Synthesis · Revealing the effect of cobalt content and ligand exchange in the bimetallic Ni–Co MOF for stable supercapacitors with high energy density

8 structured synthesis routes

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

Complete recipeSource: Main

Route 1: Hydrothermal

p003 · 2.2

Metal precursorsCo(NO3)2.6H2O only; 5.5 mmol total metal ions

Linker precursorsH3BTC, 4 mmol

Solvents20 mL deionised water + 20 mL DMF

Atmospherenot reported

Temperature120

Time24

Work-upCool to room temperature; wash with 25 mL DMF and 25 mL ethanol, five times for each solvent.

ActivationVacuum drying at 60 deg C overnight

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Co(NO3)2.6H2O	5.5 mmol total metal ions, Co only	p003 · 2.2
Linker	H3BTC	4 mmol	p003 · 2.2
Solvent	deionized water + DMF	20 mL + 20 mL	p003 · 2.2

Partial recipeSource: Main

Route 2: Other

p010 · 3.4 · Fig. 7

Metal precursorsKNiCoPO4 positive active material

Solvents2 M NaOH electrolyte solution

Additivesactivated carbon negative electrode

Atmospherenot reported

Work-upPositive and negative electrode masses balanced using q+ = q-.

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	KNiCoPO4 positive electrode	m+/m- = 1:5	p010 · 3.4 · Fig. 7
Other	activated carbon negative electrode	m+/m- = 1:5	p010 · 3.4 · Fig. 7
Electrolyte	NaOH	2 M	p010 · 3.4 · Fig. 7

Complete recipeSource: Main

Route 3: Hydrothermal

p003 · 2.2

Metal precursors0.2 g NiCo-M (10:1) precursor

Linker precursorsPhosphate supplied by K3PO4; BTC ligand from precursor is replaced

Solvents20 mL ethanol-water mixture (1:1)

Additives0.26 g K3PO4

Atmospherenot reported

Temperature160

Time15

Work-upStir 1 h, sonicate 15 min, autoclave, cool, wash five times with 25 mL deionised water.

ActivationDrying at 60 deg C overnight

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	NiCo-M (10:1)	0.2 g	p003 · 2.2
Additive	K3PO4	0.26 g	p003 · 2.2
Solvent	ethanol-water mixture (1:1)	20 mL	p003 · 2.2

Complete recipeSource: Main

Route 4: Hydrothermal

p003 · 2.2

Metal precursorsNi(NO3)2.6H2O only; 5.5 mmol total metal ions

Linker precursorsH3BTC, 4 mmol

Solvents20 mL deionised water + 20 mL DMF

Atmospherenot reported

Temperature120

Time24

Work-upCool to room temperature; wash with 25 mL DMF and 25 mL ethanol, five times for each solvent.

ActivationVacuum drying at 60 deg C overnight

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Ni(NO3)2.6H2O	5.5 mmol total metal ions, Ni only	p003 · 2.2
Linker	H3BTC	4 mmol	p003 · 2.2
Solvent	deionized water	20 mL	p003 · 2.2
Solvent	DMF	20 mL	p003 · 2.2

Complete recipeSource: Main

Route 5: Hydrothermal

p003 · 2.2

Metal precursorsNi(NO3)2.6H2O and Co(NO3)2.6H2O; 5.5 mmol total metal ions; Ni/Co = 10:1

Linker precursorsH3BTC, 4 mmol

Solvents20 mL deionised water + 20 mL DMF

Atmospherenot reported

Temperature120

Time24

Work-upCool to room temperature; wash with 25 mL DMF and 25 mL ethanol, five times for each solvent.

ActivationVacuum drying at 60 deg C overnight

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Ni(NO3)2.6H2O	stoichiometric portion of 5.5 mmol total metal ions; Ni/Co = 10:1	p003 · 2.2
Metal Source	Co(NO3)2.6H2O	stoichiometric portion of 5.5 mmol total metal ions; Ni/Co = 10:1	p003 · 2.2
Linker	H3BTC	4 mmol	p003 · 2.2
Solvent	deionized water + DMF	20 mL + 20 mL	p003 · 2.2

Complete recipeSource: Main

Route 6: Hydrothermal

p003 · 2.2

Metal precursorsNi(NO3)2.6H2O and Co(NO3)2.6H2O; 5.5 mmol total metal ions; Ni/Co = 1:10

Linker precursorsH3BTC, 4 mmol

Solvents20 mL deionised water + 20 mL DMF

Atmospherenot reported

Temperature120

Time24

Work-upCool to room temperature; wash with 25 mL DMF and 25 mL ethanol, five times for each solvent.

ActivationVacuum drying at 60 deg C overnight

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Ni(NO3)2.6H2O and Co(NO3)2.6H2O	5.5 mmol total metal ions; Ni/Co = 1:10	p003 · 2.2
Linker	H3BTC	4 mmol	p003 · 2.2
Solvent	deionized water + DMF	20 mL + 20 mL	p003 · 2.2

Complete recipeSource: Main

Route 7: Hydrothermal

p003 · 2.2

Metal precursorsNi(NO3)2.6H2O and Co(NO3)2.6H2O; 5.5 mmol total metal ions; Ni/Co = 1:1

Linker precursorsH3BTC, 4 mmol

Solvents20 mL deionised water + 20 mL DMF

Atmospherenot reported

Temperature120

Time24

Work-upCool to room temperature; wash with 25 mL DMF and 25 mL ethanol, five times for each solvent.

ActivationVacuum drying at 60 deg C overnight

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Ni(NO3)2.6H2O and Co(NO3)2.6H2O	5.5 mmol total metal ions; Ni/Co = 1:1	p003 · 2.2
Linker	H3BTC	4 mmol	p003 · 2.2
Solvent	deionized water + DMF	20 mL + 20 mL	p003 · 2.2

Complete recipeSource: Main

Route 8: Drop Cast

p003 · 2.4

Metal precursorsActive material: Ni-M, NiCo-M, Co-M, or KNiCoPO4 depending on electrode

SolventsNMP

Additivescarbon black and PVDF binder

Atmospherevacuum drying

Temperature80

Timeovernight

Substrate orientation0.5 x 0.5 cm2 Toray carbon paper TGP-H-060

Work-upSlurry coated onto carbon paper.

ActivationVacuum drying at 80 deg C overnight

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	active material	70 wt%	p003 · 2.4
Additive	carbon black	15 wt%	p003 · 2.4
Additive	PVDF	15 wt%	p003 · 2.4
Solvent	NMP	Not specified	p003 · 2.4