis of Co-doped Ni-MOFs
Solvent	DMF	as for Ni-MOF route	2 · 2.1.2 Synthesis of Co-doped Ni-MOFs
Acid	HCl	0.5 ml	2 · 2.1.2 Synthesis of Co-doped Ni-MOFs

Partial recipeSource: Main

Route 5: Drop Cast

2 · 2.3.1 Electrochemical measurements in a three-electrode configuration

Additivesacetylene black; polytetrafluoroethylene

Temperature80

Substrate orientationnickel foam slice, 2.0 cm x 1.0 cm

Work-upSlurry coated on nickel foam.

ActivationDried in a vacuum oven at 80 deg C.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	active material	80 wt%	2 · 2.3.1 Electrochemical measurements in a three-electrode configuration
Additive	acetylene black	10 wt%	2 · 2.3.1 Electrochemical measurements in a three-electrode configuration
Additive	poly tetra fluoroethylene	10 wt%	2 · 2.3.1 Electrochemical measurements in a three-electrode configuration
Other	nickel foam	2.0 cm x 1.0 cm	2 · 2.3.1 Electrochemical measurements in a three-electrode configuration

Complete recipeSource: Main

Route 6: Hydrothermal

2 · 2.1.1 Synthesis of Ni-MOFs

Metal precursorsNi(NO3)2.6H2O (8 mmol)

Linker precursors1,4-benzenedicarboxylic acid (4 mmol)

SolventsDMF; 30 mL for solution A and 30 mL for solution B

AdditivesHCl (0.5 mL)

Temperature180

Time24

Work-upRecovered by centrifugation; rinsed three times with DMF and ethanol.

ActivationVacuum oven drying for 12 h at 60 deg C; BET degassing at 150 deg C for 4 h before porosity test.

Scalability context100 mL Teflon-lined stainless autoclave batch.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Ni(NO3)2.6H2O	8 mmol	2 · 2.1.1 Synthesis of Ni-MOFs
Linker	1,4-benzenedicarboxylic acid	4 mmol	2 · 2.1.1 Synthesis of Ni-MOFs
Solvent	DMF	30 ml for solution A; 30 ml for solution B	2 · 2.1.1 Synthesis of Ni-MOFs
Acid	HCl	0.5 ml	2 · 2.1.1 Synthesis of Ni-MOFs