Synthesis · A two-dimensional semiconducting covalent organic framework with nickel(II) coordination for high capacitive performance

6 structured synthesis routes

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

Partial recipeSource: SI

Route 1: Other

SI p.3 · Electrochemical performance experiments

Solvents3 M KOH aqueous electrolyte

AdditivesActivated carbon negative electrode

Work-upAsymmetric supercapacitor assembled with Ni-COF positive and activated carbon negative electrodes.

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	Ni-COF positive electrode	Not specified	SI p.3 · Electrochemical performance experiments
Other	activated carbon (AC) negative electrode	Not specified	SI p.3 · Electrochemical performance experiments
Electrolyte	KOH aqueous electrolyte	3 M	SI p.3 · Electrochemical performance experiments

Complete recipeSource: SI

Route 2: Other

SI p.3 · Electrochemical performance experiments

SolventsEthanol dispersion solvent

AdditivesAcetylene black and poly(tetrafluoroethylene) binder

Substrate orientationNi foam substrate, 1 cm2

Work-upUltrasonication to make slurry; slurry coated on Ni foam.

Scalability contextMass loading of active material on Ni foam was 5.0 mg cm^-2.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	Ni0-COF active material	8 parts by mass in active material:acetylene black:PTFE = 8:1:1	SI p.3 · Electrochemical performance experiments
Additive	acetylene black	1 part by mass	SI p.3 · Electrochemical performance experiments
Additive	poly(tetrafluoroethylene)	1 part by mass	SI p.3 · Electrochemical performance experiments
Solvent	ethanol	Not specified	SI p.3 · Electrochemical performance experiments

Complete recipeSource: SI

Route 3: Solvothermal

SI p.6 · Synthesis of Ni0-COF

Linker precursorsBTA, 20 mg, 0.07 mmol; HBC, 27.4 mg, 0.14 mmol

Solvents0.5 mL mesitylene and 1.5 mL 1,4-dioxane

Additives0.2 mL of 3 M aqueous acetic acid (AcOH)

AtmosphereSealed Teflon-lined stainless steel autoclave; atmosphere not specified.

Temperature120

Time72

Work-upCooled to room temperature; brown precipitate collected by filtration and washed with THF (3 x 20 mL), DMF (3 x 20 mL), and MeOH (3 x 20 mL).

ActivationSoxhlet extracted by THF for 24 h, then dried at 80 C under vacuum for 24 h.

Scalability contextSmall autoclave batch in ca. 10 mL glass bottle; 81% yield reported.

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Linker	1,2,4,5-benzenetetraamine tetrahydrochloride (BTA)	20 mg, 0.07 mmol	SI p.6 · Synthesis of Ni0-COF
Linker	2,5-dihydroxy-1,4-benzenedicarboxaldehyde (HBC)	27.4 mg, 0.14 mmol	SI p.6 · Synthesis of Ni0-COF
Acid	aqueous acetic acid (AcOH)	0.2 mL · 3 M	SI p.6 · Synthesis of Ni0-COF
Solvent	mesitylene	0.5 mL	SI p.6 · Synthesis of Ni0-COF
Solvent	1,4-dioxane	1.5 mL	SI p.6 · Synthesis of Ni0-COF

Complete recipeSource: SI

Route 4: Other

SI p.3 · Electrochemical performance experiments

SolventsEthanol dispersion solvent

AdditivesAcetylene black and poly(tetrafluoroethylene) binder

Substrate orientationNi foam substrate, 1 cm2

Work-upUltrasonication to make slurry; slurry coated on Ni foam.

Scalability contextMass loading of active material on Ni foam was 5.0 mg cm^-2.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	Ni-COF active material	8 parts by mass in active material:acetylene black:PTFE = 8:1:1	SI p.3 · Electrochemical performance experiments
Additive	acetylene black	1 part by mass	SI p.3 · Electrochemical performance experiments
Additive	poly(tetrafluoroethylene)	1 part by mass	SI p.3 · Electrochemical performance experiments
Solvent	ethanol	Not specified	SI p.3 · Electrochemical performance experiments

Complete recipeSource: Both

Route 5: Solvothermal

SI p.5 · Synthesis of Ni-COF

Metal precursorsExcess Ni(OAc)2.4H2O

Linker precursorsBTA, 20 mg, 0.07 mmol; HBC, 27.4 mg, 0.14 mmol

Solvents0.5 mL mesitylene and 1.5 mL 1,4-dioxane

AtmosphereSealed Teflon-lined stainless steel autoclave; atmosphere not specified.

Temperature120

Time72

Work-upCooled to room temperature; black precipitate collected by filtration and washed with THF (3 x 20 mL), DMF (3 x 20 mL), and MeOH (3 x 20 mL).

ActivationSoxhlet extracted by THF for 24 h, then dried at 80 C under vacuum for 24 h.

Scalability contextSmall autoclave batch in ca. 10 mL glass bottle; 86% yield reported.

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Linker	1,2,4,5-benzenetetraamine tetrahydrochloride (BTA)	20 mg, 0.07 mmol	SI p.5 · Synthesis of Ni-COF
Linker	2,5-dihydroxy-1,4-benzenedicarboxaldehyde (HBC)	27.4 mg, 0.14 mmol	SI p.5 · Synthesis of Ni-COF
Metal Source	Ni(OAc)2.4H2O	excess	SI p.5 · Synthesis of Ni-COF
Solvent	mesitylene	0.5 mL	SI p.5 · Synthesis of Ni-COF
Solvent	1,4-dioxane	1.5 mL	SI p.5 · Synthesis of Ni-COF

Vague recipeSource: Main

Route 6: Other

main p.3, article p.19678 · Electrical conductivity · Fig. 2i

Substrate orientationQuartz substrate